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task2/task2-chunks/2_UV╖└╬э╥║╩╣╙├╦╡├ў╩щ.json
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[
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{
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"id": 1,
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"chunk": "# UV 防雾液产品说明",
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"category": " Introduction"
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},
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{
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"id": 2,
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"chunk": "# 一、产品简介 \n\nUV 防雾液是一款杂化高分子功能材料液体。本产品主体成分为UV 亲水树脂，在PC 塑料板上有着良好的附着并有着优异的防雾性。对人体无刺激，适应性强，施工性优异。",
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"category": " Introduction"
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},
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{
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"id": 3,
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"chunk": "# 二、产品特点 \n\n硬化优异 \n持久防雾性强 \n良好的黏胶覆膜适应性 \n附着力佳",
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"category": " Results and discussion"
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},
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{
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"id": 4,
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"chunk": "# 三、施工参数 \n\n<html><body><table><tr><td>编号</td><td>项目</td><td>单位</td><td>参数</td><td>备注</td></tr><tr><td>1</td><td>开稀比例</td><td>/</td><td>0~30%</td><td></td></tr><tr><td>２</td><td>涂层厚度</td><td>μm</td><td>5-8</td><td></td></tr><tr><td>3</td><td>流平烘烤温度</td><td>℃</td><td>50~60</td><td></td></tr><tr><td>4</td><td>UV固化能量</td><td> J/cm²</td><td>480-550</td><td></td></tr></table></body></html> \n\n本产品可以直接进行淋涂，根据需要进行适当稀释，稀释比例不得超过 $30\\%$ 。",
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"category": " Materials and methods"
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},
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{
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"id": 5,
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"chunk": "# 四、存储和运输 \n\n1）运输过程中防止撞击和挤压，防止暴晒，按一般危险品运输。 \n2）密封储存于阴凉、干燥通风处，防潮防水，远离火源、热源。需要防潮。 \n3）最好存放请保存环境请低于 $30^{\\circ}\\mathrm{C}$ ，但不建议低于 $10^{\\circ}\\mathrm{C}$ 。保存环境的相对湿度低 \n于 $40\\%\\mathrm{RH}$ 为佳。 \n4）使用期限：6 个月。",
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"category": " Materials and methods"
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}
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]
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task2/task2-chunks/AI╙├╙┌╙╨╗·-╛█║╧╬я║╧│╔.json
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[
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{
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"id": 1,
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"chunk": "# AI技术在化工行业设计工作中的应用展望 \n\n姜宜君 \n\n（中海油石化工程有限公司，山东青岛 266101） \n\n摘 要：随着人工智能（Artifi cial Intelligence, AI）技术的飞速发展，其在化工行业设计工作中的应用已经引起了广泛关注。AI 技术以其强大的自然语言处理能力、数据分析能力和逻辑推理能力，为化工行业设计带来了革命性的变化。首先解析了AI 技术具备数据分析、自然语言处理、知识融合、机器视觉能力，发现这些 AI 能力能够在化工设计领域发挥一定的价值。其次，深入探讨了 AI 技术在化工设计领域的知识管理、图纸管理、设计流程自动化等诸多核心设计过程的应用场景。化工设计场景在AI 的赋能下，不仅提高了设计效率，降低了成本，还实现了知识共享的愿景。然后，针对 $\\mathrm{AI^{+}}$ 化工设计应用场景，识别出目前 AI 在智能化设计、跨学科融合和人工智能伦理安全的风险与挑战。最后，对 AI 技术在化工行业设计中的未来发展进行了展望，预见其将实现更高级别的智能化、更广泛的应用领域以及更紧密的产业融合，并进一步推动化工行业设计的创新与发展。 \n\n关键词：AI 技术；人工智能；化工设计；智能设计；数字化中图分类号：TP29 文献标志码：A 文章编号 ：1003-6490（2025）01-0103-04",
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"category": " Abstract"
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},
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{
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"id": 2,
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"chunk": "# Application Prospect of AI Technology in Chemical Industry Design \n\nJIANG Yijun \n\nAbstract: With the rapid development of artificial intelligence technology, its application in the design work of the chemical industry has attracted extensive attention. With its powerful natural language processing capabilities, data analysis capabilities, and logical reasoning capabilities, AI technology has brought revolutionary changes to the design of the chemical industry. Firstly, this paper analyzes the capabilities of AI technology in data analysis, natural language processing, knowledge fusion, and machine vision, and finds that these AI capabilities can play a certain value in the field of chemical design. Secondly, this paper deeply discusses the application scenarios of AI technology in many core design processes in the field of chemical design, such as knowledge management, drawing management, and design process automation. With the empowerment of AI, the chemical design scenario not only improves design efficiency and reduces costs, but also realizes the vision of knowledge sharing. Then, for the application scenario of $\\mathrm{AI^{+}}$ chemical design, the current risks and challenges of AI in intelligent design, interdisciplinary integration and artificial intelligence ethical security are identified. Finally, the future development of AI technology in the design of the chemical industry is prospected, and it is foreseen that it will achieve a higher level of intelligence, a wider range of application fields and closer industrial integration, and further promote the innovation and development of design in the chemical industry. \n\nKeywords: AI technology; artificial intelligence; chemical engineering design;intelligent design; digitization",
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"category": " Abstract"
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},
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{
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"id": 3,
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"chunk": "# 0 序言 \n\nAI 技术是一种让计算机具备人的学习、思考、推理和自主学习技术，旨在能够让计算机“以人的行为和思维方式”完成一系列工作或任务。2022年OpenAI 的 ChatGPT 横空出世，各行业、专业领域、业务场景不断探索出与 AI 融合的业务场景或商业模式，不断提升业务智能化的进程。同时，这些 AI 场景，也在反向促进AI 的发展。尽管业务搭上AI 的便车实现了更高效、智能的发展，但是，正由于 AI“能够以人的思维方式”工作，这也不由得引起人们对其安全性、可靠性、保密性等诸多方面的担忧。我们希望搭建安全可信的AI 应用场景，一方面，借助于 AI 在各行业、专业领域、各业务部门之间搭建更加高效的协同桥梁，降低因专业壁垒导致的技术鸿沟，另一方面，也应该提升 AI 的安全性，在共享业务系统和知识的过程中，避免数据泄露，并让 AI 基于化工基本伦理工作，减少上述忧虑。",
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"category": " Introduction"
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},
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{
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"id": 4,
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"chunk": "# 1 AI 技术及其在化工设计中的应用背景 \n\n化工设计行业专业性较高，并且设计过程复杂，因其在效率、成本、质量、安全等方面均有较高的要求，一直以来，针对这些问题并没有较好的解决方案。而AI 能够基于大数据，通过对数据的挖掘和自我学习，发现化工设计过程中隐藏的设计模式，帮助设计过程更加科学、高效，进而提出创新性的解决方案，在化工设计应用过程中可发挥巨大作用。",
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"category": " Introduction"
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},
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{
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"id": 5,
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"chunk": "# 1.1 数据分析与优化功能 \n\n在化工设计中，AI 技术通过对行业设计数据和公司已交付工程进行数据机器学习和深度学习，挖掘出化工设计过程的设计规律和发展趋势，为化工设计人员提供高效的数据分析和优化能力，并对化工设计过程提供较完备的设计建议。同时，因机器学习算法具备自我学习和进化的能力，从而能够在不断对新产生设计数据的挖掘和学习过程中，根据正向的知识反馈，不断优化算法，提升数据分析的准确性，进而反馈质量和效率“双高”的设计建议。 \n\n在未来的设计过程中，设计人员可以借助于生成式AI，改变传统的设计模式：将“以人的经验为中心”的设计模式，转变为“用 AI 辅助”的设计模式。在新的设计模式下，设计人员可以将项目背景、设计规范以及设计要求以“提示词”的形式投喂给 AI，让AI 辅助生成初步的设计图纸。这些设计图纸，为设计人员提供比较丰富的设计灵感和参考思路，为基础设计阶段打下坚实的基础。进入详细设计阶段后，设计人员将基础设计阶段选型的设计图纸，结合进一步细化的设计需求和相关业务调度要求，以提示词的形式与 AI 进行交互，在经过多轮的交互后，得到既满足业务需求，又具有创新性的设计方案[3]。",
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"category": " Introduction"
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},
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{
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"id": 6,
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"chunk": "# 1.2 自然语言处理与知识管理功能 \n\n自然语言处理（Nature Language Processing, NLP）技术因其能够理解并处理自然语言，所以在化工设计过程中，可以使用NLP 技术解析行业规范、化学文献、实验报告等文本数据，从中提取出对设计有价值的信息和知识，搭建具备 NLP 功能的知识管理能力，提升设计人员的知识检索效率。此外，NLP 能够将分散的设计系统、行业知识进行关联，形成独有专业的“知识图谱”，为化工设计工作者提供全方位的设计指引，避免因为遗漏设计规范和法规条例出现设计反复修改甚至设计事故。",
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"category": " Introduction"
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},
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{
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"id": 7,
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"chunk": "# 1.3 计算机视觉与专家系统 \n\n计算机视觉具有强大的监控和检测功能，在笔记识别、绘图识别、实物识别等领域有广泛的应用 [4]。通过图像和视频数据，实时监控生产过程、检测产品质量、设备状态等关键信息，及时发现并预警各个业务环节出现的问题和异常信息。例如，对于化工反应过程中颜色、气泡等显著特性的变化，机器视觉可以自动识别反应结果，帮助设计师及时调整工艺参数。现阶段某些可燃气体检测仪便是运用了机器视觉技术，达到了对气体泄漏的检测甚至提前预测的目的。 \n\n专家系统则集成了化工领域的专业知识和经验，能够模拟人类专家的思考过程，解决复杂的设计问题，为此，专家系统能够为设计师提供权威的决策支持和建议 [5]。在化工设计过程中，一方面，专家系统能够根据设计师人员的需求和约束条件，为其提供更加贴近项目实际场景的设计方案、材料选型和工艺参数等建议；另一方面，专家系统基于对历史数据和实时数据的分析，预测出生产过程中的潜在风险，并提供针对性的解决方案。当然，为了达到以上的应用效果，专家系统需要对海量的设计文件、行业经验、文献、规范等非结构化的“自然语言”文本不断迭代和学习，提升 AI 的自主推理和学习能力，保证专家系统具备“专家能力”。 \n\n化工设计可以借助于AI 相关的数据分析与优化、自然语言处理与知识管理、计算机视觉与专家系统等多种功能和应用场景，提高化工设计的效率和质量，挖掘更多的创新场景和发展机遇。",
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"category": " Introduction"
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},
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{
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"id": 8,
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"chunk": "# 2 AI 技术在化工设计过程中的应用场景",
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"category": " Introduction"
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},
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{
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"id": 9,
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"chunk": "# 2.1 AI+化工设计知识管理应用场景",
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"category": " Introduction"
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},
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{
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"id": 10,
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"chunk": "# 2.1.1 自动化与智能化整合 \n\n在化工设计领域，利用机器学习技术的自动化搜索和智能分类能力，可极大地提高设计人员查找和整合规范文档的效率。利用深度学习和自然语言处理技术，机器学习模型能够自动从海量规范中提取关键特征，以向量的形式关联业务关键点，形成知识图谱的底层数据要素，构建高效的搜索索引，形成垂直领域的知识图谱，方便设计人员向 AI 发起基于专业提示词的对话。 \n\nAI 通过对提示词的解析，在专业知识库中完成快速、精准检索后，将结果组装后反馈给设计人员。此外，机器学习还能将设计领域与其他相关领域的知识图谱进行关联和融合，实现跨领域级知识的关联和检索，更好地为设计工作提供相关领域知识的智能推荐和业务指引。如针对工程师基于设计规范、专业背景和项目需求等特征，由 AI 提供跨领域融合的智能化解决方案，有效帮助工程师获取完备的设计规范，同时也能够促进设计行业的知识发现和业务创新。",
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"category": " Introduction"
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},
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{
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"id": 11,
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"chunk": "# 2.1.2 预测性分析与可视化展示 \n\n机器学习不仅提供了高效的信息整合和检索能力，还具备对业务数据的可视化展示和预测性分析的能力。通过对历史数据和行业动态的分析，机器学习能够预测规范的发展趋势和潜在变化，帮助企业提前做好应对策略，以在新的发展阶段寻求发展机遇和应对挑战。同时，机器学习还能将规范信息以流程图、思维导图、热力图、数据流图等可视化的方式展示，帮助工程师更直观地理解规范内容，让工程师将设计过程聚焦在行业规范和风险特征较高的设计流程中，减少因对冗余信息的检索和排查而导致的沉没成本，提高信息的吸收和应用效率。此外，机器学习模型具有自我学习和持续进化的能力，随着数据的积累和模型的优化，其对设计要素的完备性和准确度将不断提升，这将有助于提升化工设计规范的整合能力与信息检索能力。",
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"category": " Results and discussion"
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},
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{
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"id": 12,
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"chunk": "# 2.2 $\\mathbf{A}\\mathbf{I}+$ 化工图纸绘制应用场景 \n\n将 AI 的视觉检测技术应用到化工设计过程中的图纸识别与分析、图纸错误检测、图纸标准化、图纸的三维建模与分析、图纸与模型的相互转换、设计参数优化、设计流程自动化等设计场景，有效提升图纸绘制的效率和准确性。",
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"category": " Introduction"
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},
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{
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"id": 13,
|
||||
"chunk": "# 2.2.1 自动化图纸识别与分析 \n\n在化工设计中，图纸是设计师们表达设计意图、展示工艺流程的重要工具。传统的手工图纸因为是由设计人员识别与分析，以至于整个设计过程不仅耗时高，而且还容易出现遗漏项导致错误率居高不下。计算机视觉技术通过先进的图像识别和模式匹配算法，能够迅速而准确地识别图纸中如管道、阀门、泵等各类元素，并理解它们之间的相关性，形成集统计、合规性于一体的分析报告。这不仅加快了设计分析的速度，提高了分析的准确性，为后续的设计修改、优化和审阅提供了坚实的基础；而且结合了 AI 的风险识别能力，依托 AI 已经整合的设计规范、法律法规和最佳设计案例，AI 能够快速并有效地根据识别出的遗漏的设计要素和“非规范化设计要素”，帮助设计人员规避业务风险。",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 14,
|
||||
"chunk": "# 2.2.2 图纸错误检测 \n\n化工设计图纸中的错误可能会导致严重的后果，轻则损坏设备，重则导致生产事故，为此，图纸错误检测在设计过程中具有相当重要的分量。因此，如何及时发现图纸中的错误，并提供有效修改建议，变得尤其重要。计算机视觉技术能够开发出高效的图纸错误检测系统，能识别图纸中的潜在错误，如设备尺寸错误、连接错误等，并及时提醒设计师进行修正。这不仅减少了设计错误发生的概率，还提高了设计的可靠性和安全性。在人与 AI 交互的过程中，设计人员不断将修改的建议迭代到 AI 的认知能力库中，逐步完善 AI 的错误检测和错误修正能力，最终实现让 AI帮助设计人员完成图纸错误检测和修正的工作，达到提高设计效率的目的。",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 15,
|
||||
"chunk": "# 2.2.3 图纸标准化 \n\n由于每一位设计人员参与的项目不同，设计习惯也因此有一定的差异，这便为图纸的标准化带来一定的挑战。图纸的标准化可以使项目风格统一、提高成品文件设计质量，更有效地实现信息共享。计算机视觉技术的应用便可以提供如检测设计文件图例是否正确、格式是否统一、数据是否完整等服务，极大地提高了标准化程度与检测的效率和准确率。",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 16,
|
||||
"chunk": "# 2.2.4 三维建模与可视化 \n\n三维建模在化工设计中已极为普遍，智慧工厂设计、数字化交付技术更是趋于成熟。计算机视觉技术甚至可以检查检修人员的巡检路线是否畅通，以便修改设计使得符合实际情况。这不仅有助于设计师更好地分析设计细节，还为后续的项目审查、优化等提供 \n\n了有力支持。",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 17,
|
||||
"chunk": "# 2.2.5 设计流程自动化 \n\n传统的化工设计流程往往需要大量的人工输入、统计和检查工作，这往往会浪费大量的时间，并且会因为复杂度的提升而容易出错。通过自动识别图纸中的元器件、工艺流程等信息，并将其记录到设计软件中，视觉技术自动完成相关设计输入和统计相关的工作，在提高设计效率的同时，自动检查设计过程中存在的疏漏或风险，确保设计的准确性和可靠性。基于此，视觉技术有效代替设计人员的手工操作，帮助设计人员完成容易遗漏的差错检测，并结合 AI 的图例能力，可逐步实现流程的自动化设计，提升流程设计的自动化水平。",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 18,
|
||||
"chunk": "# 3 AI 技术在化工设计中面临的挑战与机遇",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 19,
|
||||
"chunk": "# 3.1 智能化设计 \n\n传统的化工设计过程往往依赖于人工经验和复杂的计算，而 AI 系统则能够凭借其强大的数据处理和分析能力，更深入地理解设计需求和市场趋势。通过机器学习、深度学习等算法，AI 系统可以自动完成部分如模拟实验、参数优化等设计工作，从而大大提高设计效率和质量。尽管 AI 算法能够根据大数据的统计规律自动生成设计方案，但往往因为 AI 使用类似的推理模型容易出现较常规和无差异化的解决方案，这难以匹配实际的业务需求，而对于设计人员的辅助设计来说，反而会将“利器”变为“累赘”。此外，AI 技术在处理复杂问题和非结构化任务时仍面临诸多挑战，其能力尚未达到人类工程师的综合决策水平。设计工程师在设计中能够综合考虑诸如环境、规范、业务需求、客户偏好、设计理念等诸多复杂和不可控的因素，而 AI 技术在这方面仍有待进一步发展和提升。 \n\n设计师可以借助于智能化设计，从繁琐的计算和模拟工作中脱离出来，从而更加专注于设计模式优化和创新。此外，AI 系统还可以根据市场反馈和消费者需求，快速调整设计方案，以满足不断变化的市场需求和发展趋势。",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 20,
|
||||
"chunk": "# 3.2 跨学科融合 \n\n化工设计是一个涉及化学、物理、机械等多个学科的复杂过程。传统的化工设计往往因为存在学科壁垒，导致各学科之间的知识和经验无法有效融合和共享，AI 技术的出现，为跨学科融合提供了新的方式。 \n\n在化工设计产品过程中，借助于AI 的信息整合能力，以“统一语言”的形式，输出让各专业领域相互理解的设计模式。因此，在化工设计过程中，AI 可以帮助各专业突破专业障碍，降低沟通难度，提升沟通和协作效率，从而促进化工产品设计的革新与开发。",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 21,
|
||||
"chunk": "# 3.3 人工智能伦理和安全的关注 \n\n尽管AI 技术在化工设计中具有丰富的应用场景，（下转第115页） \n\n压缩机基础荷载较大，采用天然地基或地基处理不能满足设计要求，应采用桩基础。因压缩机厂房基础底部的拔力较大，需要桩能提供很大的抗拔力，所以本工程选用干作业灌注桩。以第 $\\textcircled{5}$ 层强风化岩为桩基持力层，计算得单桩竖向抗压承载力特征值为 $1~100\\mathrm{kN}$ 。需要注意的是，根据《动力机器基础设计标准》（GB50040—2020）第 3.3.1 条及 3.3.3 条，桩基承载力需要乘以动力折减系数，旋转式机器基础可取0.8。 \n\n采用PKPM 基础设计版块进行基础的设计，基础底板尺寸为 $15\\mathrm{m}\\times6.9\\mathrm{m}$ ，布置三行六列灌注桩。计算得最大桩基反力为 $550\\mathrm{kPa}$ ，平均桩基反力为 $514~\\mathrm{kPa}$ ，满足承载力要求。",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 22,
|
||||
"chunk": "# 2 结语 \n\n当动力机器基础的振动响应超过容许振动标准时，会造成动力机器机器振动过大，减少使用寿命，降低工作效率，被迫停止工作，造成设备附属管道和零部件损坏，会对操作人员舒适性造成不良影响，会对附属建筑结构造成损伤、破坏，甚至引发工程事故。因此进行动力机器基础的动力计算很有必要。通过工程计算实践证明，STAAD.Pro 非常适用于构架式压缩机基础的动力计算。其空间建模方便，计算模型合理，而且结果直接详细，为大型构架式动力机器的发展提供了便利的条件。 \n\n构架式压缩机基础设计是一项繁重而复杂的过程，不仅仅是为了避免经济损失，更是为了保证操作人员的人身安全。作为一个合格的设计人员，我们要对自己负责，也要对别人负责，做新时代的好青年。",
|
||||
"category": " Conclusions"
|
||||
},
|
||||
{
|
||||
"id": 23,
|
||||
"chunk": "# 参考文献 \n\n[1] 中华人民共和国工业和信息化部 . 石油化工压缩机基础设计规范 : SH/T 3091—2012[S]. 北京 : 中国石化出版社 , 2013. \n[2] 中华人民共和国住房和城乡建设部 . 动力机器基础设计标准 : GB 50040—2020[S]. 北京 : 中国计划出版社 ,2021.",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 24,
|
||||
"chunk": "# （上接第105页） \n\n也能为化工设计过程带来便捷的设计体验，但因其具备“人的思维方式”，我们不得不面临AI带来的伦理和安全方面的诸多挑战。 \n\n人工智能伦理问题应优先考虑。随着 AI 系统在化工设计中的应用日益广泛，如何确保 AI 系统的道德合规性、避免潜在的伦理风险成为亟待解决的问题。我们需要制定相应的伦理规范和监管机制来确保 AI能够秉持化工伦理的基本准则来赋能化工各场景。 \n\n数据安全也是 $\\mathrm{AI^{+}}$ 化工场景的关键问题。在大数据时代，尽管设计师可以借助 AI 的学习成果，提高设计团队的协作效率，发现设计过程中的潜在风险，以便提前采取预防措施，但设计人员投喂给 AI 的资料，也必将成为 AI 的学习资料，这将很有可能出现数据泄露的风险，进而出现公司、行业和国家机密泄露的风险。所以，AI 在化工行业应用的过程中，如何保障数据安全将成为至关重要的环节。 \n\n综上，我们需要采取有效的技术手段和管理措施来防止数据泄露、非法获取和滥用等风险的发生。",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 25,
|
||||
"chunk": "# 4 结论 \n\nAI 技术在化工设计过程中具有广泛的应用前景，也面临着安全与伦理等诸多方面的挑战。通过提高设计效率和质量、降低设计风险、实现个性化定制设计、推动设计业务流程高效协同等多种场景的融合，AI技术将为化工设计带来新的变革。",
|
||||
"category": " Conclusions"
|
||||
},
|
||||
{
|
||||
"id": 26,
|
||||
"chunk": "# 参考文献 \n\n[1] 梁庆国. AI 人工智能技术应用于设计专业实践教学的跨界合作与创新模式研究 [J]. 现代职业教育 , 2024(4): 153-156. \n[2] Huang J W. Digital engineering transformation withtrustworthy AI towards industry 4.0: emerging paradigmshifts[J]. ArXiv e-Prints, 2023: arXiv: 2301.00951. \n[3] 黎锐垣. 工业设计的转变: 人工智能全流程应用[J]. 产业创新研究 , 2024(4): 38-40. \n[4] 马明 , 贾楠 , 苏璐 . 工程图纸图像识别技术在数字化交付中的应用 [J]. 石油化工建设 , 2021, 43(6): 63-65. \n[5] 李强 . 人工智能教育研究专家系统构建框架及实施 [J].天津市教科院学报 , 2020, 32(1): 42-48.",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 27,
|
||||
"chunk": "# 版 权 声 明 \n\n录稿通知发出后，视为投稿人已阅读并理解我刊“投稿须知”等内容。例如，投稿人投稿时请勿“一稿多投”；根据国家著作权法，编辑部享有作品的汇编权和文字修改权等权力，所发表文章版权归编辑部所有。投稿人将作品交本刊刊载的同时也同意将其信息网络传播权授予我编辑部等等。本声明所说的信息网络传播权，包含相应的电子版本复制权。如发现已录用稿件有学术不端行为嫌疑的，编辑部有权将其从美国《化学文摘》、知网、万方、维普、超星等数据库平台撤稿。 \n\n《化工设计通讯》编辑部",
|
||||
"category": " References"
|
||||
}
|
||||
]
|
||||
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|
||||
[
|
||||
{
|
||||
"id": 1,
|
||||
"chunk": "# (19)国家知识产权局",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 2,
|
||||
"chunk": "# (12)发明专利 \n\n(21)申请号 202210559327 .7(22)申请日 2022.05.23(65)同一申请的已公布的文献号申请公布号 CN 115521452 A(43)申请公布日 2022.12.27(73)专利权人 武汉中科先进材料科技有限公司地址 430000 湖北省武汉市经济技术开发区201M地块华人汇和科技园（华中智谷）一期F10研发楼1-2层 \n\n(72)发明人 康翼鸿 喻学锋 吴列 杨帆程文杰 甄亚枝 \n\n(74)专利代理机构 武汉高得专利代理事务所(普通合伙) 42268专利代理师 陈挥秀",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 3,
|
||||
"chunk": "# (54)发明名称 \n\n一种光固化低聚物、其制备方法及含有该低聚物的光固化涂料 \n\n(51)Int.Cl. C08G 65/3 3(2006.01) C09D 171/02(2006.01) \n\n(56)对比文件 CN 102762657 A,2012.10.31 CN 107057555 A,2017 .08.18 US 5907023 A,1999.05.25 JP 2014218621 A,2014 .11 .20 CN 112048051 A,2020.12.08 CN 113943529 A,2022.01 .18 \n\n审查员 贺勇",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 4,
|
||||
"chunk": "# (57)摘要 \n\n本发明属于高分子材料技术领域，具体地说，涉及一种光固化低聚物、其制备方法及含有该低聚物的光固化涂料。该种光固化低聚物结构为以脲基基团为交联点、聚氧乙烯醚为主链段的脲基丙烯酸酯。低聚物具有低黏度、高速固化、有特殊功能等优点，针对部分基材难以附着的特点，在PMMA、聚砜、聚苯乙烯上均有较好的附着力，可应用在难附着基材的防雾、防污、减阻、润湿等领域。 \n\n \n\n1.一种光固化低聚物，其特征在于，具有以下结构： \n\n \n\n其中， $\\mathrm{y}\\approx39$ ， $\\mathrm{X^{+}Z}{\\approx}6$ 。 \n\n2.权利要求1所述的光固化低聚物的制备方法，其特征在于，包括以下步骤： \n\n(1)聚醚胺与三(2‑羟乙基)异氰脲酸三丙烯酸酯在 $60-80^{\\circ}\\mathrm{C}$ 下进行加成反应，得到异氰尿酸聚醚胺丙烯酸酯；(2)羟乙基丙烯酸酯与异佛尔酮二异氰酸酯在 $30-50^{\\circ}\\mathrm{C}$ 下反应0.5‑1h，得到脲基丙烯酸酯；(3)将步骤(1)和步骤(2)所得产物在 $30-50^{\\circ}\\mathrm{C}$ 下进行聚合反应，反应0.5‑1h，即得到所述光固化低聚物，命名为异氰尿酸聚氧乙烯醚丙烯酸酯。3.根据权利要求2所述光固化低聚物的制备方法，其特征在于，所述步骤(1)中聚醚胺与三(2‑羟乙基)异氰脲酸三丙烯酸酯的摩尔比为1：2。4.根据权利要求2所述光固化低聚物的制备方法，其特征在于，所述步骤(2)中羟乙基丙烯酸酯与异佛尔酮二异氰酸酯的摩尔比为1：1。5.根据权利要求2所述光固化低聚物的制备方法，其特征在于，所述步骤(1)和步骤(2)所得产物的摩尔比为1：1。6.一种光固化涂料，包含权利要求1所述光固化低聚物、丙烯酸酯单体、光引发剂、助剂和溶剂。7.根据权利要求6所述光固化涂料，其特征在于：光引发剂为2‑羟基‑2‑甲基‑1‑苯基丙酮，1‑羟基环己基苯基甲酮，2,4,6‑三甲基苯甲酰基‑二苯基氧化膦中的一种或多种。8.根据权利要求6所述光固化涂料，其特征在于：助剂为流平剂、消泡剂、增稠剂、分散剂、润湿剂中的一种或多种。9.根据权利要求6所述光固化涂料，其特征在于：溶剂为乙醇、异丙醇、乙酸乙酯、乙酸丁酯、丙二醇甲醚中的一种或多种。",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 5,
|
||||
"chunk": "# 一种光固化低聚物、其制备方法及含有该低聚物的光固化涂料",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 6,
|
||||
"chunk": "# 技术领域 \n\n[0001] 本发明属于高分子材料技术领域，具体地说，涉及一种光固化低聚物、其制备方法及含有该低聚物的光固化涂料。",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 7,
|
||||
"chunk": "# 背景技术 \n\n[0002] 紫外光固化涂料技术是指一种表面处理技术，该技术通过光引发剂或者光敏剂，经紫外光辐照产生自由基而引发活性单体、低聚物或树脂发生聚合反应。近年来，人们对环保的要求越来越高，溶剂型涂料因为挥发性有机物(VOC)的排放受到越来越严格的限制，以紫外光固化涂料(UVCC)、水性涂料、高固体分涂料和粉末涂料为代表的绿色环保型涂料成为人们关注和研究的热点。与其它几类涂料相比，UVCC具有固化速度快、固化温度低、环保节能、涂层性能优异，可用于塑料、纸张和木材等热敏性底材的涂布等优势。 \n\n[0003] 低聚物是UV固化涂料最重要的组分，它决定了固化膜的物理机械性能，如硬度、柔韧性、强度、耐磨性、附着力等，也影响光固化速度。目前的低聚物通常是聚乙二醇丙烯酸酯等附着力低的物质或聚氨酯丙烯酸酯等亲水性差的物质，难以保持附着力与亲水性的平衡。 \n\n[0004] 目前常见的光固化低聚物包括环氧丙烯酸酯、聚氨酯丙烯酸酯、聚酯丙烯酸酯等，具有黏度低、固化速度快等优点，但是低聚物往往没有丰富的基团，附着力差。高聚后链段较软，机械强度差。",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 8,
|
||||
"chunk": "# 发明内容 \n\n[0005] 本发明的目的是针对现有技术的不足，提供附着力优异的一种光固化低聚物、其制备方法及含有该低聚物的光固化涂料。可实现高附着力、高耐磨、耐水泡、耐腐蚀等的功能。 \n\n[0006] 为实现上述目的，本发明首先提供一种光固化低聚物，如(Ⅰ)所示，结构为以脲基基团为交联点、聚氧乙烯醚为主链段的脲基丙烯酸酯，可命名为异氰尿酸聚氧乙烯醚丙烯酸酯； \n\n[0007] 所述光固化低聚物表面张力低，对基材润湿性好；对于PMMA、聚砜、聚苯乙烯等塑料基材有较强的渗透溶胀能力，固化交联后可在基材与涂层之间形成一层很薄的互穿网络结构，从而增强附着力，同时所述光固化低聚物含有多种官能团，能提高附着力。 \n\n[0008] 按照GB/T 9286‑1998进行光固化低聚物的附着力测试，0级代表最好，5级代表最差，具体方法为将光固化低聚物与光引发剂TPO以质量比24：1混合，UV灯下固化30s，测试附着力，结果附着力均为0级。 \n\n \n（I) \n\n[0010] 本发明还提供一种光固化低聚物的制备方法，具体如下： \n\n[0011] (1)聚醚胺(ED2003)与三(2‑羟乙基)异氰脲酸三丙烯酸酯(THEICTA)在 $60-80^{\\circ}\\mathrm{C}$ 下进行加成反应，得到聚氧乙烯醚异氰尿酸丙烯酸酯； \n[0012] (2)羟乙基丙烯酸酯(HEA)与异佛尔酮二异氰酸酯(IPDI)在 $30-50^{\\circ}\\mathrm{C}$ 下反应0 .5‑1h，得到脲基丙烯酸酯； \n[0013] (3)将步骤(1)和步骤(2)所得产物在 $30-50^{\\circ}\\mathrm{C}$ 下进行聚合反应，反应0.5‑1h，即得到所述光固化低聚物。 \n[0014] 具体的，所述步骤(1)中聚醚胺与三(2‑羟乙基)异氰脲酸三丙烯酸酯的摩尔比为1：2。 \n[0015] 具体的，所述步骤(2)中羟乙基丙烯酸酯与异佛尔酮二异氰酸酯的摩尔比为1：1。[0016] 具体的，所述步骤(1)和步骤(2)所得产物的摩尔比为1：1。 \n[0017] 本发明还提供一种光固化涂料，包含上述光固化低聚物 $50\\sim70\\$ 份、丙烯酸酯单体$10\\sim20$ 份、光引发剂 $2\\sim5$ 份、助剂 $1\\sim2$ 份、溶剂 $14\\sim27$ 份。 \n[0018] 具体的，丙烯酸酯单体为1,6己二醇二丙烯酸酯(HDDA)、三羟甲基丙烷三丙烯酸酯(TMPTA)、二丙二醇二丙烯酸酯(DPGDA)中的一种或多种。 \n[0019] 具体的，光引发剂为2‑羟基‑2‑甲基‑1‑苯基丙酮(1173)，1‑羟基环己基苯基甲酮(184)，2,4,6‑三甲基苯甲酰基‑二苯基氧化膦(TPO)中的一种或多种。 \n[0020] 具体的，助剂为流平剂、消泡剂、增稠剂、分散剂、润湿剂中的一种或多种。 \n[0021] 具体的，溶剂为乙醇、异丙醇、乙酸乙酯、乙酸丁酯、丙二醇甲醚中的一种或多种。[0022] \n\n本发明与现有技术相比，本发明具有如下的有益效果： \n\n[0023] 1、低聚物具有低黏度、高速固化、有特殊功能等优点，光固化配方的基体树脂，构成固化产品的基本骨架，即固化后产品的基本性能(硬度、柔韧性、附着力、光学性能、耐老化等)主要由低聚物树脂决定。针对部分基材难以附着的特点，设计合成了新型的高PMMA、聚砜、聚苯乙烯附着力的光固化低聚物，通过对表面张力，基材的渗透溶胀、官能度设计从而增强涂层在基材的附着力，同时光固化低聚物含有多种基团增强附着力。可应用在难附着基材的防雾、防污、减阻、润湿等领域。 \n\n[0024] 2、本发明的光固化低聚物结合其他光固化单体可以形成交联的互穿网络，提高涂层硬度、机械强度，可锁住表面活性剂，延长防雾耐久时间。",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 9,
|
||||
"chunk": "# 附图说明 \n\n[0025] 图1实施例1所得可光固化低聚物B1H NMR谱图； \n[0026] 图2实施例1所得可光固化低聚物B FTIR谱图。",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 10,
|
||||
"chunk": "# 具体实施方式 \n\n[0027] 下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明，但不以任何形式限制本发明。应当指出的是，对本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进。这些都属于本发明的保护范围。 \n\n[0028] 实施例1光固化低聚物的制备1 \n\n[0029] 将1mol聚醚胺(ED2003)与2mol三(2‑羟乙基)异氰脲酸三丙烯酸酯(THEICTA)在60℃下反应4h，将1mol羟乙基丙烯酸酯(HEA)与1mol异佛尔酮二异氰酸酯(IPDI)在 $30^{\\circ}\\mathrm{C}$ 下反应0.5h，将两步反应所得产物在 $30^{\\circ}\\mathrm{C}$ 下反应0.5h得到光固化低聚物B。 \n\n[0030] 实施例2光固化低聚物的制备2 \n\n[0031] 将1mol聚醚胺(ED2003)与2mol三(2‑羟乙基)异氰脲酸三丙烯酸酯(THEICTA)在80℃下反应4h，将1mol羟乙基丙烯酸酯(HEA)与1mol异佛尔酮二异氰酸酯(IPDI)在 $50^{\\circ}\\mathrm{C}$ 下反应1h，将两步反应所得产物在 $50^{\\circ}\\mathrm{C}$ 下反应1h得到光固化低聚物B。 \n\n[0032] 实施例3光固化低聚物的制备3 \n\n[0033] 将1mol聚醚胺(ED2003)与2mol三(2‑羟乙基)异氰脲酸三丙烯酸酯(THEICTA)在70$\\mathrm{{^\\circC}}$ 下反应4h，将1mol羟乙基丙烯酸酯(HEA)与1mol异佛尔酮二异氰酸酯(IPDI)在 $50^{\\circ}\\mathrm{C}$ 下反应1h，将两步反应所得产物在 $40^{\\circ}\\mathrm{C}$ 下反应1h得到光固化低聚物B。 \n\n[0034] 实施例3光固化低聚物的测试结果 \n\n[0035] 以氘代氯仿为溶剂，将实施例1制备的可光固化低聚物B溶解，在布鲁克400MHz核磁共振NMR波谱仪测试1H NMR，如图2所示。其在5.5‑6.5ppm之间的峰为 $\\mathrm{CH2=}$ CH‑的特征峰，4.2ppm左右的峰为O‑CH2‑CH2‑O链段的特征峰，分子式中所有的氢的峰都能与谱图中的峰相对应，鉴定结构为可光固化低聚物B。 \n\n[0036] 将实施例1制备的可光固化低聚物B测试红外光谱(FITR)，其谱图如图2所示。上述结构谱图中丙烯酸酯、脲基、聚乙二醇链段峰都在谱图中呈现，红外谱图与可光固化低聚物B结构相符。 \n\n[0037] 实施例4光固化低聚物的应用及效果[0038] 本发明将实施例1所得50份低聚物与20份丙烯酸酯单体HDDA、3份光引发剂1173、2份流平剂与消泡剂、25份乙醇、乙酸乙酯混合溶剂进行复配，可制备紫外光固化防雾涂料组合物，该涂料可在聚砜塑料基材上制备超亲水涂层。该涂层具有良好的防雾、防污、减阻、润湿等效果，且涂层附着力好、不易脱落、硬度高、耐久性好。 \n\n[0039] 实施例5光固化低聚物的应用及效果[0040] 本发明将实施例2所得60份低聚物与10份丙烯酸酯单体TMPTA、2份光引发剂184、1份增稠剂与分散剂、27份异丙醇、乙酸丁酯混合溶剂等进行复配，可制备紫外光固化防雾涂料组合物，该涂料可在PMMA塑料基材上制备超亲水涂层。该涂层具有良好的防雾、防污、减阻、润湿等效果，且涂层附着力好、不易脱落、硬度高、耐久性好。 \n\n[0041] 实施例6光固化低聚物的应用及效果[0042] 本发明将实施例3所得70份低聚物与常规的10份丙烯酸酯单体DPGDA、5份光引发剂TPO、1份润湿剂、14份丙二醇甲醚溶剂进行复配，可制备紫外光固化防雾涂料组合物，该涂料可在聚苯乙烯塑料基材上制备超亲水涂层。该涂层具有良好的防雾、防污、减阻、润湿等效果，且涂层附着力好、不易脱落、硬度高、耐久性好。 \n\n \n图1 \n\n \n图2",
|
||||
"category": " Materials and methods"
|
||||
}
|
||||
]
|
||||
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task2/task2-chunks/ChemDFMг║╗п╤з┴ь╙Є╡─┤є╨═╙я╤╘╗∙┤б─г╨═.json
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217
task2/task2-chunks/ChemDFMг║╗п╤з┴ь╙Є╡─┤є╨═╙я╤╘╗∙┤б─г╨═.json
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task2/task2-chunks/Corkuna Introduction.json
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217
task2/task2-chunks/Corkuna Introduction.json
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@@ -0,0 +1,217 @@
|
||||
[
|
||||
{
|
||||
"id": 1,
|
||||
"chunk": "# Corkuna Introduction",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 2,
|
||||
"chunk": "# Agenda \n\n \n\nCompany Introduction \n\nNano coating technology roadmap and application \n\nProduct Introduction (BEK/VCN)",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 3,
|
||||
"chunk": "# Corkuna Facility",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 4,
|
||||
"chunk": "# Background \n\n",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 5,
|
||||
"chunk": "# Waterproof is a solid need for the electronics \n\n \nCell Phone \n\n \nWearable \n\n \nEarphone \n\n \nUnmanned aerial vehicle \n\n \nAutomotive",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 6,
|
||||
"chunk": "# Background|Waterproof market analysis \n\nAT-RISK SYSTEMS MARKET \nTOTAL: 1,150Bn \n\n \nTOTAL: \\$950Bn \n\n<html><body><table><tr><td>System</td><td>CAAGR 2017-2022</td></tr><tr><td>Personal Computing</td><td>-1.1%</td></tr><tr><td>Other Computing/Infra.</td><td>8.4%</td></tr><tr><td>MobilePhones</td><td>2.5%</td></tr><tr><td>Communications Infra.</td><td>7.4%</td></tr><tr><td>Consumer</td><td>7.6%</td></tr><tr><td>Automotive</td><td>6.3%</td></tr><tr><td>Industrial</td><td>5.7%</td></tr><tr><td>Medical</td><td>3.7%</td></tr><tr><td>Military/Aerospace</td><td>5.2%</td></tr><tr><td>Total</td><td>3.9%</td></tr></table></body></html>\n\nN318.17 5jd-rugg ed",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 7,
|
||||
"chunk": "# Our Timeline \n\n \n\ngeneration coating product with 2 components and more features planned. \n\nBEK series launched.",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 8,
|
||||
"chunk": "# Company Introduction \n\nCorkuna HQ (SH) \n\nR&D/Production Center \n\nSales Office \n\nVietnam Office (CQ1 2020) \n\nOversea office-CUPT (on going) \n\n",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 9,
|
||||
"chunk": "# Company Introduction| Core Technical Team \n\n",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 10,
|
||||
"chunk": "# Technical Roadmap \n\n",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 11,
|
||||
"chunk": "# Core Technology \n\n",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 12,
|
||||
"chunk": "# Molecular Design & synthesis \n\nCoating chemicals molecular Coating structure Molecular self assembly \n\n \n\nCoating Chemicals Lean Production \n\nManufacture under inert protection Package under inert protection \n\n \n\nRecipe Design & Formulation \n\n$\\spadesuit.$ Synergistic technology $\\spadesuit$ Chemical interface modification \n\n",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 13,
|
||||
"chunk": "# Coating Process Design \n\n$\\spadesuit$ Surface treatment $\\spadesuit$ Spray/Dispensing $\\spadesuit$ Automation",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 14,
|
||||
"chunk": "# Application background| Development and Trend",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 15,
|
||||
"chunk": "# Electronics W/P market Share trend in 2022 \n\n \nElectronics W/P market Share in 2017",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 16,
|
||||
"chunk": "# W/P Application Category \n\n",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 17,
|
||||
"chunk": "# Mechanical protection \n\n• Semipermeable vents, cover, foam tape, rubber sealing, etc. • Easy to design and easy to use \n\n \n\nBarrier for smaller and more delicate structural design. Not fully waterproof.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 18,
|
||||
"chunk": "# Potting \n\n• Direct filling on interior PCB boards, etc. • Complete sealing and protection. \n\n \n\nHard for repairing. \nHeat spreading problems.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 19,
|
||||
"chunk": "# PCB board surface conformal coating \n\n• Direct coating on PCB board. \nComplete coverage. \nSaves space for structural design. \nGood for heat spreading. \n\n",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 20,
|
||||
"chunk": "# Conformal Coating Category \n\n",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 21,
|
||||
"chunk": "# Waterproof paint layer \n\nSpecial paint with waterproof feature Easy to apply. Lower in cost. \n\n \n\nOnly provides a covering layer with basic $w/p$ function. Not complete W/P Rubber-based. Not solvent free",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 22,
|
||||
"chunk": "# Nano Coating Layer \n\nVery thin layer of specially designed molecules coated on PCB \nApplied with glue dispenser/PVD/CVD, etc. \nVery good water and grease proof feature with functional molecule designing. \nEnvironmental-friendly.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 23,
|
||||
"chunk": "# Application |PCB Nano Coating \n\n \n\nWater/salt/dust/grease proof. \n\nHard surface substrate for protection. \n\nFill the gaps and fissures. \n\n \n\n\\*Notice: if on FPC board coating may be required to withstand some shape changing $\\mid\\rightarrow$ flexibility features also recommended. \n\n",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 24,
|
||||
"chunk": "# Application| PCB Nano Coating Methods \n\n \n\n \n\n",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 25,
|
||||
"chunk": "# PVD \n\nPhysical vapor deposition. Gasified coating material deposits on the surface forming a very thin protection layer. Higher cost. Longer time. Flexibility cannot be convinced.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 26,
|
||||
"chunk": "# CVD \n\nChemical vapor deposition. Coating layer is formed through deposition (similar to PVD) and chemical reaction on surface. Higher cost. Longer time. Flexibility cannot be convinced.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 27,
|
||||
"chunk": "# Soaking \n\nSoak the PCB board directly in the solution of coating material. \nWith time a protection film will cover the surface. \nEasy, less time but lower coverage \nespecially in small gaps.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 28,
|
||||
"chunk": "# Application| PCB Nano Coating Methods",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 29,
|
||||
"chunk": "# Spraying through dispenser \n\n \n\nEasier and convenient to control the coating evenness, thickness and qty of coating material \nHigh coverage even in gaps and fissures with different spraying angles and spraying pressure adjustment \nShorter time and less cost compared with PVD/CVD. \n\n",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 30,
|
||||
"chunk": "# Application| PCB Nano Coating Methods \n\n",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 31,
|
||||
"chunk": "# Product Introduction | BEK Series \n\n \n\nGood adhesion to PCBs, glass, metal, modified plastic, resin and ceramic. \n\nOne step to use with glue dispenser. \n\nFor general PCB/FPC and module coating. \n\n",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 32,
|
||||
"chunk": "# Product Introduction | BEK Series TDS \n\n \n\n<html><body><table><tr><td colspan=\"2\">Properties of Post Treatment Coating</td></tr><tr><td>Coating thickness</td><td>300nm-15um (in accordance with customer needs)</td></tr><tr><td>Glossiness</td><td>High</td></tr><tr><td>Adhesion Cross-Cut Test</td><td>5B</td></tr><tr><td>Abrasion Test</td><td>5000t - 10oo0t (Depend with the usage and substrates)</td></tr><tr><td>Anti-corrosion in salt solution</td><td>Excellent</td></tr><tr><td>Water Contact Angle (Coated on Glass)</td><td>110° (Depend with the usage and substrates)</td></tr><tr><td>Transmittance % (Coated on Glass)</td><td>93% (Glass=91~92%)</td></tr><tr><td>Fluorescent inspection</td><td>Yes</td></tr><tr><td>Working in water</td><td>Electronic Product, No Shell, Over 60min by coating 5-10g/m² (the lifetime for coated electronics working in Water is depended with the usage. )</td></tr></table></body></html>",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 33,
|
||||
"chunk": "# Product Introduction | VCN L1-B and L2 Combo \n\n \n\nVCN L1-B: better inner structural filling and better flexibility \n\nVCN L2: Repels water and oil on the surface. Also providing hard surface texture \n\nSpecial reaction between groups of L1-B and L2 molecules $\\rightarrow$ strong linking and adhesion. \n\nTwo steps to apply VCN L1-B and L2 on the surface.",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 34,
|
||||
"chunk": "# Product Introduction | VCN L1-B and L2 Combo",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 35,
|
||||
"chunk": "# SEM pictures of VCN L1-B AND l2 layer \n\n \n\n \n\n \n\nThe FESEM picture of VCN L1-B displayed a Hilly-like and porous structures that own the high specific surface area can bond with VCN L2. \n\nThe FESEM picture of VCN L2 displayed a high densely and homogenously structures. \n\nThe FESEM picture of coated VCN L1-B and L2 that displayed the multilayer and high densely structure.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 36,
|
||||
"chunk": "# Product Introduction | VCN L1-B and L2 Combo \n\n",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 37,
|
||||
"chunk": "# Product Introduction | VCN L1-B and L2 Combo TDS \n\n \n\n<html><body><table><tr><td colspan=\"4\">Properties of Post Treatment Coating</td></tr><tr><td rowspan=\"2\">Dielectric Constant</td><td>2.96(@1MHZ)</td><td>1.669(@1MHZ)</td><td></td></tr><tr><td colspan=\"2\">2.97@10kHZ, 2.75@100kHZ, 2.58@1MHZ (Combined)</td><td></td></tr><tr><td>Dielectric Strength (Fully curing)</td><td colspan=\"3\">> 200V/um (Combined)</td></tr><tr><td>Hardness</td><td colspan=\"3\">2-3H (Coated on Glass substrate)</td></tr><tr><td>Surface Resistance (@24 °C Humidity 50%) Water Contact Angle (Coated on Glass)</td><td colspan=\"2\">6.5x1011 @500V (Combined) 106° - 110° (Depend with the usage and substrates)</td><td></td></tr><tr><td>Transmittance % (Coated on Glass)</td><td>86 % (Glass=91%)</td><td>92 % (Glass=91%)</td><td></td></tr><tr><td>Volume Resistivity Ohms, 24 C, 50% RH</td><td></td><td>8.45x1013@500V (Combined)</td><td></td></tr><tr><td>Dissipation Factor</td><td colspan=\"3\">0.01-0.02@10kHZ, 0.016-0.017@100kHZ, 0.017-0.018@1MHZ (Combined)</td></tr></table></body></html>",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 38,
|
||||
"chunk": "# Product Introduction | Salt Mist Comparison \n\n<html><body><table><tr><td colspan=\"5\">Salt mist comparison test result</td></tr><tr><td>Category</td><td>NO coating</td><td>Competitor A</td><td>Competitor B</td><td>VCN coating</td></tr><tr><td>Post 24hrs</td><td></td><td></td><td></td><td></td></tr><tr><td> Post 48hrs</td><td></td><td></td><td></td><td></td></tr><tr><td>Post 72hrs</td><td></td><td></td><td></td><td></td></tr><tr><td>Post 96hrs</td><td></td><td></td><td></td><td></td></tr></table></body></html>",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 39,
|
||||
"chunk": "# Product Introduction | Application Method \n\n \n\nPCB or FPC fixed in clips then put in the convey belt. \n\nPlasma surface cleaning and pretreatment \n\nCoating \n\nCuring in tunnel oven under certain condition \n\nFinished product. Can be checked under UV light.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 40,
|
||||
"chunk": "# Corkuna Facility|Production facility \n\n1. VCN L2 production line \n2. VCN L1-B production line \n3. BEK-04 production line \n4. Auto packing line \n\n \n\n",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 41,
|
||||
"chunk": "# Corkuna Facility|Production facility \n\nFlow velocity adjusting during production. \n\n \n\nCross control material input \n\nSample collection for quality check. \n\nFinished product packing.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 42,
|
||||
"chunk": "# Corkuna Facility | Testing Equipment \n\n",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 43,
|
||||
"chunk": "# Corkuna Facility | Application Equipment \n\n \nHeating chamber \n\nGlue dispenser \n\nLaser Demask",
|
||||
"category": " Materials and methods"
|
||||
}
|
||||
]
|
||||
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187
task2/task2-chunks/HDI╚¤╛█╠х╡─╙ж╙├US9676895B2.json
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187
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@@ -0,0 +1,87 @@
|
||||
[
|
||||
{
|
||||
"id": 1,
|
||||
"chunk": "# Highly transparent superhydrophilic graphene oxide coating for antifogging \n\nXuebing Hu a,b,n, Yun Yu b,nn, Yong Wang b, Yongqing Wang a, Jianer Zhou a, Lixin Song b \n\na Key Laboratory of Inorganic Membrane, Jingdezhen Ceramic Institute, Jingdezhen 333001, China b Key Laboratory of Inorganic Coating Materials, Shanghai Institute of Ceramics, Chinese Academy of Science, Shanghai 201800, China",
|
||||
"category": " Abstract"
|
||||
},
|
||||
{
|
||||
"id": 2,
|
||||
"chunk": "# a r t i c l e i n f o",
|
||||
"category": " Abstract"
|
||||
},
|
||||
{
|
||||
"id": 3,
|
||||
"chunk": "# a b s t r a c t \n\nArticle history: \nReceived 29 March 2016 \nReceived in revised form \n28 June 2016 \nAccepted 29 June 2016 \nAvailable online 30 June 2016 \nKeywords: \nGraphene oxide \nFunctional \nSuperhydrophilic \nTransparent \nAntifogging \nSurfaces \n\nThe superhydrophilic property of the surface allows water to spread completely across the surface rather than remain as droplets, thus making the surface antifogging. In this work, graphene oxide was prepared by the modified Hummers method, and the superhydrophilic and highly transparent functional graphene oxide coating had been fabricated on the glass substrate through a spin coating process. The as-prepared coated glass had a static water contact angle of $3.7^{\\circ}$ and a relatively high transmittance reaching about $76\\%$ throughout the visible region. For comparison, we studied the antifogging properties of the graphene oxide coated glass and the bare glass surfaces. The result shows these glass exhibits absolutely different fogging characteristics, and the graphene oxide coated glass has the superior antifogging property. \n\n$\\circledcirc$ 2016 Elsevier B.V. All rights reserved.",
|
||||
"category": " Abstract"
|
||||
},
|
||||
{
|
||||
"id": 4,
|
||||
"chunk": "# 1. Introduction \n\nThe wettability of solid surface is an attractive topic due to its importance in fundamental research and practical applications [1]. Water vapor can condense on solid surface at a certain temperature or humidity, and water will form little droplets on a solid surface if the surface is poor hydrophilic or hydrophobic. Therefore the light would be refracted and scattered by water droplets so that the transparent materials turn hazy, which causes fogging problem [2]. Endowing the solid surface with excellent wetting characteristic such as superhydrophilicity is a very efficient way to solve the above-mentioned problem [3]. Nowadays, superhydrophilic surface, a special wettability with a water contact angle of less than $5^{\\circ}$ , has received great attention as antifogging coating [4]. Numerous materials, for example, metal oxide $\\mathrm{TiO}_{2}$ , $z_{\\mathrm{{nO}}}$ , $\\mathsf{S n O}_{2}$ and ${\\mathsf{W O}}_{3}$ ) and graphene had been developed for preparing superhydrophilic surface [5–9]. \n\nFollowing the studies on graphene, graphene oxide (GO) has been widely investigated in recent decade, since its many unique and interesting properties such as large external surface area, excellent corrosion-resistant, good antibacterial property, and high mechanical strength, with the advantage of having a simple and inexpensive synthesis process [10,11]. Nowadays, GO based coating can be used for a wide range of applications such as corrosion protection, bacterial growth inhibition, water treatment and so on [12–14]. In particular, due to the presence of various oxygen containing functional groups such as epoxy, hydroxyl and carbonyl groups on its basal planes and edges, GO exhibits hydrophilic property and its wetting ability can be adjusted by the synthesis process [15–17]. However, it is difficult for common graphene oxide coating to be used as superhydrophilic surface material, since the microstructure and functional groups composition of GO coating can not be tailored easily. The previous preparation methods of superhydrophilic GO coating mostly included the complex step of reduction and bridization [18–20]. Therefore, a fast and facile approach for the high optical transmittance and superhydrophilic GO coating fabrication needs to be explored. Especially, due to the above-mentioned intriguing properties of GO, GO based coating has become a very competitive and promising candidate for anti-fogging application. \n\nIn the current work, we present a simple and low-cost method for preparing high performance GO coating on the glass substrate. The coating exhibits superhydrophilicity, superior antifogging property and high optical transmittance throughout the visible region. Our work would greatly simplify the fabrication procedure of high performance GO coating and accelerate its promising applications in industry and daily life, such as mirrors, window glasses, windshields of automobiles, and so on.",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 5,
|
||||
"chunk": "# 2. Experimental procedure",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 6,
|
||||
"chunk": "# 2.1. Materials \n\nMicrocrystalline graphite powders $99.9\\%$ purity) were purchased from Qingdao Sanyuan Graphite Co., Ltd. Potassium permanganate (AR), sodium nitrate (AR), concentrated sulfuric acid (AR, $98\\%$ ), hydrogen peroxide (AR, $30\\mathrm{wt\\%}$ aqueous solution), and quantitative filter paper were purchased from Sinopharm Chemical Reagent Co., Ltd.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 7,
|
||||
"chunk": "# 2.2. Synthesis of GO \n\nGO was prepared using the modified Hummers method [15]. To remove the onus of oxidant and other inorganic impurity, the GO slurry was washed with the deionized water by repeated vacuum filtration through a $100\\mathrm{nm}$ cellulose acetate membrane. Then the suspension was centrifuged (13,000 rpm for $80\\mathrm{min}_{,}$ ), the supernatant was kept. Finally, the supernatant was diluted with deionized water to a total volume of $200\\mathrm{ml}$ in a $500\\mathrm{ml}$ flask to make a homogeneous GO suspension $(0.2\\mathrm{mg}1^{-1})_{\\cdot}$ ) for storing.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 8,
|
||||
"chunk": "# 2.3. Preparation of GO coating \n\nGO coating was deposited on the glass substrate by a spin coating process. Initially, the substrate was ultrasonically cleaned in ethanol and deionized water. After cleaning, the substrate was dried at $60^{\\circ}\\mathsf C$ for $^{1\\mathrm{h}}$ . Then, the above-mentioned GO suspension was dropped on the glass substrate and spun at $500\\mathrm{rpm}$ for $10s$ and dried at $60^{\\circ}C$ for $^{3\\mathrm{~h~}}$ to enhance the mechanical property of the coating. The other side of glass substrate was operated by the same procedure. Finally, the both sides of glass substrate were covered with GO coating.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 9,
|
||||
"chunk": "# 2.4. Characterization and measurement methods \n\nX-ray diffraction (XRD, D8 ADVANCE, Germany) was recorded on a D/max $2550\\mathrm{V}$ diffractometer with Cu Ka radiation $\\scriptstyle\\lambda=0.1542\\mathrm{nm}$ ). X-ray photoelectron spectroscopy (XPS, MICROLAB 310F, Thermo Scientific, UK) spectra were measured using Mg Ka as the exciting resource. The microstructure of the sample was investigated by Transmission electron microscopy (TEM, JEM200CX, Japan). The morphology of as-prepared GO coating was obtained by field emission scanning electron microscopy (FE-SEM, Hitachi SU8220, Japan). The root mean square (RMS) surface roughness of the GO coating was examined with an atomic force microscope (AFM, Bruker, Germany) operating in the tapping mode. The superhydrophilicity of the sample was evaluated with the water contact angle instrument (SL200B, China) by measuring the static contact angle of the deionized water droplet. The transmittance of the samples was carried out by UV–visible spectrophotometer (UV2310, China) at normal incidence in the wavelength between 300 and ${900}\\mathrm{nm}$ . For examination of antifogging property, a GO coated glass and a bare glass were cooled at ca. $-15^{\\circ}C$ for $^{3\\mathrm{h}}$ in a refrigerator, and then exposed to humid laboratory air (room temperature: $20{-}30^{\\circ}\\mathsf C$ , relative humidity: 20– $40\\%$ .",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 10,
|
||||
"chunk": "# 3. Results and discussion",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 11,
|
||||
"chunk": "# 3.1. XRD patter, XPS spectrum and microstructure of GO \n\nThe XRD pattern of GO is shown in Fig. 1a. GO has a low intensity peak at $11.8^{\\circ}$ , which attributes to the (001) reflection of GO. The C 1s XPS spectrum of GO is presented in Fig. 1b. The spectrum is decomposed into three fitted peaks using a Gaussian function. A binding energy of $284.9\\mathrm{eV}$ indicates the existence of C–C sp2 bonds in GO, while $287.1\\ \\mathrm{eV}$ results from C–O bonds (epoxy and hydroxyl groups), and $288.5\\mathrm{eV}$ shows ${\\mathsf{C}}{=}0$ bonds (carbonyl) are formed during the oxidation process [21]. \n\nThe sp2 carbon (C–C) fraction can characterize the oxidation degree in GO, which can be estimated by dividing the area by C 1s peak area [17]. From Fig. 1b, the C–C fraction of GO is about $46.4\\%$ . The result shows there are fewer C–C groups in GO and also reflects GO has more oxygen-containing functional groups. With the increase of these groups, the hydrophilic property of GO will be enhanced [22]. \n\nThe microstructure of GO is inspected by TEM. From Fig. 1c, the average size of GO nanosheets is about $150\\mathrm{nm}$ and GO has excellent dispersibility.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 12,
|
||||
"chunk": "# 3.2. The surface morphology and wettability of GO coating \n\nThe surface morphology of the GO coating was characterized by FE-SEM and the tapping mode AFM. As shown in Fig. 2a, it indicates some aggregations have been formed due to the larger amount of GO loading, so that the coating surface is not smooth. The cross-section image of GO coating is shown in Fig. 2b, which indicates the thickness of GO coating is about $100\\mathrm{nm}$ As displayed in Fig. 2c, it is also observed the surface of the coating presents some roughness that possibly arises from the random overlap and aggregation of individual GO sheets. The RMS roughness ups to $9.32\\mathrm{nm}$ . \n\nFrom Fig. 2d, the static water contact angle (WCA) of $\\sim3.7^{\\circ}$ is observed for GO coating. The small water contact angle suggests the coating represents the superhydrophilic property. From Fig. 2c, we can know the coating surface has a higher surface roughness. According to Wenzel equation [23]: \n\n \nFig. 1. (a) XRD pattern, (b) XPS spectrum and (c) TEM image of GO. \n\n \nFig. 2. FE-SEM images in (a) top view and (b) cross-sectional view of a GO coating, (c) three-dimensional AFM image, (d) water contact angle of GO coating on the glass substrate. \n\n$$\n\\mathrm{cos\\theta_{w}}=\\gamma\\mathrm{cos\\theta_{e}}\n$$ \n\nwhere $\\uptheta_{\\mathrm{w}}$ is the apparent WCA in Wenzel state, $\\boldsymbol{\\upgamma}$ is the surface roughness factor and $\\uptheta_{\\mathrm{e}}$ is the equilibrium WCA on the horizontal and smooth surface. In the case of a principally hydrophilic surface, a decrease of WCA is predicted following an increase of $\\boldsymbol{\\upgamma}$ . \n\nAs shown in Fig. 2c, it is clear that there are some corrugations on the coating surface and the RMS surface roughness is $9.32\\mathrm{nm}$ . The results indicate the coating has a higher surface roughness so that the value of $\\boldsymbol{\\upgamma}$ increases, which is beneficial to magnify the intrinsic wetting characteristic of the surface. It has also been further confirmed by Fig. 2d.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 13,
|
||||
"chunk": "# 3.3. The transmittance of GO coating \n\nTo evaluate the optical transmission, a comparative test about the transmittance of the bare and GO coated glasses was carried out by UV–visible measurement. \n\nAccording to the UV–visible spectra in Fig. 3, the GO coated glass shows a high transmittance reaching about $76\\%$ , while the transmittance of the bare glass is about $90\\%$ throughout the visible region. It is observed there was a decrease in transmittance with the GO coated, which can be ascribed to the light reflecting and scattering resulting from the surface roughness and the air-coating and the coating-substrate interfaces [24]. \n\nGenerally, the high roughness and high transmittance is a pair of competitive properties due to extensive light scattering [25]. Interestingly, it can be revealed from the above results of experiment that the GO coated glass has a good transmittance with the \n\n \nFig. 3. UV–Vis transmission spectra of GO coated glass and bare glass. \n\nRMS surface roughness ups to $9.32\\:\\mathrm{nm}$ .",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 14,
|
||||
"chunk": "# 3.4. The antifogging of GO coating \n\nWe investigated the antifogging properties of the GO coated glass and the bare glass, as shown in Fig. 4. Both glass samples were cooled at ca. $-15^{\\circ}C$ for $^{3\\mathrm{h}}$ in a refrigerator, and then simultaneously exposed to humid laboratory air. \n\nAs shown in Fig. 4, the bare glass (left) fogged immediately and presented a large amount of tiny condensed droplets causing a significant reduction of the optical transmittance. As a comparison, the GO coated glass (right) remained clear and excellent transparency during the whole antifogging test. Thus, the GO coating should play an active role in antifogging property of glass. This special antifogging ability should be attributed to that the nearly instantaneous spreading of water droplets on the superhydrophilic surface. Thus, water could evaporate soon and the GO coated glass surface was kept clear at all times. \n\n \nFig. 4. Images of the fogging comparison experiment between GO coated glass and bare glass after cooling.",
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"category": " Results and discussion"
|
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},
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{
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"id": 15,
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"chunk": "# 4. Conclusion \n\nWe presented a facile route to fabricate highly transparent superhydrophilic GO coating on glass substrate. The resultant superhydrophilic surface shows a static water contact angle of $3.7^{\\circ}$ and a transmittance reaching about $76\\%$ throughout the visible region. We also discussed the antifogging characteristic of GO coated glass and bare glass, the result demonstrates the GO coated glass has a superior antifogging property.",
|
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"category": " Conclusions"
|
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},
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{
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"id": 16,
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"chunk": "# Acknowledgements \n\nThe authors gratefully acknowledge the support of this research by the National Natural Science Foundation of China (Grant No. 51262012) and the Foundation of Jiangxi Science and Technology Committee (Grant Nos. 20133ACB20007 and 20161ACB21008). The project also was funded by the Key Laboratory of Inorganic Coating Materials, Chinese Academy of Sciences (Grant No. KLICM-2014-07).",
|
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"category": " References"
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||||
},
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{
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"id": 17,
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||||
"chunk": "# References \n\n[1] Z. Pan, J.A. Weibel, S.V. Garimella, Influence of surface wettability on transport mechanisms governing water droplet evaporation, Langmuir 30 (2014) \n\n9726–9730. [2] Y. Yuan, R. Liu, C. Wang, J. Luo, X. Liu, Synthesis of UV-curable acrylate polymer containing sulfonic groups for anti-fog coatings, Prog. Org. Coat. 77 (2014) 785–789. [3] X. Li, B. Shi, M. Li, L. Mao, Synthesis of highly ordered alkyl-functionalized mesoporous silica by co-condensation method and applications in surface coating with superhydrophilic/antifogging properties, J. Porous Mater. 22 (2015) 201–210. [4] P. Chen, Y. Hu, C. Wei, Preparation of superhydrophilic mesoporous $\\mathrm{SiO}_{2}$ thin films, Appl. Surf. Sci. 258 (2012) 4334–4338. [5] R. Dong, S. Jiang, Z. Li, Z. Chen, H. Zhang, C. Jin, Superhydrophilic $\\mathrm{TiO}_{2}$ nanorod films with variable morphology grown on different substrates, Mater. Lett. 152 (2015) 151–154. [6] J. Li, L. Yan, W. Li, J. Li, F. Zha, Z. Lei, Superhydrophilic-underwater superoleophobic ZnO-based coated mesh for highly efficient oil and water separation, Mater. Lett. 153 (2015) 62–65. [7] K. Yadav, B.R. Mehta, K.V. Lakshmi, S. Bhattacharya, J.P. Singh, Tuning the wettability of indium oxide nanowires from superhydrophobic to nearly superhydrophilic: effect of oxygen-related defects, J. Phys. Chem. C 119 (2015) 16026–16032. [8] A. Srinivasan, M. Miyauchi, Chemically stable ${\\sf W O}_{3}$ based thin-film for visiblelight induced oxidation and superhydrophilicity, J. Phys. Chem. C 116 (2012) 15421–15426. [9] J. Rafiee, M.A. Rafiee, Z.Z. Yu, N. Koratkar, Superhydrophobic to superhydrophilic wetting control in graphene films, Adv. Mater. 22 (2010) 2151–2154. \n[10] Y. Gao, C. Qin, Z. Qiao, B. Wang, W. Li, G. Zhang, R. Chen, L. Xiao, S. Jia, Imaging and spectrum of monolayer graphene oxide in external electric field, Carbon 93 (2015) 843–850. \n[11] D.R. Dreyer, A.D. Todd, C.W. Bielawski, Harnessing the chemistry of graphene oxide, Chem. Soc. Rev. 43 (2014) 5288–5301. \n[12] R.K. Upadhyay, N. Soin, G. Bhattacharya, S. Saha, A. Barman, S.S. Roy, Grape extract assisted green synthesis of reduced graphene oxide for water treatment application, Mater. Lett. 160 (2015) 355–358. \n[13] K. Krishnamoorthy, A. Ramadoss, S.J. Kim, Graphene oxide nanosheets for corrosion-inhibiting coating, Sci. Adv. Mater. 5 (2013) 406–410. \n[14] J.H. Park, J.M. Park, Electrophoretic deposition of graphene oxide on mild carbon steel for anti-corrosion application, Surf. Coat. Technol. 254 (2014) 167–174. \n[15] X.B. Hu, Y. Yu, W.M. Hou, J.E. Zhou, L. Song, Effects of particle size and pH value on the hydrophilicity of graphene oxide, Appl. Surf. Sci. 273 (2013) 118–121. \n[16] R. Rasuli, Z. Mokarian, R. Karimi, H. Shabanzadeh, Y. Abedini, Wettability modification of graphene oxide by removal of carboxyl functional groups using non-thermal effects of microwave, Thin Solid Films 589 (2015) 364–368. \n[17] X.B. Hu, Y. Yu, J.E. Zhou, L. Song, Effect of graphite precursor on oxidation degree, hydrophilicity and microstructure of graphene oxide, Nano 9 (2014) 1450037. \n[18] H. Zanin, E. Saito, H.J. Ceragioli, V. Baranauskas, E.J. Corat, Reduced graphene oxide and vertically aligned carbon nanotubes superhydrophilic films for supercapacitors devices, Mater. Res. Bull. 49 (2014) 487–493. \n[19] L. Kou, C. Gao, Making silica nanoparticle-covered graphene oxide nanohybrids as general building blocks for large-area superhydrophilic coatings, Nanoscale 3 (2011) 519–528. \n[20] H. Zanin, E. Saito, F.R. Marciano, H.J. Ceragioli, A.E.C. Granato, M. Porcionatto, Fast preparation of nano-hydroxyapatite/superhydrophilic reduced graphene oxide composites for bioactive applications, J. Mater. Chem. B 1 (2013) 4947–4955. \n[21] T. Kuila, S. Bose, P. Khanra, A.K. Mishra, N.H. Kim, J.H. Lee, A green approach for the reduction of graphene oxide by wild carrot root, Carbon 50 (2012) 914–921. \n[22] J. Chen, B. Yao, C. Li, G. Shi, An improved Hummers method for eco-friendly synthesis of graphene oxide, Carbon 64 (2013) 225–229. \n[23] V. Tamilselvan, D. Yuvaraj, R.R. Kumar, K.N. Rao, Growth of rutile $\\mathrm{TiO}_{2}$ nanorods on $\\mathrm{TiO}_{2}$ seed layer deposited by electron beam evaporation, Appl. Surf. Sci. 258 (2012) 4283–4287. \n[24] J. Bravo, L. Zhai, Z. Wu, R.E. Cohen, M.F. Rubner, Transparent Superhydrophobic films based on silica nanoparticles, Langmuir 23 (2007) 7293–7298. \n[25] Y.H. Lin, K.L. Su, P.S. Tsai, F.L. Chuang, Y.M. Yang, Fabrication and characterization of transparent superhydrophilic/superhydrophobic silica nanoparticulate thin films, Thin Solid Films 519 (2011) 5450–5455.",
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"category": "e to analyze the text segment as it appears to reference an image link, which I cannot access or interpret. If you can provide the text segment directly, I'd be happy to help classify it based on the categories provided."
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"chunk": "# Dr.R.Lomolder Mr.F.Plogmann Mr.P.Speier \n\n摘要：在一项针对异佛尔酮二异氰酸酯(IPDI)于氨基甲酸酯反应中的选择性之模型研究中,提示了催化剂类型和温度的影响。同时通过选择伯丁醇和仲丁醇作为反应对象,介绍了羟基类型的影响。 \n\n需特别指出的是，催化剂的选择对最终产品的组成有着极重大的影响。模型研究的最重要结论在NCO预聚物的合成中得到了肯定。",
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"category": " Abstract"
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},
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{
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"id": 3,
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"chunk": "# The influence of temperature,catalyst and coreagent on reactivity of two isocyanate group in isophorone diisocyanate \n\nAbstract:In a model study for the reactivity of two isocyanate groups of isophorone disocyanate,it reveals the influence of temperature and catalyst in urethane reaction.Using primary and secondary butanol as coreagent the article decribes the influence on type of hydroxy group.It is emphasized that the selection of catalyst has great influence on the composition of final product.In NCO prepolymer synthesis the most important conclusion of this model study is confirmed.",
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"category": " Abstract"
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},
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{
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"id": 4,
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"chunk": "# 1概论 \n\n异佛尔酮二异氰酸酯(IPDI)(图1)是在世界范围内制备光稳定性氨基甲酸酯改性涂料用树脂的首选脂环族二异氰酸酯。所能制备的树脂包括PU分散体、氨酯改性醇酸、辐射固化氨基甲酸酯丙烯酸酯和潮气固化异氰酸酯预聚物。除其与众多的共反应物和溶剂有着极广泛的相容性外，本品用途之所以日益得到扩展的主要原因之一是，一个在脂肪族伯位上与一个在脂环族仲位上的IP-DI的两个异氰酸酯基团反应活性不相等。这种不相等所造成的结果是：最终产品粘度低；分子量分布窄；游离的二异氰酸酯单体含量小。过去，IPDI在反应活性上的这种差别曾是探讨的课题。根据对差别成因所作出的许多假设，根据化学计算，反应对象以及根据所采取的试验方法和对试验的解释，人们得到了这样的结果：真有不同反应活性的NCO基团的活性差在0.2:1-12:1的范围内。 \n\n本项研究中的内容包括：在氨基甲酸酯反应中各种催化剂、温度（在所有以前的研究中温度被设定为常数)、位阻和/或醇类的反应活性对模型反应的选择性影响以及其对工业中可予实践体系的适用性。 \n\n与取代基在环己烷上可能的定向相呼应，IPDI分化为顺式(Z)和反式(E)异构体。工业级的IPDI是异构体的混合物，异构体的比例大致为75:25,以顺式(Z)为主。 (图2) \n\n \n图1异佛尔酮二异氰酸酯 \n\n \n图2顺式/反式IPDI异构体 \n\nIPDI与醇类的反应可以以四个速率常数(K1-K4)予以完全的表达。这个常数是与IPDI异构体中每一个异构体上的两个不相等的NCO基(伯/仲)相呼应的。合计起来，要加以考虑的有八个速率常数和八个产物（图3)。对这个非常复杂的体系可以按照其反应速率给予某种清楚明显的简化来加以处理。 \n\n \n图3IPDI与醇类反应的速率常数 \n\n假设：（a）单氨基甲酸酯单异氰酸酯的氨基甲酸酯官能团对残余异氰酸酯基的反应活性既无催化剂性质、也无阻遇性质的影响；（b）顺式和反式IPDI具有可比的反应活性。 \n\n根据以上假设，图3已被简化成为两个速率常数和四个产物的体系(图4)。 \n\n万万数据 \n\n \n图4IPDI的氨基甲酸酯反应的简化动力学模型[K(顺) ${\\bf\\Pi}={\\bf K}$ （反）] \n\n在一个异氰酸酯处于过量状态，异氰酸酯转化率为已知的体系中，按照Peebles的说法，速率常数的比例可以通过最终产出混合物的游离单体含量来加以确定。按一个非对称的例子所进行的计算，一个计算量为2：1的 $\\boldsymbol{\\mathrm{NCO}}/\\mathrm{~OH~}$ 反应其二异氰酸酯转化率与K1和K2的商I之间产生了一定的相关性。",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 5,
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||||
"chunk": "# 2试验部分 \n\n模型反应不用溶剂，是在一个有搅拌的反应器中，在氮气保护下恒温进行。将赫斯公司（Huels AG）的VESTANATIPDI和催化剂加人反应器中，将醇在5h内滴加完。化学计算量为 $\\mathbf{NCO}{:}0\\mathbf{H}=2{:}1_{\\circ}$ 反应持续进行到转化完全为止。以十四碳烷为标准进行凝胶色谱分析以测定其单体含量。在反应中使用1-丁醇，使我们有可能解析IPDI四个单氨基甲酸酯和1－丁醇。所用的1－丁醇和2-丁醇都含有 $<0.2\\%$ 的水，多元醇 $<0.5\\%$ 。水含量是按Karl-Fischer法测定的。叔胺类催化剂是由Aldrich提供；DBTL（二月桂酸二丁基锡)由Elf-Atochem提供;辛酸锌溶解在石油溶剂中，石油溶剂中脂肪族对芳香族的比例为80：20，锌含量为 $8\\%$ ，由Borchers 公司提供。乙酰乙酸铁（FeAcAc）由赫斯公司提供；催化剂Coscat83( $16\\%$ 秘）由Caschem公司提供。",
|
||||
"category": " Materials and methods"
|
||||
},
|
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{
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"id": 6,
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"chunk": "# 3结果和讨论",
|
||||
"category": " Results and discussion"
|
||||
},
|
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{
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"id": 7,
|
||||
"chunk": "# 3.1应用各种氨基甲酸酯催化剂时的.IPDI",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 8,
|
||||
"chunk": "# 选择性 \n\n金属类催化剂（路易氏酸）以及叔胺类催化剂（路易氏碱）在氨基甲酸酯化学中是人所熟知的。表1所示为IPDI/1－丁醇反应的结果，这个反应是在 $\\tt N C O/O H$ 化学计算量2:1的条件下和 $20\\%$ 的温度下进行的。反应使用了 $\\smash{\\mathsf{S n}_{\\searrow}Z_{\\mathbf{n}_{2}}}$ Fe和Bi催化剂，用量按恒定的金属原子／离子浓度确定。实验还使用了四种叔胺催化剂，二氮杂双环[2.2.2]辛烷(DABCO)1,8二氮杂双环－[5.4.0]－十-—烯－7(DBU)，N，N－二甲基环己基胺(DMCA)和1,5-二氮杂一环[2.3.0]壬烯－5(DBN)，四者均按IPDI体系的典型浓度$0.4\\%$ (DBU为 $0.2\\%$ )的量使用。未催化体系亦列出以供参考(表1)。 \n\n表1催化剂对IPDI与1-丁醇的氨基甲酸酯反应的影响 \n\n\n<html><body><table><tr><td>催化剂</td><td>T= k1/k2 完全转化时间</td></tr><tr><td>无</td><td>5.5 8d</td></tr><tr><td>DBTL(0.075%)</td><td>11.5 6h</td></tr><tr><td>辛酸锌(0.42%)</td><td>7 IdX.</td></tr><tr><td>Bi催化剂(0.135%)</td><td>2.5 6h</td></tr><tr><td>FelILAcAc(0.042% )</td><td>5.5 6h</td></tr><tr><td>DABCO(0.4%)</td><td>0.18 1dX.</td></tr><tr><td>DBU(0.2%)</td><td>5.5 同上</td></tr><tr><td>DMCA(0.4%)</td><td>4.4 同上</td></tr><tr><td>DBN(0.4% )</td><td>6.2 3d</td></tr></table></body></html>\n\n$\\mathrm{X}_{\\mathsf{I}}:>6\\mathrm{h},<24\\mathrm{h}$ 条件： $\\mathbf{\\widetilde{NCO}:O H}=2:1,20\\mathbf{\\widetilde{C}}$ \n\n催化的效果是明显的，这是共性。除此之外，催化剂的有效性也存在着差别。除Zn催化体系外，所有的金属催化均比叔胺催化更为有效。令人惊异的是所使用的催化剂类型的选择性。DBTL是本项研究中最具选择性的催化剂。未催化体系的I值为5.5，而对DBTL来说却达到了11.5。就叔胺类而言，DABCO造成了选择性的逆转，而所有其它叔胺类，则未显示出明显的影响。 \n\nDBTL催化剂使选择性显著增加的情形 \n\nHatada和Pappas也曾提及。他们用氢’和碳技术进行核磁共振测定证实，当以DBTL催化时，脂环族仲NCO基无疑更为活泼。很明显，伯NCO基被 $\\beta$ 基取代物、环己烷和与之相邻的甲基有效的遮蔽起来了。 \n\n金属催化之所以使选择性增加的原因可以通过考察这些催化剂的机制找到；金属以路易氏酸的形式发挥作用并通过对羧基的配置而使异氰酸酯基得到活化。活化转变状态对额外空间的需求是导致已经很活泼并且位阻也较小的NCO基优先得到催化的原因。 \n\n叔胺类催化氨基甲酸酯反应主要是通过活化醇的羟基之途径而实现的，但其对NCO基团的活化问题也有人进行过讨论。通过OH基的活化，活化转变状态所要求的空间比使用金属催化剂时的要求要小些。这应该是胺类催化剂没有额外选择性的原因。除DABCO外，叔胺类对IPDI的选择性没有明显的影响。很有意思的是，DABCO所造成的选择性逆转使伯NCO基变得更为活泼。一个可能的解释是，DABCO－1-丁醇络合物的残余游离叔胺官能被更为活泼的仲NCO基所预配位化。通过重组为分子内的大环，活化OH基可以指向伯NCO基。",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 9,
|
||||
"chunk": "# 3.2温度对IPDI选择性的影响 \n\n已发表对IPDI选择性问题的研究报告均以温度作为一个常数。为了显示温度的影响，作为一个例子，对未催化的体系和使用具有非同寻常催化效果的DBTL的体系进行了研究目的是在 $20-100\\mathrm{\\PhiC}$ 范围内确定温度对选择性的影响。产物的粘度被作为体系更深入的参数。 \n\n对于一个未催化而在 $20-100\\mathrm{\\textperthousand}$ 进行的IPDI/正丁醇（NCO： $\\mathbf{OH}=2\\colon1\\rangle$ 之氨基甲酸酯反应 ${\\boldsymbol\\Gamma}$ 进程和产物粘度来说，如所预期的，随着温度的增加，选择性从 ${\\pmb5.5}(20{\\pmb\\mathrm{\\qquade}})$ ）向反方向变化为 $3.9(100^{\\circ}\\mathrm{C})$ 。较低的选择性导致了二氨基甲酸酯比例增加和粘度的相应增长。在进行未催化树脂合成时，从对粘度和经济性因素( $100\\%$ 的转化在 $20\\%$ 需要8d，而在 $80\\%$ 仅需 $\\boldsymbol{6\\mathrm{h}}$ ）的考虑出发， $60-80\\mathcal{\\mathbf{C}}$ 的温度范围似乎是最佳的。 \n\n \n图5IPDI与1-丁醇在氨基甲酸酯反应中使用DBTL催化剂 $0.075\\%$ ） $(\\mathbf{NCO}:\\mathbf{OH}=\\mathbf{2}:\\mathbf{1}_{i}^{\\cdot}$ .IPDI的选择性和最终产物粘度 \n\n图5清楚地显示，DBTL具有更高的选择性，对温度的依赖比未催化体系也更强。然而，在 $100\\%$ 的选择性高于未催化反应在$20\\%$ 时的选择性。有趣的是，产出混合物的粘度在直到 $80\\%$ 温度下几乎保持恒定。对于未催化体系来说，其粘度会随着二氨基甲酸酯浓度提高而有所增加，这是可以预期的。很明显，在产物组成的系列中，包括有单体、单氨基甲酸酯和二氨基甲酸酯。因二氨基甲酸酯含量提高而带来的粘度提高效应会被较高的单体浓度所带来的粘度降低效应所抵销。让人奇怪的是在 $80-100\\mathrm{^c}$ 之间观察到粘度有急剧提高的现象。SFC法确认了在$100\\%$ 的反应混合物中存在有 $2\\%$ 的高分子量组成，这或者是从二氨基甲酸酯得来的脲基甲酸酯或者是IPDI的单异氰酸酯。 \n\n基于在 $40-60\\%$ 范围内的副产物以及万方数据 \n\nDBTL催化后明显的选择性，可得出的结论是，工业性IPDI氨基甲酸酯反应以在此温度范围内实施为宜，且应选择催化体系。 \n\n以凝胶色谱技术对四个单氨基甲酸酯进行分离，就可以以IPDI与1-丁醇的DBTL催化反应温度为函数来显示出顺式和反式IPDI的选择性。关于仲对伯单氨基甲酸酯的比例显示了顺式和反式IPDI的选择性问题，如所预期的，两种异构体都随着温度的提高而表现出选择性下降的情性。反式异构体的选择性明显较高（在 $40-100\\mathrm{\\textperthousand}$ 温度下系数约为2),额外的位阻为2-丁醇。 \n\n为弹性体市场生产的异氰酸酯预聚物通常是以仲OH基占优势的聚丙二醇为基础。因此，把对选择性的研究进一步扩展到位阻更大、而反应性较弱的2-丁醇，则是引起人们兴趣的事。在图6中，就IPDI与1-丁醇和2－丁醇在DBTL催化下的反应对温度的依赖关系作了比较。 \n\n据推测，因2－丁醇的使用致使出现对额外空间的需求，使IPDI的选择性有了进一步的增加。在 $20\\%$ 下的速率常数之比为17,作为比较的数据是使用1－丁醇时的11.5(DBTL)和5.5(未催化)。使用2-丁醇时，在$80\\mathbf{\\%}$ 的转化比使用1－丁醇在 $20\\mathbf{\\%}$ 的转化更具选择性，两条曲线均为平行走向，这意味着选择性对温度的依赖就两者而言是类似的。 \n\n在此项研究中所选用的气相色谱不能把反式IPDI的单异氰酸酯和2-丁醇分离出来。在与2-丁醇的反应中，顺式异构体的选择性增加到了反式异构体与1-丁醇反应时的水平（ $20\\%$ 仲单异氰酸酯／伯单异氰酸酯$\\begin{array}{r l r}{\\mathrm{~}}&{{}}&{=30.1/1\\dot{\\mathrm{~,~}}}\\end{array}$",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 10,
|
||||
"chunk": "# 3.3 回到实践中：NCO预聚物 \n\n用于潮气固化涂料的IPDI预聚物一般是由分子量分布在500－3000之间、含2－3羟基官能团的聚合物所制备，按化学计算量，NCO: $\\mathbf{OH}=1.8\\colon1$ 到2：1。为了说明使用1-丁醇和2-丁醇模型体系结果的适用性，IPDI是与四种不同的多元醇按2：1化学计算量反应的。所使用的多元醇有线型NPG(新戊二醇)，己二酸酯，分子量差不多的聚（四次甲基二醇）醚和聚（丙二醇）醚以及一种分子量为540的三官能聚己酸内酯，后者是以 $75\\%1-$ 甲氧丙基-2-醋酸酯(MOP醋酸酯)溶液的形式使用的(表2)。 \n\n表2基于各种多元醇的IPDI预聚物 \n\n\n<html><body><table><tr><td></td><td></td><td>预聚物</td><td></td></tr><tr><td></td><td>A B</td><td>C</td><td>D</td></tr><tr><td>基础</td><td>聚酯 P - THF</td><td>PPG</td><td>聚己内酯</td></tr><tr><td>多元醇分子量</td><td>1000 1000</td><td>1000</td><td>540</td></tr><tr><td>官能度</td><td>2 2</td><td>2</td><td>3</td></tr><tr><td>固体含量(%)</td><td>100 100</td><td>100</td><td>(MOP醋酸酯）</td></tr></table></body></html> \n\n表3不同温度下合成预聚物的结果$\\mathbf{\\left\\langleNCO:OH=2:1,DBTL\\right.}-$ 催化剂 $\\mathbf{-0.075\\%}$ \n\n\n<html><body><table><tr><td>A</td><td>B C</td><td>D</td></tr><tr><td>T(℃) 23℃ IPDI 23°℃ Pa·s % Pa·s</td><td>粘度 单体 粘度 单体 粘度 单体 粘度 单体 IPDI 23℃ IPDI % Pa·s % Pa·s</td><td>23℃ IPDI % 4.8 5.0</td></tr><tr><td>20 206 40 216 60 219</td><td>3.9 16.7 4.3 12.2 3.2 4.0 18.7 4.4 12.5 3.3 4.1 19.1 4.4 13.0 3.6</td><td>3.4 4.2 4.2 5.2</td></tr><tr><td>100 264</td><td>4.3 22.8 4.5 16.0 3.7</td><td>4.3 6.5</td></tr><tr><td>80,无 284 催化剂</td><td>6.3 27.2 6.0 15.0 5.7</td><td>5.6 8.8</td></tr></table></body></html> \n\n按照Wendish等人的说法，脂环族基团更倾向于一个对等的位置。按照这个说法，反式异构体的NCO基正好处于轴线的对等位置上，比顺式异构体的侧位会有更有效的位阻屏蔽效应。(见图6) \n\n异佛尔酮衍生物的反式异构体伯基团屏蔽性更强，反应性更低的另一效应最近围绕环氧体系而有所报道；在双组分环氧配方中，更多的反式IPDA(异佛尔酮二胺)能使其使用寿命有所延长。 \n\n \n图6IPDI与1-丁醇、2-丁醇在氨基甲酸酯反应中的选择性 $\\mathbf{(NCO:OH=2:1}$ ，DBTL－催化剂 $\\mathbf{\\sigma}=\\mathbf{\\sigma}$ $\\mathbf{0.075\\%}$ ） \n\n表3综合了预聚物合成的结果，包括在各个温度下的催化制备和在 ${\\bf809}\\mathrm{\\overline{{C}}}$ 未经催化制备的结果。这个结果与模型研究的结果非常接近；使用DBTL者，随温度的增加（20-${\\bf60^{\\circ}C}$ ）粘度和单体含量有微小增加；在 $80\\mathbf{\\hat{C}}$ 时反应的未催化体系粘度和单体含量最高。NPG体系在80时所造成的无催化剂反应产物粘度较低 $(15\\mathrm{Pa}.\\mathbf{s})$ ，这似乎令人惊讶，但却与多元醇相对较弱的骨干链热降解可能有关。在 $100\\%$ 催化反应的产物粘度比在${\\bf60^{*}C}$ 反应者显著高出较多，但仍然与模型研究的结果相平行，这与脲基甲酸酯的形成有关。 \n\n在 $100\\%$ 的催化反应与模型研究有显著的偏离。与 ${\\bf60^{\\circ}C}$ 的反应相比，单体含量只有微小的增加(预聚物A-C)。这个结果通过模型与预聚物体系的 ${\\bf\\delta T}$ 对照列于表4中。它表明，IPDI在预聚物合成中更具选择性。由于预聚物与模型体系相比，有着更高的粘度，IPDI单体的扩散更将受到阻碍。这意味着，相当程度的脉基甲酸酯形成作为一个竞争性的反应存在应当予以考虑。这个事实导致最终产物较低的单体含量。这可能被误解为较高的选择性。这种解释因低粘度的 $75\\%$ 预聚物溶液(D体系)而得到了确认。在这个溶液中，在 $100\\%$ 时的单体含量有一个飞跃。 \n\n(下转第49页) \n\n剪切速率粘度。有时候转换供应商也可解决问题。调配基料制造商亦正发展较能与缔合型增稠剂相容的产品。 \n\n流变助剂的副作用跟配方有关，不可能尽列。可以这样说，由于不同系统有不同作用，实验是不可避免的，但通过仔细筛选及咨询供应商，试验工作量可减至最低。",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 11,
|
||||
"chunk": "# 3总结 \n\n选择流变助剂可以分成几个有系统的步骤，把选择范围缩至几个产品，根据这些步骤可以剔除不适合的产品，避免浪费试验时间。 \n\n最重要的也许是确定需要哪一种流动形态，配方设计者必须为最终产品鉴定清晰一 Titiitiitiiti-iit-ititiiiiii-ii（上接第14页） \n\n表4合成预聚物(A一D)与模型反应物(1-丁醇,2-丁醇)的速率常数比 \n\n\n<html><body><table><tr><td colspan=\"2\">r</td></tr><tr><td>T(℃)</td><td>1-丁醇 A B D 2-丁醇</td></tr><tr><td>20,DBTL</td><td>11.5 11.5 10.2 14.5 17.0</td></tr><tr><td>40,DBTL 10.5</td><td>16.5 10.9 9.5 12.9 15.0 15.7</td></tr><tr><td>60,DBTL 9.0</td><td>10.5 9.5 12.0 12.2 12.6</td></tr><tr><td>100,DBTL 6.5</td><td>9.3 9.3 7.2 10.1 12.0</td></tr><tr><td>80,无催化剂 4.1 3.6</td><td>4.3 3.2 3.3 4.3</td></tr></table></body></html> \n\n对预聚物合成和模型反应的I所进行的比较(表4)，本质上已能表现出很好的相关性，不仅是伯羟基／IPDI反应（1-丁醇和A、B、D体系）和仲羟基/IPDI反应（2-丁醇和C体系）的『绝对值如此，而直至 ${\\pmb60}{\\pmb\\Upsilon}$ 时对温度的依赖性以及DBTL催化剂对粘度和单体含量的影响也均如此。 \n\n一般来说，本项研究从粘度、单体含量和经济性角度方面确认了在 $40-60^{\\circ}C$ 温度下使用DBTL催化剂进行IPDI预聚物合成的可行性。",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 12,
|
||||
"chunk": "# 4综述 \n\n异佛尔酮二异氰酸酯(IPDI)在氨基甲酸万方数据 \n\n目标，亦需要明白不同类别助剂的一般特性。供应商提供的产品说明书及数据表上的资料都有帮助，有某些的确是推广的术语，但其中的理论通常都有道理的。配方设计者应花时间阅读，并与供应商讨论具体问题，几分钟的电话时间可以节省几小时的试验工夫。 \n\n三个要点分别是：需要的流动形态、用哪种助溶剂及工厂条件的限制，对有经验的配方设计者这些步骤是显而易见；其他的步骤是微调，只是从几个类似产品中选择一个，在这阶段实验工作是不可避免的。 \n\n显然今天碰到的问题仍需要很多时间解决，但希望循着以上步骤，选择流变助剂在实验室里不再是最花时间的一项。 \n\n酯反应中显示出对温度、催化剂类型和不同反应对象有强烈的依赖性。 \n\n对IPDI的选择性进行的模型研究是以伯和仲丁醇作为反应对象而进行的。这一系列的金属催化剂（Sn、Zn、Bi和 $\\mathbf{Fe}$ )和叔胺类催化剂的影响进行了研究。与未经催化的体系相比较，所有的催化剂均能加速氨基甲酸酯反应。原则上说，金属催化剂可改善IPDI的选择性，而DBTL是最具选择性的催化剂。在一系列的叔胺催化剂中，只有DABCO使选择性逆转。其它叔胺类无显著影响。 \n\n随温度的增加而出现的选择性下降现象一般来说得到了确认。使人惊异的是，DBTL对IPDI的催化却促成了比不用催化剂且在低温下所得到的还要高的选择性，温度提高时尤其如此。 \n\n对影响选择性的另两个因素有所判断。仲丁醇能比伯丁醇产生更高的选择性，这说明了反应对象不同的影响。此外，反式IPDI比IPDI更富选择性。观察到，预聚物合成与模型反应之间存在着很好的相关性。对IPDI预聚物合成的最佳条件可推荐如下：40-60C的温度，使用DBTL催化剂。",
|
||||
"category": " Results and discussion"
|
||||
}
|
||||
]
|
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|
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[
|
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{
|
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"id": 1,
|
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"chunk": "# RSC Advances \n\n \n\nThis is an Accepted Manuscript, which has been through the Royal Society of Chemistry peer review process and has been accepted for publication. \n\nAccepted Manuscripts are published online shortly after acceptance, before technical editing, formatting and proof reading. Using this free service, authors can make their results available to the community, in citable form, before we publish the edited article. This Accepted Manuscript will be replaced by the edited, formatted and paginated article as soon as this is available. \n\nYou can find more information about Accepted Manuscripts in the Information for Authors. \n\nPlease note that technical editing may introduce minor changes to the text and/or graphics, which may alter content. The journal’s standard Terms & Conditions and the Ethical guidelines still apply. In no event shall the Royal Society of Chemistry be held responsible for any errors or omissions in this Accepted Manuscript or any consequences arising from the use of any information it contains.",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 2,
|
||||
"chunk": "# RSC Advances",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 3,
|
||||
"chunk": "# Synthesis and characterization of UV-curable acrylate film modified by functional methacrylate terminated polysiloxane hybrid oligomer \n\nHongleiWanga,b,c, WeiquLiua,b\\*, ZhenlongYana,b,c, JianquanTana,b,c and Guolun Xia-Houa,b,c \n\na Guangzhou Institute of Chemistry, Chinese Academy of Sciences, Guangzhou 510650, China \n\nb Key Laboratory of Cellulose and Lignocellulosics Chemistry, Chinese Academy of Sciences, Guangzhou 510650, China \n\nc University of Chinese Academy of Sciences, Beijing 100049, China \n\n\\* Corresponding author: Email: liuwq@gic.ac.cn \n\nPostal address: Prof. Weiqu Liu, Guangzhou Institute of Chemistry, Chinese Academy of Sciences, Guangzhou 510650, China Tel: +86-20-85231660 Fax: +86-20-85231660",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 4,
|
||||
"chunk": "# Abstract \n\nA series of novel methacrylate terminated polysiloxane hybrid oligomer and functional acrylate oligomer were synthesized and characterized by GPC, FT-IR and NMR. Functional polysiloxane oligomer was introduced into acrylate UV-curing system to improve its surface and thermal properties. With increasing the content of organosiloxane segments, contact angle data of the UV-cured films increased, suggesting the organosiloxane segments migrated to the top surface. The SEM and EDS results demonstrated the migrating of organosiloxane segments. The refraction indexes results showed that the optical performance didn’t reduce after organosiloxane segments being incorporated. According the TGA curves, the decomposition temperatures of the polysiloxane/acrylate composite UV-cured films were higher than that of pure acrylate UV-cured film, which demonstrated organosiloxane groups enhanced the thermal properties of acrylate film due to the high energy of the Si-C bond. The observation of the fractured-surface morphology showed that the organosiloxane segments floated onto the surface of the UV-cured films. \n\nKeyword: Methacrylate terminated siloxane; Functional acrylate oligomer; UV-cured film; Hydrophobic surface",
|
||||
"category": " Abstract"
|
||||
},
|
||||
{
|
||||
"id": 5,
|
||||
"chunk": "# RSC Advances",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 6,
|
||||
"chunk": "# 1． Introduction \n\nUV-curing polymerization is widely used because of its beneficial properties [1-4], such as rapid curing speed, free-VOC, clean and efficient energy and moderate curing condition [5-8]. (Meth)acrylate groups have been employed widely for photopolymerization because of their strong reactivity, their characteristics of optical clarity, mechanical properties, adhesion and chemical stability, showing rapid, near-complete conversions (i.e., on residual unreacted monomers) with low heat generation [9]. Through the proper selection of acrylic/methacrylic monomers and curing agents, the cured polymers can be tailored to specific performance characteristics. Acrylic/methacrylic polymers form materials which are well known for their uses and applications in many important fields especially in the formulation of paints and surface coatings [10, 11]. However, in these applications materials with poor hydrophobicity are not useful unless they are modified. The acrylic/methacrylic polymers are inferior to some silicon-containing materials in terms of elasticity, flexibility, hydrophobicity and the heat resistance ability [12, 13]. In order to meet the need of high-performance coatings in high-technology areas, the UV-curable acrylic/methacrylic coating formulations must be continuously improved. \n\nPolysiloxanes are the most important class of polymers with a non-carbon backbone, exhibiting a large degree of main-chain flexibility and high thermal stability due to Si-O groups [14-18]. Therefore, polysiloxanes have attracted much",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 7,
|
||||
"chunk": "# RSC Advances \n\ninterest and are widely used in modifying polyacrylate coatings. Nevertheless, there is a problem that polysiloxane isn’t compatible well with polyacrylate due to their difference of solubility parameters. To solve this problem, many efforts have been made for the purpose of combining these two materials through chemical methods. Bourgeat-Lami, Bai and Zhao et al. researched on synthesis of polysiloxane and polyacrylate through emulsion polymerization [19-21]. Yu et al. synthesized and evaluated two series of polyacrylate-polydimethylsiloxane (PDMS) block and graft copolymers used in anti-icing coatings [22]. Mostly, research focused on incorporating polysiloxane into the main chain of a polymer, most frequently by emulsion polymerization methods, in order to improve the compatibility. However, emulsion polymerization products showed poor hydrophobicity. Thus, there is an ever increasing demand for polysiloxane modified polyacrylate with better defined, improved and novel physical, chemical and mechanical properties. In this research, we prepared polysiloxane oligomers and then introduced acrylic double bonds by the hydrolysis reaction with methacryloxy propyl trimethoxylsilane at a certain stage. Methacrylate terminated polysiloxane (MATSi) was thus obtained. Owing to the partly similar structure of methacryloxy propyl trimethoxylsilane and polyacrylate, the compatibility between functioned polysiloxane and polyacrylate could be improved. \n\nThe polyacrylate in this work was synthesized as a novel UV-curable polyacrylate (PA). 6-methylheptyl methacrylate was used as the major monomer since it could",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 8,
|
||||
"chunk": "# RSC Advances \n\nprovide good plasticity and was economic at the same time. Minor amount of hydroxyethylmethacrylate were added to promote adherence property. Glycidyl methacrylate was used to introduce epoxy groups to react with methacrylate (MA) in the following reaction step. Furthermore, a series of organosiloxane modified polyacrylate (OSPAs) at different organosilicone concentration ratios were respectively prepared by mixing PA with MATSi. In the presence of photoinitiator, OSPAs were crosslinked by the radical polymerization of the carbon-carbon double bonds in UV irradiation, and then the OSPA cured composite coatings were fast prepared. In this way, various properties and enhanced performance could be obtained in the form of OSPA cross-linked structure. The obtained polymers were characterized by gel permeation chromatography (GPC), fourier transform infrared (FT-IR) spectroscopy and nuclear magnetic resonance (NMR). Furthermore, the surface hydrophobic, optical, and thermal property of the cross-linked coatings made from obtained polymers was investigated by gel content test, flexibility test, pencil hardness test, contact angle (CA) analysis, refraction index test, scanning electron microscope, energy dispersive spectrometer, differential scanning calorimetry thermograms and thermogravimetric analyzer.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 9,
|
||||
"chunk": "# 2. Experimental",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 10,
|
||||
"chunk": "# 2.1 Materials \n\nOctaphenylpolyoxyethylene (OPE) was obtained from Quzhoumingfeng chemical company. Irgacure 1173 was obtained from Ciba Specialty Chemicals.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 11,
|
||||
"chunk": "# RSC Advances \n\nDodecylbenzene sulfonic acid (DBSA), glycidyl methacrylate (GMA), hydroxyethylmethacrylate (HEMA), 6-methylheptyl methacrylate (MHMA), methacrylic acid (MA) and methacryloxy propyl trimethoxylsilane (KH570) were purchased from Aladding Industrial Corporation. Octamethylcyclotetrasiloxane $\\mathrm{(D_{4})}$ was provided by Guangzhou Jiahua chemical company. Distilled water, methanol, triethanolamine and azobisisobutyronitrile (AIBN) were purchased from Jingke Chemical Glass Instrument Co., Ltd. Butanone, tetrabutyl ammonium bromide (TBAB) and ethylalcohol were purchased from Sinopharm Chemical Reagent Co., Ltd. All the above materials were used as received without further purification.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 12,
|
||||
"chunk": "# 2.2 Synthesis of polyacrylate \n\nThe polyacrylate was prepared by using 1:1:8 weight ratio of GMA, HEMA and MHMA in the presence of $4\\mathrm{wt\\%}$ AIBN as initiator and butanone as solvent at a temperature of $80^{\\circ}\\mathrm{C}$ . The reaction was carried out in a four-neck reaction kettle equipped with mechanical stirring, nitrogen inlet, water condenser and thermometer. The reaction was carried out for $8\\mathrm{{h}}$ to obtain desired product. Subsequently, butanone was removed by reduced pressure distillation. The retained desired product was labeled as GHM and was transported into another four-neck kettle. Afterwards, a certain amount of MA was added into the kettle in the presence of $0.8\\mathrm{wt\\%}$ TBAB. The reaction was carried out at $102^{\\circ}\\mathrm{C}$ to reach $99.5\\%$ of the conversion determined by standard acid value. After remaining butanone and unreacted MA were discarded by reduced pressure distillation, the product was obtained and labeled as PA. The general \n\nprocedure was shown in Scheme 1.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 13,
|
||||
"chunk": "# Scheme 1.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 14,
|
||||
"chunk": "# 2.3 Synthesis of MATSi \n\nMATSi was synthesized by emulsion polymerization. The distilled water, surfactants (DBSA and OPE) and monomers $\\mathrm{(D_{4})}$ were added into a four-necked flask equipped with a thermometer, a reflux condenser, a mechanical stirrer and a nitrogen inlet. DBSA acted as acid catalyst as well. Nitrogen was added into the flask to remove oxygen at first. The reaction was carried out for $8\\mathrm{~h~}$ at $80^{\\circ}\\mathrm{C}$ with stirring at about 500rpm. After being neutralized with NaOH solution to stop the reaction, the final latex of PDMS was obtained. Then a certain quality of KH570 was added into PDMS latex. The condensation reaction of PDMS and KH570 was performed at $80^{\\circ}\\mathrm{C}$ for $^{3\\mathrm{~h~}}$ . The copolymers were precipitated in ethanol and dried in vacuum drying oven. The product was purified in ethanol and hexane several times to remove the unreacted monomers and surfactants. Through this procedure, the product was obtained and designated as MATSi. The reaction scheme is shown in Scheme 2.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 15,
|
||||
"chunk": "# Scheme 2.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 16,
|
||||
"chunk": "# 2.4 Preparation of OSPA UV curable films \n\nPA and MATSi where used in relative mass ratios in the range of 100:0 to 90:10 as reported in Table 1. An amount of $5\\mathrm{wt\\%}$ photoinitiator (Irgacure 1173/triethanolamine $\\begin{array}{r l}{=}&{{}2{:}3}\\end{array}$ w/w) was added into each formulation while stirring for 10 min. Triethanolamine was used to avoid the oxygen inhibition during the UV-curing process. Then films were cast onto a glass plate using $5\\%$ w/v solutions of the",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 17,
|
||||
"chunk": "# RSC Advances \n\ncopolymers in methanol by means of a wire-wound applicator. The coated films were laid in room temperature for at least 5 minutes until the solvent was evaporated. Then the films were irradiated by a high-pressure mercury lamp (500W) for 30s with a distance of $20\\ \\mathrm{cm}$ from lamp to the surface of samples in air atmosphere. The thickness of the final coating was about $100\\upmu\\mathrm{m}$ . \n\nTable 1.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 18,
|
||||
"chunk": "# 2.5 Characterization \n\nThe molecular weight and distributions of PA and MATSi oligomer samples were measured at $25^{\\circ}\\mathrm{C}$ by gel permeation chromatography (GPC) on Waters 2410 instrument with THF as the solvent $\\mathrm{(1.0~ml/min)}$ and polystyrene as the calibration standards. \n\nThe FT-IR spectra were recorded with TENSOR27, Bruker, Germany spectrometer over the range $400{\\cdot}4000{\\mathrm{cm}}^{-1}$ . 1HNMR and $^{29}\\mathrm{Si}$ NMR were recorded with a 400MHz Bruker NMR spectrometer using $\\mathrm{CDCl}_{3}$ as solvent and tetramethylsilane as the internal reference. \n\nThe gel content method was performed on the cured films by measuring the weight loss after a 48-h extraction at $80^{\\circ}\\mathrm{C}$ , according to the standard test method ASTM D2665-84[23]. Gel content was calculated as: \n\n$$\n{\\mathrm{Gel~content}}={\\frac{W t}{W o}}\\times100\\%\n$$ \n\nwhere $W_{0}$ is the initial weight of the film, and $W t$ is the final weight after extraction.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 19,
|
||||
"chunk": "# RSC Advances \n\nFlexibility of the UV-cured films was measured according to standard test method (ASTM D522) for elongation of attached coatings with conical mandrel apparatus (QTY-32, Shanghai Junda Co., China). Pencil hardness test was conducted on UV-cured films according to the Stander test method ASTM D2263. \n\nThe contact angle measurements were done by an optical contact angle meter (Shanghai Zhongchen, China) at room temperature $(25^{\\circ}\\mathrm{C})$ using water and ethylene glycol as pendant drops. Each sample was tested more than 5 times at different locations and averaged readings were recorded to obtain a reliable value. The surface free energy was calculated by means of geometric–mean equation which was described by Owens and Wendt [24]. According to Owens and Wendt, the surface energy of a given solid can be determined using an equation applied to two liquids [24, 25]. \n\n$$\n(1+\\mathrm{cos}\\Theta)\\gamma_{1}{=}2(\\gamma_{\\mathrm{s}}^{\\mathrm{\\scriptsize~d}}\\gamma_{1}^{\\mathrm{\\scriptsize~d}})^{1/2}+2(\\gamma_{\\mathrm{s}}^{\\mathrm{\\scriptsize~nd}}\\gamma_{1}^{\\mathrm{\\scriptsize~nd}})^{1/2}\n$$ \n\nwhere $\\upgamma_{\\mathrm{s}}$ and $\\upgamma_{\\mathrm{l}}$ are the surface free energies of the solid and pure liquid, respectively. The superscripts $\\cdot_{\\mathrm{d}},$ and ‘nd’ represent the dispersive and non-dispersive contributions to the total surface energy, respectively. Water $\\mathrm{(\\gamma_{l}=}72.8\\mathrm{mJ/m}^{2}$ , $\\gamma_{\\mathrm{l}}^{\\mathrm{d}}{=}21.8$ $\\mathrm{mJ}/\\mathrm{m}^{2}$ , $\\gamma_{\\mathrm{l}}^{\\mathrm{nd}}{=}51\\ \\mathrm{mJ/m}^{2}$ ), ethylene glycol $\\scriptstyle(\\gamma_{1}=48\\mathrm{mJ}/\\mathrm{m}^{2}$ , $\\gamma_{\\mathrm{l}}^{\\mathrm{d}}{=}29\\mathrm{mJ}/\\mathrm{m}^{2}$ , $\\gamma_{\\mathrm{l}}^{\\mathrm{nd}}{=}19\\mathrm{mJ}/\\mathrm{m}^{2})$ . According to Pinnau and Freeman[26], the contact angle, θ, in Eq. (2) was obtained from the following equation: \n\n$$\n\\scriptstyle\\Theta=\\cos^{-1}(\\frac{c o s\\bar{\\Theta}_{a}+c o s\\bar{\\Theta}_{r}}{2})\n$$ \n\nwhere $\\theta_{\\mathrm{a}}$ and $\\uptheta_{\\mathrm{r}}$ are the advancing and receding contact angles, respectively.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 20,
|
||||
"chunk": "# RSC Advances \n\nThe refraction index of the coatings was determined by an Abbe refractometer (WAY-2W, Shanghai Electronics Physical Optics Instrument Co., Ltd) at $20^{\\circ}\\mathrm{C}$ . \n\nScanning electron microscopy (SEM) and Energy dispersive spectrometer (EDS) were performed. Cross-section morphologies and elementary distribution of the fracture cured coating films were studied by environmental scanning electron microscopy (Hitachi S-4800 FESEM) with an energy dispersive spectrometer. For SEM inspection, samples were fixed to aluminum stubs with conductive tape prior to coating with ${\\sim}20~\\mathrm{nm}$ of gold in an Ernest Fullam sputter coater. \n\nThe thermal stability of cured polymeric materials was determined using a thermogravimetric analyzer (TGA, TG209F3, NETZSCH, Germany). The thermogravimetric analysis of selected coatings were carried out at heating rate of $20^{\\mathrm{{o}}}\\mathrm{C/min}$ under nitrogen atmosphere (flow rate is $30\\mathrm{ml/min}$ ) in the temperature range of $40–600^{\\mathrm{{o}}}\\mathrm{{C}}$ . The differential scanning calorimetry (DSC) thermograms of UV-cured coating samples were performed using the DSC204 (NETZSCH, Germany) over the range from $-60$ to $120^{\\circ}\\mathrm{C}$ at heating rate of $10^{\\mathrm{{o}}}\\mathrm{{C}/\\mathrm{{min}}}$ and held at $120^{\\circ}\\mathrm{C}$ for 5 min to remove the thermal history under $\\Nu_{2}$ atmosphere. \n\n3. Results and discussion \n\n3.1 Synthesis and characterization of OSPA \n\nFive UV-curable organosiloxane modified polyacrylates, OSPA1, OSPA2, OSPA3, OSPA4, OSPA5 were first prepared in this work in order to study the effects of silicon on the properties of UV-curable composite coatings. The general synthetic scheme for",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 21,
|
||||
"chunk": "# RSC Advances \n\nthe preparation of the copolymers used in the coating formulations is shown in Scheme 1 for PA and in Scheme 2 for MATSi. GPC, FT-IR, 1HNMR and 29SiNMR spectra were performed to measure the structures of the products. The molecular weights and polydispersity index of the oligomers were characterized by GPC. The typical molecular weight distributions for PA and MATSi were shown in Fig. 1. As shown in Table 2, the number-average molecular weight of PA and MATSi are 2740 and $1295\\mathrm{\\g/mol}$ , respectively. The two mono-modal GPC curves suggested the formation of the two oligomers. \n\nTable 2. \n\nThe recorded FT-IR spectra of GHM and PA were reported in Fig 2. Compared with the two traces of GHM and PA in Fig. 2, the disappearance of the characteristic absorption peaks of epoxide group at $910~\\mathrm{cm}^{-1}$ indicates the completion of the reaction. The peaks at $1640~\\mathrm{{cm}^{-1}}$ (methacrylate double bond) and $700~\\mathrm{{cm}^{-1}}$ (C-O-H bending) indicate that the epoxy groups have reacted by addition of MA by a ring-opening addition reaction producing one equivalent of hydroxyl groups. Simultaneously, $\\scriptstyle{\\mathrm{C=C}}$ group was introduced into GHM. Absorbance at frequencies characteristic for acrylates (carbonyl $\\scriptstyle{\\mathrm{C=O}}$ stretch at $1720\\mathrm{{cm}^{-1}}$ , C-O stretch four bands $1140\\mathrm{{cm}^{-1}}$ to $1180~\\mathrm{{cm}^{-1}}$ , $1180~\\mathrm{{cm}^{-1}}$ to $1280~\\mathrm{{cm}^{-1}}$ ,etc) are shown [27]. And meanwhile,",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 22,
|
||||
"chunk": "# RSC Advances \n\nthe characteristic absorption peaks at 1000 and $900~\\mathrm{{cm}^{-1}}$ for C-O is present in the spectra. Skeleton vibration of $\\mathrm{C=C}$ group was also present at $483~\\mathrm{{cm}^{-1}}$ . \n\nFig. 3 shows the $^{1}\\mathrm{HNMR}$ spectra of PA in $\\mathrm{CDCl}_{3}$ , peaks in the chemical shift range of 0.7-1.2 ppm and 1.3-1.7 ppm are assigned as $\\mathrm{\\-CH}_{3}$ (a, h, l, u, t) and $\\begin{array}{r}{-\\mathrm{CH}_{2}\\left(\\mathsf{b},\\mathsf{i},\\mathsf{m},\\right.}\\end{array}$ ， o, p, q, r), respectively. The protons resonance signals of –CH (s) and $\\mathrm{\\-CH}_{3}$ (g) appear in the region of 1.5-1.6 ppm and $1.7–2.0\\ \\mathrm{ppm}$ , respectively. The chemical shift of 3.6-3.7 ppm is attributed to protons of $\\mathrm{HO-CH}_{2}(\\mathrm{k})$ and the chemical shift signals at 3.8-3.9 ppm are attributed to proton of HO-CH (d). The peaks at the chemical range of 4.0-4.2 ppm are corresponding to O- $\\mathrm{CH}_{2}$ (c, j, e, n). Peaks at 5.64-5.68 ppm and 6.11-6.18 ppm are assigned as the protons of $\\scriptstyle\\mathrm{C=CH}_{2}$ double bonds (f), indicating that epoxide groups reacted with methacrylic acid thus $C{=}C$ photosensitive groups were introduced. \n\nThe $^{29}\\mathrm{Si}$ NMR signals of mono $\\left(\\mathrm{T}^{1}\\right)$ )-bi $(\\mathrm{T}^{2})$ -and $\\operatorname{tri}(\\mathbf{T}^{3})$ -fold Si-O-linked silicons can be typically observed in -45,…, -50 ppm, -55,…, -60 ppm and -65,…, -70 ppm region, respectively [28]. In Fig.4, the $^{29}\\mathrm{Si}$ NMR spectra of MATSi are shown. The signal at -68.8 ppm is usually assigned to ${\\boldsymbol{\\mathrm{T}}}^{3}$ which represents KH570 after condensation",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 23,
|
||||
"chunk": "# RSC Advances \n\npolymerization. The signal of ${\\mathrm{D}}^{2}$ appears in the region of -21.8 ppm. It indicates the ring-opening and condensation polymerization reactions of Octamethylcyclotetrasiloxane. Poly(dimethylsiloxane) with hydroxyl group on the end is the product of the reactions. The peak at chemical shift of -19 ppm belongs to $\\mathbf{D}^{1}$ signal of Si-O group in MATSi structure. There are no signals in the region of -45,..., -50 ppm and -55,…, -60 ppm, which indicates there are no T1and T2 Si-O-linked silicons in the MATSi structure. It also manifests completely hydrolysis and condensation reactions of KH570. These results confirm that the MATSi is successfully prepared. \n\nThe FT-IR method was also used to confirm the reaction between ring-opened $\\mathrm{D}_{4}$ (PDMS) and KH570. From the IR spectra in Fig.5 it can clearly be observed that PDMS having characteristic peaks at $1018~\\mathrm{{cm}^{-1}}$ and $1089~\\mathrm{{cm}^{-1}}$ which are the characteristic absorption peaks of Si-O-Si. Si- $\\mathrm{CH}_{3}$ stretching vibration peak at 797 $\\mathrm{cm}^{-1}$ was also observed. The peaks of Si-OH at $3699~\\mathrm{{cm}^{-1}}$ indicate that the ring in $\\mathrm{D}_{4}$ was opened and formed polysiloxane. The production MATSi was gained after PDMS reacting with KH570. The spectra of MATSi shows additional absorption peaks at $1722\\ \\mathrm{cm}^{-1}(\\mathrm{C}{=}\\mathrm{O})$ and $1639\\ \\mathrm{cm^{-1}(C{=}C)}$ which represents the reaction between PDMS and KH570. \n\nThe five UV-cured formulations of PA and MATSi are similar to each other and OSPA3 was shown in Fig. 6. After irradiation, the characteristic $C{=}C$ vibrations at $1640\\mathrm{cm}^{-1}$ decreased apparently. \n\nThe characteristic peaks discussed above demonstrated the UV-curable hybrid oligomers based on acrylate containing organosilicone groups were successfully synthesized.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 24,
|
||||
"chunk": "# 3.2 Degree of conversion in UV curing \n\nFT-IR spectroscopy was used to determine the degree of conversion during the UV crosslinking reaction. The absorption band at $1640~\\mathrm{{cm}^{-1}}$ due to $\\scriptstyle{\\mathrm{C=C}}$ vibration was monitored using FT-IR to determine the degree of conversion. The degree of conversion was determined using Eq. (4) [29, 30] $\\mathrm{{Degree~of~conversion}}=(1{-}{\\frac{\\mathit{a t}}{\\mathit{a o}}})\\times100\\$ (4) where $A_{o}$ is the absorption before UV exposure and $A_{t}$ is the absorption after UV exposure. The coating formulation was coated on a KBr window and then exposed to UV radiation for 30 s. As shown in Fig. 7, the decrease in peak area of the $C{=}C$ peak at $1640~\\mathrm{{cm}^{-1}}$ was monitored. Table 3 shows the degree of conversion in coatings after 30s of exposure to UV radiation. All of the OSPA formulations reached high conversion.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 25,
|
||||
"chunk": "# RSC Advances \n\nTable 3 \n\n3.3 Gel content, flexibility and hardness characterization of the UV-cured coatings For the purpose of assessing the amount of insoluble part in cured films and the mechanical properties of the cured coatings, gel content measurements were conducted. In Table 4, the measured values are summarized. The gel content values of all the films are high enough to indicate the nearly complete cross-linked network of the pure PA and the composite OSPAs. In terms of flexibility, all of the composite OSPA samples passed the test of $8\\mathrm{mm}$ and 6mm diameter, and most of them passed the test of $5\\mathrm{mm}$ diameter, while the pure PA sample failed all the test of $8\\mathrm{mm}$ , 6mm and $5\\mathrm{mm}$ diameter. The hardness value of the samples rises from 3H to 6H with the increasing addition of MATSi. The flexibility and hardness test suggests that introduction of flexible silicon-oxygen segments enhanced mechanical properties of the UV-cured coatings. \n\nTable 4. \n\n3.4 Surface and optics characterization of the cured coatings In order to determine the effect of organosilicone on surface and optical properties",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 26,
|
||||
"chunk": "# RSC Advances \n\nof the UV-cured hybrid oligomers films, contact angle and refraction index were tested respectively. Table 5 presents the contact angle of the five samples. It can be seen that contact angle values of both water and ethylene glycol for pure PA film are much lower than any OSPA cured film. With the increasing of MATSi content, the contact angle values on OSPA cured film surfaces showed a gradually increasing change. It was found that based on the increase of organosilicone concentration, OSPA tended to be more hydrophobic compared with the virgin PA. Since organosilicone possesses low surface energy, they can easily move towards the air-polymer interface causing their enrichment on coating surface to some extent [31, 32]. Thereby, the presence of MATSi could lead to a great decrease in the surface free energy, and among these composite films, OSPA5 presented a very low surface free energy value down to $8.89~\\mathrm{mN/m}$ . Surfaces from mixtures of PA/ MATSi with a ratio of 1:0.02 still show hydrophobicity although the organosilicone content is low. The results shown in Table 5 indicate that organosilicone contribute to the surface hydrophobicity.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 27,
|
||||
"chunk": "# Table 5. \n\nThe refraction index of the coatings was measured by an Abbe refractometer at $20^{\\circ}\\mathrm{C}$ . The obtained refraction indexes for samples OSPA1, OSPA2, OSPA3, OSPA4, and OSPA5 were listed in Fig. 8. As expected the refraction indexes ranged between 1.5612 and 1.5571 and are consistent with expected values for slight amount of",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 28,
|
||||
"chunk": "# RSC Advances \n\norganosilicone content in the films. The refraction index of the samples gained a very small change with the increase of the organosilicone content which would not affect the optical properties of the composited material.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 29,
|
||||
"chunk": "# Fig. 8 \n\n3.5 Thermal properties of the cured coatings \n\nOverall weight loss was observed in composite films with different organosilicone content. The TGA traces of all cured coatings are included in Fig.9, and plots of mass loss versus temperature are shown. To gain better understanding of the degradation behavior of the cured composite coatings, virgin PA film was compared with these composites at three specific degradation temperatures: (a) the temperature of the initial $5\\%$ mass loss $(\\mathrm{T}_{5\\%})$ ; (b) the temperature of the $50\\%$ mass loss $(\\mathrm{T}_{50\\%})$ and (c) residual weight percent at $600^{\\mathrm{{o}}}\\mathrm{{C}}$ . Three specific degradation data are summarized in Table 6. It shows that the typical onset temperature of the degradation is higher for the composites than the virgin PA. The thermal stability of the OSPA composites is enhanced relative to that of virgin PA. All the OSPA samples exhibit an apparent higher temperature at $50\\%$ weight loss during decomposition compared with pure PA. The different thermal properties between virgin PA and OSPA may be attributed to some interaction between organosilicone and PA that serves to stabilize the composite. The thermal stability of the composites systematically increases with increasing organosiloxane. The results demonstrate that the incorporated organosiloxane play an",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 30,
|
||||
"chunk": "# RSC Advances \n\nimportant role during decomposition. The residual silicon-contained compound act as an insulator and mass transport barrier to the volatile products generated during decomposition. Meanwhile, compared with virgin PA, the more complex OSPA network reduced the overall rate of volatiles evolution. \n\nGlass transition temperature $(T_{\\mathrm{g}})$ of the UV-cured films were investigated by differential scanning calorimetry (DSC). Fig. 10 shows the DSC thermograms of PA and OSPAs. The $T_{\\mathrm{g}}$ value of all the samples are summarized in Table 6. There was an increasing trend of $T_{\\mathrm{g}}$ value as the amount of MATSi in pure PA increasing. \n\nTable 6. . \n\nFig. 9. \n\n3.6 Micro-morphology of the cured coatings \n\nFig.11 shows the fractured-surface microstructure of the cured films cast onto glass slides from a PA/ MATSi ratio of 98:2, 96:4, 94:6, 92:8 and 90:10. Sample (a) exhibits a uniform distribution for the network of virgin PA. However, the fracture surface of OSPAs showed rougher features than that of virgin PA. These observations also indicate that the distribution of organosilicone copolymer in virgin PA is not homogeneous. In addition, it can be clearly observed that a certain extent of sphere",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 31,
|
||||
"chunk": "# RSC Advances \n\nwere enriched closed to the air side surface and there were also spheres in the matrix. This observation evidenced that the silicon-contained groups moved towards the air side surface of the cured films. These results can be explained as follows: During the solvent evaporation, silicon-contained groups move towards the top side surface of the UV-cured formulations owing to the poor compatibility with PA. These observations are in good agreement with the results obtained by contact angle value. When the content of MATSi increases, the phase separation appeared and became more obviously at the interphase [33-35]. It can be inferred that the hydrophobic surface may resulted from the silicon-contained segments in MATSi groups. The EDS results in Fig.12 showed energy-spectrum scanning from bottom to top of the film. It also indicated that the silicon-contained groups assembled on the surface of the films which agrees well with SEM and contact angle data. Furthermore, the silicon spheres are always at the end of the crack, which means they could efficiently absorb the energy generated in the fracture process and prevent aggravated fracture.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 32,
|
||||
"chunk": "# 4. Conclusion \n\nA novel methacrylate terminated polysiloxane was synthesized by hydrolysis reaction using octamethylcyclotetrasiloxane and methacryloxy propyl",
|
||||
"category": " Conclusions"
|
||||
},
|
||||
{
|
||||
"id": 33,
|
||||
"chunk": "# RSC Advances \n\ntrimethoxylsilane. Methacrylate groups were incorporated into functional polysiloxane oligomer to enhance the compatibility between organosiloxane segments and acrylate film. With the incorporation of organosiloxane OSPA gained increased thermal and mechanical properties compared to the virgin PA. Besides that, it was determined that owing to the hydrophobicity of organosilicone segments, the cured coating films containing PDMS had low surface free energy, and higher thermal degradation temperature. SEM and EDS studies of the coatings depicted that silicon-contained groups gathered on the air-side surface of the cured films. The low cost hydrophobic UV-curable OSPA coatings have a promising combination of physical and mechanical properties which will lead to potential application in industrial coatings fields such as printing inks, paints, adhesives and packaging overcoat film.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 34,
|
||||
"chunk": "# 5. Acknowledgements \n\nThis study was financially supported by the Program “Tianhe District science and technology plan”.",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 35,
|
||||
"chunk": "# References \n\n[1] C. Chen, M. L. Li, Y. J. Gao, J. Nie and F. Sun, RSC Adv., 2015, 5, 33729. \n[2] D. Knittel and E. Schollmeyer, Polym. Int., 1998, 45 (1): 110-117. \n[3] K. J. van den Berg, L.G. J. van der Ven and H. J. W. van den Haak, Prog. Org. Coat., 2008, 61: 110-118.",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 36,
|
||||
"chunk": "# RSC Advances \n\n[4] X. Liu, R. Liu, J. Zheng, Z. Li and J. liu, RSC Adv., 2015, DOI: 10.1039/C5RA03881B. \n[5] S. P. Pappas, Radiation curing: science and technology, New York: Plenum, 1992. \n[6] J. H. Lee, R. K. Prud'Homme, I. A. Aksay, J. Mater. Res., 2001, 16(12): 3536-3544. \n[7] H. D. Hwang, C. H. Park, J. I. Moon, H. J. Kim and T. Masubuchi, Prog. Org. Coat., 2011, 72: 663-675. \n[8] R. Mehnert, A. Pincus, I. Janorsky, R. Stowe and A. Berejka, UV and EB Curing Technology and Equipment, vol. I, SITA Technology Ltd., London, 1998. \n[9] B. Türel Erbay and I. E. Serhatlı, Prog. Org. Coat., 2013, 76: 1-10. \n[10] O. Chiantore, L. Trossarelli and M. Lazzari, Polymer, 2000, 41(5): 1657-1668. \n[11] P. A. Christensen, A. Dilks, T. A. Egerton and J. Temperley, J. Mater. Sci., 1999, 34 (23): 5689-5700. \n[12] S. J. Jeon, J. J. Lee, W. Kim, T. S. Chang and S. M. Koo, Thin Solid Films., 2008, 516: 3904-3909. \n[13] H. Li, S. Liu, J. Zhao, D. Li and Y. Yuan, Thermochim. Acta., 2013, 573: 32-38. \n[14] B. U. Ahn, S. K. Lee, S. K. Lee, J. H. Park and B. K. Kim, Prog. Org. Coat., 2008, 62: 258-264. \n[15] H. D. Hwang and H. J. Kim, React. Funct. Polym., 2011, 71: 655-665. \n[16] J. P. Lewicki, J. J. Liggat and M. Patel, Polym. Degrad. Stabil., 2009, 94: 1548-1557.",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 37,
|
||||
"chunk": "# RSC Advances \n\n[17] S. W. Zhang, Z. D. Chen, M. Guo, J. Zhao and X. Y. Liu, RSC Adv., 2014, 4, 30938. \n[18] M. Alexandre and P. Dubois, Mater. Sci. Eng: R: Reports., 2000, 28(1): 1-63. \n[19] M. Lin, F. Chu, A. Guyot, J. L. Putaux and E. Bourgeat-Lami, Polymer., 2005, 46: 1331-1337. \n[20] H. Li, S. Liu, J. Zhao, D. Li and Y. Yuan, Thermochim. Acta., 2013, 573: 32-38. \n[21] R. Bai, T. Qiu, F. Han, L. He and X. Li, Appl. Surf. Sci., 2012, 258: 7683-7688. \n[22] ASTM D2665-84, Standard Specification for Poly(Vinyl Chloride) (PVC) Plastic Drain, Waste, and Vent Pipe and Fittings, reapproved 2009. \n[23] D. Yu, Y. Zhao, H. Li, H. Qi, B. Li and X. Yuan, Prog. Org. Coat., 2013, 76: 1435-1444. \n[24] D. K. Owens and R. C. Wendt, J. Appl. Polym. Sci., 1969, 12: 1741-1747. \n[25] T. Ç. Çanak and Đ. E. Serhatlı, Prog. Org. Coat., 2013, 76: 388-399. \n[26] Formation and modification of polymeric membranes: overview, in: I. Pinnau,B.D. Freeman (Eds.), 214th National Meeting of the American-Chemical-Society, Las Vegas, NE, 1997, pp. 1– 22. \n[27] V. V. Krongauz, Thermochim. Acta., 2010, 503-504: 70-84. \n[28] K. Albert, E. Bayer and B. Pfleiderer, J. Chrom., 1990, 506: 343. \n[29] W. Xiao and W. Tu, J. Chem. Eng. Chin. Univ., 2009, 2: 13. \n[30] I. Rehman, E. H. Andrews and R. Smith, J. Mater. Sci: Mater. Med., 1996, 7(1): 17-20. \n[31] H. Tavana, F. Simon, K. Grundke, D. Y. Kwok, M. L Hair and A. W. Neumann,",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 38,
|
||||
"chunk": "# RSC Advances \n\nJ. Colloid. Interf. Sci., 2005, 291(2): 497-506. \n\n[32] Y. S. Kim, J. S. Lee, Q. Ji and J. E. McGrath, Polymer., 2000, 43(25): 7161-7170. \n[33] Z. Yan, W. Liu, N. Gao, H. Wang and K. Su, Appl. Surf. Sci., 2013, 284: 683-691. \n[34] M. Sangermano, W. Carbonaro, R. Bongiovanni, R. R. Thomas and C. M. Kausch, Macromol. Mater. Eng., 2010, 295(5): 469-475. \n[35] W. Liu, S. Ma, Z. Wang, C. Hu and C. Tang, Macromol. Res., 2010, 18(9): 853-861. \n\nFigure captions: \n\nScheme 1. Synthesis route of UV-cured PA \n\nScheme 2. Synthesis route of MATSi \n\nFigure 1. GPC traces of PA (a) and MATSi (b) \n\nFigure 2. FT-IR spectra of GHM and PA \n\nFigure 3. $\\mathrm{^1H}$ NMR spectra of PA \n\nFigure 4. $^{29}\\mathrm{Si}$ NMR spectra of the synthesis of MATSi \n\nFigure 5 FT-IR spectra of the synthesis of MATSi \n\nFigure 6. FT-IR spectra of the synthesis of OSPA \n\nFigure 7. FT-IR spectra of the UV-curable film formulations of PA and OSPAs. a) \n\nBefore irradiation; b) After UV-curing \n\nFigure 8. Refraction Indexes of the UV-cured coatings \n\nFigure 9. TGA curves of the UV-cured coatings. \n\nFigure 10. DSC thermograms of the UV-cured PA and OSPA coatings \n\nFigure 11. SEM images of fractured-surface morphologies of the UV-cured coatings: \n\n(a)PA; (b)OSPA1; (c)OSPA2; (d)OSPA3; (e)OSPA4; (f)OSPA5. \n\nFigure 12. EDS images of fractured surface of the UV-cured coatings",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 39,
|
||||
"chunk": "# RSC Advances \n\n \n\n \nScheme 1. Synthesis route of UV-cured PA $70{\\times}173{\\ m m}$ $600\\times600$ DPI) \n\n \nScheme 2. Synthesis route of MATSi $21\\times30\\mathsf{m m}$ $600\\times600$ DPI) \n\n \nFig.1. GPC traces of PA (a) and MATSi (b) $70\\times49\\mathsf{m m}$ ( $300\\times300$ DPI) \n\n \nFig.2. FT-IR spectra of GHM and PA 201x141mm ( $300\\times300$ DPI) \n\n \nFig.3. $<1>H$ NMR spectra of PA 201x140mm ( $300\\times300$ DPI) \n\n \nFig.4. ${<}29{>}\\mathsf{S i}$ NMR spectra of the synthesis of MATSi $70\\times49\\mathsf{m m}$ $300\\times300$ DPI) \n\n \nFig.5. FT-IR spectra of the synthesis of MATSi $210{\\times}148\\mathsf{m m}$ ( $300\\times300$ DPI) \n\n \nFig.6. FT-IR spectra of the synthesis of OSPA 201x141mm ( $300\\times300$ DPI) \n\n \nFig.7. FT-IR spectra of the UV-curable film formulations of PA and OSPAs. a) Before irradiation; b) After UVcuring. 201x140mm (300 x 300 DPI) \n\n \nFig.8. Refraction Indexes of the UV-cured coatings $70\\times49\\mathsf{m m}$ ( $300\\times300$ DPI) \n\n \nFig.9. TGA curves of the UV-cured coatings $70\\times49\\mathsf{m m}$ $300\\times300$ DPI) \n\n \nFig.10. DSC thermograms of the UV-cured PA and OSPA coatings $70\\times49\\mathsf{m m}$ $300\\times300$ DPI) \n\n \nFig.11. SEM images of fractured-surface morphologies of the UV-cured coatings: (a)PA; (b)OSPA1; (c)OSPA2; (d)OSPA3; (e)OSPA4; (f)OSPA5 49x23mm ( $300\\times300$ DPI) \n\n \n\nFig.12. EDS images of fractured surface of the UV-cured coatings $90\\times90\\mathrm{mm}$ $300\\times300$ DPI)",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 40,
|
||||
"chunk": "# RSC Advances \n\nTable 1. Mass ratio of PA and MATSi. \n\n\n<html><body><table><tr><td>Samples</td><td>PA (%)</td><td>MATSi (%)</td></tr><tr><td>Pure PA</td><td>100</td><td>0</td></tr><tr><td>OSPA1</td><td>98</td><td>2</td></tr><tr><td>OSPA2</td><td>96</td><td>4</td></tr><tr><td>OSPA3</td><td>94</td><td>6</td></tr><tr><td>OSPA4</td><td>92</td><td>８</td></tr><tr><td>OSPA5</td><td>90</td><td>10</td></tr></table></body></html>",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 41,
|
||||
"chunk": "# RSC Advances \n\nTable 2. Molecular weights of PA and MATSi oligomers \n\n\n<html><body><table><tr><td>Samples</td><td> Mna</td><td>PDIb</td></tr><tr><td>PA</td><td>2740</td><td>2.18</td></tr><tr><td>MATSi</td><td>1295</td><td>2.09</td></tr></table></body></html>\n\n$^{\\mathrm{a}}\\mathrm{Mn}$ : the number-average molecular weight, determined by GPC. bPDI:the polydispersity index, determined by GPC. \n\nTable 3. Degree of conversion of double bonds in the UV cured coatings \n\n\n<html><body><table><tr><td>Coating</td><td>Conversion (%)</td></tr><tr><td>PA</td><td>95</td></tr><tr><td>OSPA1</td><td>96</td></tr><tr><td>OSPA2</td><td>97</td></tr><tr><td>OSPA3</td><td>99</td></tr><tr><td>OSPA4</td><td>97</td></tr><tr><td>OSPA5</td><td>98</td></tr></table></body></html>",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 42,
|
||||
"chunk": "# RSC Advances \n\nTable 4.Gel content, flexibility and hardness characterization of the UV-cured coatings. \n\n\n<html><body><table><tr><td rowspan=\"2\">Samples</td><td rowspan=\"2\">Gel content (%)</td><td colspan=\"3\">Flexibility</td><td rowspan=\"2\">Pencil hardness</td></tr><tr><td>8mm</td><td>6mm</td><td>5mm</td></tr><tr><td>Pure PA</td><td>97</td><td>Fail</td><td>Fail</td><td>Fail</td><td>3H</td></tr><tr><td>OSPA1</td><td>98</td><td>Pass</td><td>Pass</td><td>Fail</td><td>5H</td></tr><tr><td>OSPA2</td><td>97</td><td>Pass</td><td>Pass</td><td>Pass</td><td>6H</td></tr><tr><td>OSPA3</td><td>98</td><td>Pass</td><td>Pass</td><td>Pass</td><td>6H</td></tr><tr><td>OSPA4</td><td>98</td><td>Pass</td><td>Pass</td><td>Pass</td><td>6H</td></tr><tr><td>OSPA5</td><td>98</td><td>Pass</td><td>Pass</td><td>Pass</td><td>6H</td></tr></table></body></html>",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 43,
|
||||
"chunk": "# RSC Advances \n\nTable 5. Contact angle of the UV-cured coatings. \n\n\n<html><body><table><tr><td colspan=\"2\">Surface free energy(mN/m)</td><td colspan=\"2\">Contact angle (0)with</td></tr><tr><td></td><td>Ys</td><td>Deionized water</td><td>Ethylene glycol</td></tr><tr><td>PA</td><td>44.28</td><td>94</td><td>55.75</td></tr><tr><td>OSPA1</td><td>11.70</td><td>102.5</td><td>91</td></tr><tr><td>OSPA2</td><td>12.73</td><td>108.5</td><td>91</td></tr><tr><td>OSPA3</td><td>10.36</td><td>108.5</td><td>94.5</td></tr><tr><td>OSPA4</td><td>13.27</td><td>109.5</td><td>91</td></tr><tr><td>OSPA5</td><td>8.89</td><td>114</td><td>99.5</td></tr></table></body></html>\n\n$\\upgamma_{\\mathrm{s}}$ surface free energy of solid.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 44,
|
||||
"chunk": "# RSC Advances \n\nTable 6. Thermal properties of the UV-cured coatings. \n\n\n<html><body><table><tr><td>Sample</td><td>T5%</td><td>T50%</td><td>wt% at 600℃</td><td>Tg</td></tr><tr><td>PA</td><td>187.8</td><td>304.1</td><td>0</td><td>15.67</td></tr><tr><td>OSPA1</td><td>220.6</td><td>339.7</td><td>0.3</td><td>22.05</td></tr><tr><td>OSPA2</td><td>211.5</td><td>338.2</td><td>0.9</td><td>24.01</td></tr><tr><td>OSPA3</td><td>190.8</td><td>335.9</td><td>1.2</td><td>27.92</td></tr><tr><td>OSPA4</td><td>183.9</td><td>343.5</td><td>2.7</td><td>27.99</td></tr><tr><td>OSPA5</td><td>224.1</td><td>345.1</td><td>8.2</td><td>27.05</td></tr></table></body></html>",
|
||||
"category": " Results and discussion"
|
||||
}
|
||||
]
|
||||
202
task2/task2-chunks/Rheology_-_2015.json
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202
task2/task2-chunks/Rheology_-_2015.json
Normal file
@@ -0,0 +1,202 @@
|
||||
[
|
||||
{
|
||||
"id": 1,
|
||||
"chunk": "Stuart G. Croll \n\nNorth Dakota State University Coatings and Polymeric Materials \n\nDiagrams by Dr. Olena Shavranska \n\nCopyright S. G. Croll, NDSU \n\nSummary \n\n• Background and Definitions \nPaint Properties \n• Viscometers \n• Solution rheology \n• Suspension rheology \n\nRheology \n\n• Rheology $\\mathbf{\\tau}=$ science of flow and deformation ( materials characteristics) \n\n• Fluid Mechanics $\\mathbf{\\tau}=$ science of where fluids flow to in given processes.",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 2,
|
||||
"chunk": "# Importance of Rheology \n\n• Most convenient state to apply coatings is as a liquid (can also be done as a powder or gas) \n\n– Brush – Roll – Spray, etc \n\n• Therefore paint must be made into a liquid form \n\n– Solution properties – Suspension properties – Mixing – Drying and Curing \n\nCopyright S. G. Croll, NDSU \n\nPaint, Inks, Sealants, Caulks, Cosmetics, and Packaged Foods etc. \n\n• Consist of: \n\n– Solutions: binder polymers, dispersants, thickeners, cross-linkers \n\n– Suspensions: latex, pigments, extenders, non-aqueous dispersions, emulsions, defoamers, surfactant micelles \n\nHow do we define flow properties? \n\n• Materials flow when pushed (forced) – Stress is important \n\n• How much they flow is important (changes of shape) \n\n– Simple liquids require no force to retain their shape \n\n– How fast they are strained is the important factor that determines how much force is needed",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 3,
|
||||
"chunk": "# Viscosity Definition \n\n• Liquids’ flow is usually determined by the shear stress imposed, or the change of flow rate through the liquid, Newton’s law: \n\n$$\n{\\boldsymbol{\\tau}}=\\eta{\\dot{\\boldsymbol{\\gamma}}}\n$$ \n\nWhere \n\nThis is Newtonian behavior $\\mathbf{\\tau}=\\mathbf{\\tau}$ linear, no time dependence \nShear rate is the time differential of the shear strain and is given, in shear, by the velocity, $\\nu$ , gradient across the flow: \n\n$$\n\\dot{\\gamma}=\\frac{\\delta\\nu}{\\delta y}\n$$ \n\nCopyright S. G. Croll, NDSU",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 4,
|
||||
"chunk": "# Viscosity \n\nViscosity $\\mathbf{\\tau}=\\mathbf{\\tau}$ resistance to flow \n\n$\\mathbf{\\Sigma}=$ resistance to movement of molecules; solvent, solute and suspended matter through space. \n\\~ inverse of diffusion coefficient of molecules or particles through the medium \n\nNewtonian flow is for liquids what Hooke’s law is for solids (elastic solids) \n\nHowever, since liquids flow to accommodate stress, the complementary variables are stress and strain-rate (in shear usually).",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 5,
|
||||
"chunk": "# Shear Deformation \n\n• Shear Deformation can be visualized like a pack of cards \n• A force $F$ is applied to the uppermost volume element (thickness $d y)$ , the material will deform by the displacement $d x$ of adjacent elements. \n\n• Shear rate $\\mathbf{\\tau}=\\mathbf{\\tau}$ rate of change of the shear strain $\\mathbf{\\Sigma}=$ change in the velocity across the thickness direction (y here) of the element $\\mathbf{\\Sigma}=\\mathbf{\\Sigma}$ [distance/time $\\div$ distance $\\mathbf{\\tau}=\\mathbf{\\tau}/\\mathrm{tim}\\mathbf{e}]=\\mathbf{s}^{-1}$ \n\n• Shear Stress $\\mathbf{\\tau}=\\mathbf{\\tau}$ Shear force, $\\mathrm{~F~}\\div$ Area, A \n\n \nShear Deformation \n\n<html><body><table><tr><td>Shear Strain</td></tr><tr><td>In shear, strain is not a relative increase in length, area or volume, but a change in shape (angle) given by: 4x</td></tr><tr><td>4y And in the infinitesmal limit by: dx 2</td></tr></table></body></html> \n\n<html><body><table><tr><td>Units and Conversions</td></tr></table></body></html> \n\nCopyright S. G. Croll, NDSU \n\n\n<html><body><table><tr><td></td><td>CGS</td><td>MKS</td><td>SI</td></tr><tr><td>Strain</td><td>dimensionless</td><td>dimensionless</td><td>dimensionless</td></tr><tr><td>Strain rate</td><td>s-1</td><td>s-1</td><td>s-1</td></tr><tr><td>Stress</td><td>dyne/cm²</td><td>Newton/m²</td><td>Pascal (Pa) (=1 Newton/m2)</td></tr><tr><td>Viscosity (liquids)</td><td>Poise (P) (=1 dyne-s/cm²) centipoise (cP) (=0.01 P = 1 m Pa-s)</td><td>Newton-s/m²</td><td>Pa-s (=10 P) mPa-s (= 10-3 Pa-s = 1 cP)</td></tr><tr><td>Modulus (solids)</td><td>dyne/cm²</td><td>Newton/m2</td><td>Pa</td></tr></table></body></html> \n\n<html><body><table><tr><td>Note: Kinematic Viscosity</td></tr><tr><td>Occasionally used = viscosity/density</td></tr><tr><td>Units: “Stokes\" in c.g.s. m²/s in S.I. or M.K.S.</td></tr><tr><td>Copyright S.G.Croll,NDSU 13</td></tr></table></body></html> \n\nExamples: orders of magnitude",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 6,
|
||||
"chunk": "# Viscosity Application Shear Rates \n\nAir, a Gas $10^{-5}$ Pa.s Water 10-3 Glycerine 1 Syrup $10^{2}$ Glass, a solid $10^{21}$ \n\nBrushing 4000-10000 s-1 Brush Pick-up $5{\\mathrm{~}}{\\mathrm{{s}}}^{-1}$ Spraying $10^{3}-10^{6}$ Settling $\\sim10^{-3}$ Sagging $10^{-2}\\ –\\ 10^{-1}$ Leveling $10^{-1}$ Coil Coating $10^{4}$ Hand Rolling $\\mathord{\\sim}500$ \n\nCopyright S. G. Croll, NDSU",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 7,
|
||||
"chunk": "# Example: Balance of Properties in HousePaint \n\nDifferent applications have different requirements on viscosity: \n\nSagging needs high viscosity to counter it \nLeveling needs low viscosity so brushmarks etc. disappear (note the problem vs. sag) \nApplication by brush and roll needs a low viscosity so that it is easy (but the coating must level and not sag) \nIf the brushing or rolling is done at too low a viscosity – the coating is too thin and may bead up \nThe viscosity has to be high enough that the brush picks up enough paint. \nSpraying viscosity must be low (for pumping and atomization) \n\nThe time-dependence and non-linear behavior of typical paint gives us ways to achieve all these properties.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 8,
|
||||
"chunk": "# Leveling Geometry \n\n \n\n<html><body><table><tr><td>Example: Leveling in Newtonian Paint</td></tr><tr><td>Leveling expresses how fast the brushmarks or roller spatter disappear. To a first approximation they disappear exponentially in time: Amplitude(t)= Ampt=o.exp(-t/t.)</td></tr><tr><td>3L'n (2π)4oh3 Where the time constant, t is given by: t, = -</td></tr><tr><td>L = wavelength of the brushmark, longer goes away more slowly, o= surface tension of the fluid, high values help leveling</td></tr><tr><td>speed. h = thickness, so leveling is very sensitive to thickness, thicker coatings level quicker</td></tr></table></body></html> \n\nExample: Sagging in Newtonian Paint \n\nThere is a balance of forces between the viscous drag within a paint film and the force of gravity making the paint run down the wall.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 9,
|
||||
"chunk": "# Coating \n\n$$\n\\scriptstyle{\\dot{\\gamma}}\\left(x\\right)={\\frac{\\rho g\\left(h-x\\right)}{\\eta}}\n$$ \n\n$g=$ acceleration due to gravity $\\rho=$ density of the paint $h=$ thickness of the paint At $x=0$ (outer surface of paint), sag movement is greatest At wall, $x=h$ , there is no movement \n\n \n\nHigh viscosity helps stop movement",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 10,
|
||||
"chunk": "# Real Materials (inc. paints) are NonNewtonian \n\n• Newtonian liquids are “ideal” – Liquid does not change under flow so viscosity does not change Real Liquids are not ideal – They change so their properties depend on the previous motion They have memory, i.e. $\\mathbf{\\Sigma}=\\mathbf{\\Sigma}$ time dependent – Molecular and particle interactions depend on rate of deformation They are non-linear – They may also be reacting and drying as well",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 11,
|
||||
"chunk": "# High vs. Low shear rate \n\n• High Shear rates \n\n– All specific interactions are overcome by high energy of flow \n– Viscosity depends mainly on viscosity of solvent and the volume concentration of dissolved or dispersed phases \n\n• Low Shear rates \n\nSpecific interactions remain between components Viscosity is often orders of magnitude higher than at high shear rates because of these interactions \n\n<html><body><table><tr><td>Time Dependent Behavior = Solid-like behavior (in liquids)</td></tr><tr><td>If liquids have memory, then they have some elements of solid-like behavior and we can use solid-like concepts to describe these attributes:</td></tr><tr><td>Elasticity</td></tr><tr><td>Yield Stress Normal Forces</td></tr><tr><td>Extensional Viscosity The overall combination of viscous and elastic behavior is</td></tr><tr><td>termed “viscoelastic\",as in solids Time-dependent solids, e.g. solid polymers, are also called</td></tr><tr><td>viscoelastic</td></tr><tr><td>PAINTSARE VISCOELASTIC Copyright S.G.Croll,NDSU 21</td></tr></table></body></html> \n\n<html><body><table><tr><td>Elasticity - a form of time-dependence in liquids</td></tr><tr><td>Liquids may recoil when shearing stops, i.e. solid-like - hence“elasticity” The response to a changing stress or shear rate may not be completely in phase with it - i.e. time-dependent properties (relaxation) - for liquids, the in-phase part of the response is the viscosity and the out-of-phase component is the shear modulus (solid-like part of the response)</td></tr></table></body></html> \n\n \nCopyright S. G. Croll, NDSU \n\nWhat if the material does not respond proportionally? \n\n• Non-linear fluids exhibit a great variety of behaviors. \n\n– Usually paints, solutions and dispersions are “shear-thinning” \n– They may exhibit a “yield stress” (plastic behavior) \n– Sometimes they “shear-thicken” \n– Occasionally they conform to other jargon \n\n“Newtonian” liquids are linear and are not timedependent.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 12,
|
||||
"chunk": "# Shear-Thinning Fluids \n\nViscosity decreases with increasing shear-rate or increasing shear stress, another term for this is “pseudoplastic” The term does not imply time-dependence necessarily (but most paints are as well) \n\nDispersions and solutions are usually shear-thinning above a dilute concentration. \n\nThe two main reasons for shear-thinning in suspensions: \n\nBreakdown of flocculation, i.e. releasing more liquid from within the flocc. to lubricate the particles and decrease the effective volume solids. \nIn non-flocculated systems, often there are inter-particle correlating forces or arrangements that are overcome at higher shear stresses when the system becomes randomized or the particles may order themselves along the direction of flow. \n\nSolutions shear-thin for similar reasons; entanglements breakdown and molecules elongate along the flow direction",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 13,
|
||||
"chunk": "# As particles align along the flow , the viscosity diminishes. \n\nLining-up occurs more at both higher deformation rates and longer times. Produces non-linear and time-dependent elements of the viscosity response \n\n \n\nLining-up occurs in spatially confined flows – most coatings applications, and in shear-thinning fluids – most of coatings, see: S. V. Loon, J. Fransaer, C. Clasen, J. Vermant, “String Formation in sheared suspensions in rheologically complex media: The essential role of shear thinning,” J. Rheol., 58(1), 237 – 254, 2014 \n\n \n\n \nPaints are Shear-Thinning and Time-Dependent, example: \n\n \nCopyright S. G. Croll, NDSU \n\n \nCopyright S. G. Croll, NDSU",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 14,
|
||||
"chunk": "# “Yield Stress” \n\n• Some fluids seem not to flow at very low stresses, but only flow above a certain critical stress referred to as the “yield” stress. – This is called “plastic” behavior by analogy to solids. \n• Below this yield, there is no flow so the viscosity is infinite(?) \nThere are those who believe that yield cannot really exist (we just need more sensitive rheometers) – but it can be a useful description of fluid behavior. \n\n \n\n \nCopyright S. G. Croll, NDSU \n\n33",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 15,
|
||||
"chunk": "# Shear-Thickening \n\nUsually happens at high shear-rates and in systems that are more concentrated. May happen because particles get jammed together and do not have enough room to move around each other quickly enough Disperse phase effectively increases in concentration $\\mathbf{\\sigma}=\\mathbf{\\sigma}$ “dilatant” behavior May also happen because strings of particles tumble at high flow rates. Flocculation can be induced at the high collision rates imposed by high shearrates. \n\nSee also: E. Brown, H. M Jaeger, “Shear thickening in concentrated suspensions: phenomenology, mechanisms and relations to jamming,” Rep. Prog. Phys. 77 (2014) 046602 (23pp) \n\n \nN. J. Wagner, J. F. Brady, \"Shear Thickening in colloidal dispersions, Physics Today, 62(10), 27 - 32 (2009)",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 16,
|
||||
"chunk": "# More about Time-Dependence \n\n“Thixotropic” behavior $\\mathbf{\\tau}=\\mathbf{\\tau}$ viscosity diminishes with time under shear – Very typical behavior in paints, food etc. – Intermolecular or inter-particle interactions breakdown with time under stress • Flocculation, hydrophobic association or polar interactions – Detected in “hysteresis” loop experiments \n\n• “Rheopexy” is the opposite behavior and unusual \n\n<html><body><table><tr><td colspan=\"4\">Thixotropic Behavior, some examples (time-dependent) > between j, and 0</td></tr><tr><td colspan=\"4\">=0 >0</td></tr></table></body></html> \n\n",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 17,
|
||||
"chunk": "# Normal Forces \n\n• In Newtonian liquids, the shear in one direction does not change the interaction or shape of molecules or particles, so everything remains balanced. \n\nIn a real liquid, shear changes interactions (depends on their closeness) or causes anisotropy, e.g. orientation of molecules, etc. \n\n– System is no longer in the initial random configuration \n– So the stresses in the three cartesian directions (normal directions) may no longer be the same $\\tau_{11}\\neq$ $\\tau_{22}\\neq\\tau_{33}$ \nWe measure “normal forces” as $\\Nu_{1}=\\tau_{11}-\\tau_{22}$ , really the first normal stress difference • $\\mathrm{{N}}_{1}$ usually exerts an outward (positive) force as measured in cone and plate rheometer Can make a difference to brush drag and other properties.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 18,
|
||||
"chunk": "# Extensional viscosity \n\n• Unusually high extensional viscosity shows up in systems that contain high molecular weight, flexible polymers in solution. \n\n– causes roller spatter and poor atomization – Stabilizes thick and long strings of paint behind roller, therefore big spatter drops \n\n• This is an extension property - not a shear property Elongational viscosity $\\mathbf{\\Psi}=\\mathbf{\\Psi}$ stress difference / elongation rate \n\n• Even Newtonian materials have viscosity in extensional flows $\\mathbf{\\tau}=3\\mathbf{x}$ shear viscosity \n\nCopyright S. G. Croll, NDSU",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 19,
|
||||
"chunk": "# Dr. Glass’ work (Union Carbide and NDSU) \n\n \nFigure3.17.Fiber development inrollcoating a high extensional viscosity paint.(From Ref.[29], withpermission.) \n\nHigh extensional viscosity means that the fibers become large before they break into large spatter droplets, and leave greater roller stipple on the painted surface.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 20,
|
||||
"chunk": "# Rheometers $\\mathbf{\\tau}=\\mathbf{\\tau}$ Viscometers",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 21,
|
||||
"chunk": "# Brookfield: rotating disk or spindle \n\nimposes a shear-rate field (rate varies across the disk) \nmeasures the resistance, gives shear stress \nCalibrated to give viscosity – Needs periodic calibration – Fluid container must be bigger than disk or spindle and provide good clearance underneath \nQuite useful and accurate but cannot impose much shear stress or rate - limited in application \n\n \nCopyright S. G. Croll, NDSU",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 22,
|
||||
"chunk": "# Stormer Viscometer \n\n \n\nImposes a shear stress (very approximately) \nusing vanes that move through the fluid at \n200 r.p.m. \nRotation rate usually monitored by stroboscope \nMeasure the weight that maintains this rotation rate \nResult is given in Krebs units (KU)ASTM \nD562 - difficult to relate to any other, \nscientific unit for viscosity \nOriginally intended to emulate stirring \nOften 90-100 KU is held to provide good brush pick-up performance and is used as a target for the lower shear-rate performance of an architectural paint \n\nCopyright S. G. Croll, NDSU \n\n \nCopyright S. G. Croll, NDSU",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 23,
|
||||
"chunk": "# Efflux Cups \n\n• Measure the time taken for a standard quantity of fluid to pour out of the bottom. • Result is usually given in seconds • Used in Quality Control more than anything else, for low viscosity, sprayed paints! – Common type is the Ford No. 4 cup.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 24,
|
||||
"chunk": "# Schematic of Ford Cup, number 4 \n\n \nCopyright S. G. Croll, NDSU",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 25,
|
||||
"chunk": "# Scientific Viscometers \n\nThese impose rigorous shear stresses or shear-rates, usually in a rotation sense. Possibilities: \n\n$\\succ$ Steady ramps \n$\\blacktriangleright$ Constant levels \n$\\succ$ Sinusoidal stresses or shear-rates \n$\\succ$ Or combinations \n\nUsually, a wide range of stress or shear-rate is available with very sensitive transducers for measuring the response. \n\nTwo geometries are common (I) cone and plate (best defined strain-rate and stress) (II) parallel plate (can achieve higher shear-rates) \n\nTwo types are used: \n\n(I) controlled stress is the input, resultant shear-rate is measured - most common \n(II) controlled shear-rate is the input, stress is measured. - requires bigger motors, more expensive",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 26,
|
||||
"chunk": "# Cone and Plate Geometry \n\n \nCopyright S. G. Croll, NDSU",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 27,
|
||||
"chunk": "# Cone and Plate Geometry \n\n• Shear Stress is given by: \n\n$$\n\\tau=\\frac{3T}{2\\pi r^{3}}\n$$ \n\n$\\mathrm{{T}=}$ torque $r=$ radius of cone \n\nShear-rate is given by: γ = $\\dot{\\gamma}=\\frac{\\omega}{a}$ \n\nWell defined while the angle is less $\\sim4^{\\circ}$ $\\boldsymbol{\\upomega}\\ =$ rotational speed, radians/second ${\\mathfrak{a}}=$ cone angle, radians (see previous slide)",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 28,
|
||||
"chunk": "# “I.C.I” Viscometers \n\nDeveloped by I.C.I Ltd (Imperial Chemical Industries, UK) (paints division now part of AkzoNobel and PPG). \n\n \n\n• Cone and plate viscometers with single or defined range of shear rates \n\n• Most common form is the model that operates at a shear rate of $10,000\\ \\mathbf{s}^{-1}$ Gauges performance in application process, e.g. brushing etc. \n\nSupplied by instrument makers. \n\nhttp://www.researchequipment.com/researchequipment.html",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 29,
|
||||
"chunk": "# Bubble Viscometers \n\nBubble rises at a speed that can be \nused to calculate a viscosity Usually determined by comparison to a standard \n\n \nCole-Parmer \n\nQuick and simple but useful only for clear solutions, resins, varnishes \n\n• Usually reported by the letter grade of the standard closest in bubble speed, A5 through Z10, (0.005 to 1,000 Stokes) ASTM D1131, D1545, D1725 Tubes do have marks, so a timing can be done and a result calculated in standard viscosity units Sets of sealed standards are available, open tubes for your sample, and a holder so that sample tubes are inverted at same time as the standard Accurate provided that temperature does not vary too much and the bubble shape remains stable. \n\nCopyright S. G. Croll, NDSU",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 30,
|
||||
"chunk": "# Solution Viscosity \n\n• Overall, solution viscosity depends on: \n\n– Temperature \n– Molecular weight \n– Molecular weight distribution \n– Solvent viscosity \n– Polymer-solvent interactions \n– Concentration",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 31,
|
||||
"chunk": "# Resin Solutions \n\nHigher molecular weight resins within about $100^{\\circ}\\mathrm{C}$ of their $T_{g}$ seem to follow a WLF (Williams-Landel-Ferry) type of dependence, as do lower molecular weight resins at all temperatures: \n\n$$\nl n\\ \\eta=\\eta_{r}-{\\frac{c_{I}\\left(T-T_{r}\\right)}{c_{2}+{\\left(T-T_{r}\\right)}}}=27.6-{\\frac{A{\\left(T-T_{g}\\right)}}{B+{\\left(T-T_{g}\\right)}}}\n$$ \n\n• Subscript $^{\\ast}\\mathrm{r}^{\\ast}$ means some curve-fitted reference value. There are “universal” values if one uses the $T_{g}$ of the polymer as the reference. $\\mathrm{A}{\\sim}17.44$ and $\\mathrm{B}{\\sim}51.6$ Important variable is the difference between the actual temperature and $\\mathrm{T_{g}}$ .",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 32,
|
||||
"chunk": "# Resin Solutions \n\n• Lower $\\mathrm{T_{g}}$ leads to lower viscosity – Polymer is more flexible and thus poses less resistance to flow. \n\n• At even higher temperatures and molecular weights the temperature dependence is closer to Arrhenuis: \n\n$$\nl n\\eta{=}l n A^{\\prime}+\\frac{E_{\\nu}}{R T}\n$$ \n\n \nFigure 3.12. Viscosity dependence of standard liquid BPA epoxy resin on temperature. (From Ref.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 33,
|
||||
"chunk": "# Dilute Solutions \n\n• If a solution is dilute, i.e. the polymer molecules act independently, the solution viscosity can be expressed as: \n\n$$\nl n~\\eta_{\\boldsymbol{r}}=\\left[\\pmb{\\eta}\\right]c+\\left[\\pmb{\\eta}\\right]^{2}c^{2}\n$$ \n\n$\\eta_{r}$ is the solution viscosity/solvent viscosity $\\mathbf{\\Sigma}=$ relative viscosity \n\nThe intrinsic viscosity [] depends on the temperature (naturally) and the hydrodynamic volume swept out by the polymer molecule - which in turn depends on the molecular weight: \n\nMark-Houwink-Skarada equation. $a$ goes from 0.3 to ${\\sim}0.8$ \n\n$$\n\\scriptstyle{[\\pmb{\\eta}]=\\pmb{K}\\pmb{M}^{a}}\n$$",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 34,
|
||||
"chunk": "# Characterizing Polymers in Dilute Solutions \n\n• The Intrinsic Viscosity [] is defined by: \n\n$$\n\\eta_{r e l}=\\frac{\\eta}{\\eta_{s}}=1+\\big[\\eta\\big]c+k c^{2}+\\dots\n$$ \n\nan alternative to equation on previous slide. \n\n• It is measured by viscosity measurements taken on a succession of dilute concentration solutions in capillary viscometers (very accurate) – usually in a tightly controlled temperature bath. \n\nCopyright S. G. Croll, NDSU \n\n",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 35,
|
||||
"chunk": "# Concentrated Solutions \n\n• There is not so much simplicity on the dependence of the viscosity on concentration: \n\n$$\nl n\\eta_{r}=\\frac{w_{r}}{k_{I}-k_{2}w_{r}+k_{3}w_{r}^{2}}\n$$ \n\n• This equation works fairly well, $w_{r}=$ weight fraction of the polymer; sometimes simpler equations are fine. \n• Polymer molecules extend in good solvents and thereby increase viscosity - choice of solvent is crucial. Poor solvents cause polymer molecules to coil upon themselves, and if the solvent is poor enough - the polymer comes out of solution.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 36,
|
||||
"chunk": "# Dispersion Viscosity \n\nDilute suspensions adhere well to Einstein’s equation: $\\eta_{r}=1+2.5\\phi$ Where $\\phi=$ volume fraction of the suspended particles $\\mathrm{\\sim}<0.1$ The factor of 2.5 assumes that the particles are spheres. \n\nFor more concentrated suspensions other equations have been proposed. The most common are, (i) the Mooney equation: \n\n$$\n\\eta_{\\mathrm{~r~}}=e x p\\left[\\frac{2.5\\phi}{I\\mathrm{~-~}\\displaystyle\\frac{\\phi}{\\phi_{\\mathrm{~m~}}}}\\right]\n$$ \n\nAnd, the most successful is (ii) the Krieger-Dougherty equation, but see next slide: \n\n$$\n\\eta_{r}=\\left(I-\\frac{\\phi}{\\phi_{m}}\\right)^{-2.5\\varphi_{m}}\n$$ \n\nCopyright S. G. Croll, NDSU \n\n \nCopyright S. G. Croll, NDSU",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 37,
|
||||
"chunk": "# How the behavior of a suspension will change with concentration \n\n \nJ. M. Brader, “Nonlinear rheology of colloidal dispersions,” J. Phys.: Condens. Matter 22 (2010) 363101 \nFigure 3. A schematic illustration of the phase diagram of hard-spheres as a function of volume fraction. Monodisperse systems undergo a freezing transition to an FCC crystal with coexisting densities $\\phi=0.494$ and 0.545. Polydispersity suppresses the freezing transition resulting in a glass transition at $\\phi\\sim0.58$ ,which lies below the random-close-packing value of $\\phi\\sim0.64$",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 38,
|
||||
"chunk": "# Dispersion Viscosity \n\n• Both the Mooney equation and the Krieger-Dougherty equations exhibit infinite viscosity at the maximum packing fraction, $\\Phi_{\\mathrm{m}}$ . The maximum packing fraction is a geometric constraint on the number of particles that can be accommodated in a given arrangement. \n0.63 – dense random packing of spheres (good 1st. choice for rheology) \n0.59 – loose random packing of spheres (good second choice) \n0.52 – simple cubic packing of spheres \n0.74 – hexagonal close packing of spheres \nFlakes, discs and rods may tumble and get in each others way so $\\Phi_{\\mathrm{m}}$ can be as low as 0.1. \n\nFlocculation usually incorporates solvent into the aggregates and so effectively increases the volume fraction of the solids and so the viscosity becomes much higher. \n\nCopyright S. G. Croll, NDSU",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 39,
|
||||
"chunk": "# Possible Advance in Rheology of Dispersions (and Granular Matter) \n\n• F. Boyer, E. Guazzelli, O. Pouliquen, “Unifying Suspension and Granular Rheology,” PRL 107, 188301 (2011) Different, but successful form of the equations for the relative viscosity of dispersions. Draws common ground between suspension and granular flow with viscous and collision contributions. \n\n \n$\\eta_{n}$ correlations of Eilers (red dashed line) and Krieger-Dougherty $\\eta_{s}$ $\\eta_{\\ast}$",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 40,
|
||||
"chunk": "# Analytical Use of Rheology \n\n• QC and Control – is it the same as the control material? – Best done at low shear rates (see below) \n\n• High Shear Rate viscosity – Will it flow/atomize well in the equipment and with the power available? \n\n• Low Shear Rate viscosity \n\n– Low shear rates do not break down flocculation or other interactions, so it is good at detecting when materials or their behavior are different \n– Very sensitive to material differences but only diagnostic by comparison with known control materials \n\nCopyright S. G. Croll, NDSU",
|
||||
"category": " Materials and methods"
|
||||
}
|
||||
]
|
||||
52
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@@ -0,0 +1,87 @@
|
||||
[
|
||||
{
|
||||
"id": 1,
|
||||
"chunk": "# Synthesis and characterization of UV curable urethane acrylate oligomers containing ammonium salts for anti-fog coatings \n\nJ.W. Hong a, H.K. Cheon a, S.H. Kim a, K.H. Hwang a, H.K. Kim b,∗ \n\na Department of Biochemical and Polymer Engineering, Chosun University, Gwangju 501-759, South Korea b Institute of Photonics &Surface Treatment, Q-Sys Co.Ltd., Gwangju, 61007, South Korea",
|
||||
"category": " Abstract"
|
||||
},
|
||||
{
|
||||
"id": 2,
|
||||
"chunk": "# a r t i c l e i n f o",
|
||||
"category": " Abstract"
|
||||
},
|
||||
{
|
||||
"id": 3,
|
||||
"chunk": "# a b s t r a c t \n\nArticle history: \nReceived 12 August 2016 \nReceived in revised form 2 March 2017 \nAccepted 6 March 2017 \nAvailable online 15 May 2017 \n\nKeywords: \nUV-curing \nAnti-fog \nPhoto-DSC \nSalts \nCoating properties \n\nUV-curable urethane acrylate oligomer (UV-UAO) containing ammonium salts, suitable for anti-fog (AF) coatings was synthesized. The expected UV-UAO structure was confirmed by FT-IR and $^1\\mathrm{H}$ NMR. This UVUAO was then formulated with reactive monomers and photoinitiator to form coating formulas. In order to compare the UV-curing behavior of UV-UAO with conventional oligomers, the photopolymerization of UV-UAO and SK cytech EBECRYL-series urethane acrylates (EB 8210 and EB 9260) was investigated by photo-differential scanning calorimetry (Photo-DSC). The anti-fog properties of UV-cured AF coating were investigated by contact angle test and anti-fog test. Coating properties such as pencil hardness, pendulum hardness, gloss, and adhesion of the UV-cured films containing UV-UAO were investigated. The results showed that the concentration of UV-UAO in the coating formulation had a great influence on the anti-fog properties of UV-cured AF coating. Especia lly, UV-cured AF coating containing UV-UAO 65 wt.% showed excellent anti-fog properties without sacrificing other desirable properties such as pencil hardness and adhesion. \n\n$\\mathfrak{C}$ 2017 Elsevier B.V. All rights reserved.",
|
||||
"category": " Abstract"
|
||||
},
|
||||
{
|
||||
"id": 4,
|
||||
"chunk": "# 1. Introduction \n\nIn the past several years, there has been increasing interest in anti-fog coatings. In general, fog occurs when the difference between air temperature and dew point is generally less than $2.5^{\\circ}\\mathsf{C}.$ This fog begins to form when water vapor condenses onto a surface to form discrete and dispersed light–diffusing water droplets, thereby restricting light transmission and optical efficiency [1]. This undesirable fogging phenomenon occurs frequently on optical materials that are in use in everyday life such as bathroom mirrors, eyeglasses, safety glasses, swimming goggles, windshields, camera lenses, and skis as well as on analytical and medical instruments. In order to overcome this predicament, a method of applying an anti-fog treatment on the surface has been suggested. \n\nThe basic concept of anti-fog is to create a hydrophilic surface that prevents the condensation of water in the form of small droplets so that light can transmit directly free of interference from scattering by the water droplets. In the early stages of anti-fog coating development, non-reactive anti-fog agents were conventionally introduced into a polymer matrix without chemical bonding. However, they do not produce stable long-term anti-fog properties because the anti-fog agents can be easily wiped off or partially lost during cleaning. \n\nAccordingly, various materials and processes have been suggested for durable anti-fog coatings. For example, Maechler et al. have reported on a multilayer transparent anti-fog coating on a polycarbonate (PC) [2]. Nuraje at al. have reported on mechanically durable, long-lasting antifog coatings based on polysaccharides [3]. Cebeci et al. prepared stable superhydrophilic nanoporous thin films fabricated from layer-by-layer assembled silica nanoparticles and a polycation [4]. Chang et al. have developed a special hydrophilic/hydrophobic bilayer structure [5]. Yuan et al. have reported on UV curable hydrophilic acrylate polymers containing a sulfonic acid group for anti-fog coatings [6]. However, many of these fabrication processes involve complicated multi-steps and are often time consuming, which poses a hindrance for practical application. Accordingly, our research interest is to develop UV curable anti-fog coatings that can be obtained without the need for cumbersome and complicated synthesis and fabrication processes. This UV curable coating also offers other advantages such as higher productivity, energy savings, and lower capital investment for curing facilities. \n\nIn this study, UV curable urethane acrylate oligomer containing ammonium salts for anti-fog coating was developed, and its antifog effectiveness and the surface properties of the coating network were investigated. \n\n \nScheme 1. Preparation of Ammonium Salt Monomer.",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 5,
|
||||
"chunk": "# 2. Experimental",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 6,
|
||||
"chunk": "# 2.1. Materials \n\nThe monomers, including ethanolamine, and 2-butanone were purchased from Aldrich Chemicals and purified by vacuum distillation. SY-40M (glycidyl ether of C12 and C14 alcohol) was purchased from Sakamoto Yakuhin Kogyo Co., Ltd. (Japan), and was used without purification. Dimethyl sulfate was purchased from Aldrich Chemicals and purified by vacuum distillation prior to use. Isophorone diisocyanate (IPDI) was purchased from Evonik. Dibutyltin dilaurate (DBTDL) was purchased from Air Products. TLC Silica gel $60\\mathsf{F}_{254}$ (Merck) was used for TLC analysis. Pentaerythritol triacrylate (PETA) and dipentaerythritol hexaacrylate (DPHA) were all supplied by Miwon Specialty Chemical Co., Ltd. (Korea).",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 7,
|
||||
"chunk": "# 2.2. Synthesis of ammonium salt (AS) monomer \n\nEthanolamine $\\cdot10.16\\mathrm{g},0.166\\mathrm{mol}$ ) was added to a $250\\mathrm{mL}$ threeneck flask equipped with water bath, thermometer, refluxing condenser, dropping funnel, and magnetic stirring bar, and heated to $60^{\\circ}C$ with stirring. $86.55{\\mathrm{g}}$ of alkyl glycidyl ether (Sy 40M) was slowly added and the mixture was maintained for $^{2\\mathrm{h}}$ at $70^{\\circ}\\mathsf C$ . Dimethyl sulfate $\\cdot20.99,0.166\\mathrm{mol}$ ) and methyl ethyl ketone (MEK, $29.8{\\mathrm{g}}{\\mathrm{,}}$ were added dropwise to the stirred mixture over $3\\ensuremath{\\mathrm{h}}$ , while maintaining the temperature at $60^{\\circ}\\mathsf C.$ The salt group of the final product was identified by the titration of the remaining amine group with $0.1\\mathsf{N}$ HCl solution. $80\\%$ of the total amine group was converted into quaternary ammonium group. The reaction product was identified with $^1\\mathrm{H}$ NMR $(\\mathsf{C D C l}_{3}$ , ${300}\\mathrm{MHz}\\mathrm{\\cdot}$ ): 4.17 ppm $(\\mathrm{N^{+}{-}C H_{2}C\\underline{{{H}}}(-0H){-}C H_{2}})$ , $4.01\\mathrm{ppm}$ $(\\mathsf{N}^{+}{-}\\mathsf{C H}_{2}\\mathsf{C}\\underline{{H}}20\\mathsf{H})$ , 3.52 ppm $(\\mathrm{CH}_{2}\\mathrm{CH}(-0\\mathrm{H}){-}\\mathrm{C}\\underline{{{H2}}}{-}0),$ 3.43 ppm $(\\mathsf{N}{+}{-}\\mathsf{C}\\underline{{H}}_{2}\\mathsf{C}\\mathsf{H}_{2}{0}\\mathsf{H})$ , 3.39 ppm $\\left(\\mathsf{N}^{+}{-}\\mathsf{C}\\underline{{H}}_{2}\\mathsf{C}\\mathsf{H}(\\mathsf{O}\\mathsf{H})\\mathsf{C}\\mathsf{H}_{2}\\right)$ , 3.29 ppm ( $\\left(\\mathsf{N}^{+}{-}\\mathsf{C}\\underline{{{H_{3}}}}^{\\cdot}$ ), 1.22 ppm ${\\mathrm{O}}({\\mathrm{CH}}_{2}){\\mathrm{C}}\\underline{{{H}}}_{3};$ (Scheme 1).",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 8,
|
||||
"chunk": "# 2.3. UV-curable urethane acrylate oligomer (UV-UAO) with ammonium salt \n\nTo a solution of IPDI $\\left(34.5\\mathrm{g},0.16\\mathrm{mol}\\right)$ ), and PETA $(100\\mathrm{g})$ in MEK $\\mathrm{\\cdot100mL)}$ , DBTDL $(0.25{\\mathrm{g}})$ was added dropwise at $10^{\\circ}\\mathsf C$ with stirring. After complete addition, the mixture was stirred at $10^{\\circ}\\mathsf C$ for $\\boldsymbol{4\\mathrm{h}}$ . The reaction progress was analyzed by TLC using ethyl acetate: hexane $=1{:}2$ $(\\nu/\\nu)$ . And then, the AS monomer $(96.2{\\mathrm{g}})$ in MEK $(20\\mathrm{mL})$ was added to the above reaction product over 4 h, while maintaining the temperature at $20^{\\circ}\\mathsf C$ The reaction product was identified with $^1\\mathrm{H}$ NMR ( $\\mathrm{\\CDCl}_{3}$ , ${300}\\mathrm{MHz}^{\\cdot}$ and FT-IR: $^1\\mathrm{H}$ NMR $(\\mathsf{C D C l}_{3})$ ): 7.9 ppm $(-\\mathsf{N}H-)$ , $6.35{-}6.25\\mathrm{ppm}$ $\\scriptstyle(-{\\mathsf{C H}}={\\mathsf{C}}{\\underline{{H_{2}}}}$ ), $5.81{-}5.72\\mathrm{ppm}$ $\\scriptstyle(-{\\mathsf{C H}}={\\mathsf{C}}{\\underline{{{H_{2}}}}}$ ), $6.03\\substack{-5.92\\mathrm{ppm}}$ $(\\mathrm{-}\\mathsf{C}\\underline{{H}}\\mathrm{=}\\mathsf{C}\\mathsf{H}_{2}$ ); FT-IR spectrum: $-\\mathsf{N H}$ stretching $3300\\mathsf{c m}^{-1}$ ), ${\\mathsf{C}}{\\mathrm{-}}{\\mathsf{H}}$ deformation mode of the acryl groups $(811\\mathrm{cm}^{-1}$ ) (Scheme 2).",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 9,
|
||||
"chunk": "# 2.4. Coating formulation and curing procedure \n\nUV curable anti-fog (AF) compositions were prepared by mixing homogenously UV-UAO with reactive diluents (PETA:DPHA $_{.=8.5:1.5}$ by weight) and the photoinitiator (1- Hydrophenyl ketone, Irgacure 184 from Ciba Specialty Chemicals, maximum peak of absorption: $245{-}330\\mathrm{nm}$ ). Different amounts of UV-UAO $(55-70\\mathrm{wt}.\\%)$ were added into the above composition and the photoinitiator concentration was kept constant at $5\\mathrm{wt.\\%}$ all on the basis of final formulation. A $20\\mathrm{-}\\upmu\\mathrm{m}$ thick coating of the resin composition was applied on the polycarbonate (PC) using bar applicator and then cured with $80\\mathsf{W/c m}$ light a medium pressure mercury lamp of conventional UV equipment.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 10,
|
||||
"chunk": "# 2.5. Water contact angle and anti-fog tests \n\nThe water contact angle of the UV-cured AF coating surface was determined by an SEO 300A from Surface & Electro-Optics Co., Ltd. This system is based on the sessile drop method. Temperature and relative humidity in the laboratory were within the range of \n\n \nScheme 2. Preparation of UV-UAO. \n\n$21^{\\circ}\\mathsf{C}_{-}25^{\\circ}\\mathsf{C}$ and $30\\%$ , respectively. DI water was used as probing liquids. \n\nAnti-fog properties were evaluated through two separate testing methods: First, a steam anti-fog test is done as follows. Hot water $(80^{\\circ}\\mathsf{C})$ was added into a cup to about half full. Then, the sample was placed on the cup with the coated surface facing down. Vapor condensed on the coating surface was observed and photographed [5]. Second, a cold anti-fog test is done as follows. The sample was put into a $-20^{\\circ}C$ refrigerator for 1 h and taken out in a $50\\%$ humidity environment.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 11,
|
||||
"chunk": "# 2.6. Curing monitoring and coating properties \n\nThe different photo calorimetry (Photo-DSC) experiments were conducted using a differential scanning calorimeter equipped with a photocalorimetric accessory (TA 5000/DSC 2920). The initiation light source was a 200 W high-pressure mercury lamp: the UV light intensity at the sample was $35\\mathrm{mW}/\\mathrm{cm}^{2}$ over a wavelength range of $200{-}440\\mathrm{nm}$ . The sample was placed in uncovered aluminum pans. TA Instruments software was employed to obtain the results from the photo-DSC experiments. \n\nmeasured on Leneta test papers using a gloss meter from Sheen Co. (ASTM D 523). The recorded values were an average of five measurements. The adhesion of the coating was measured by using the cross-cut kit by Precision Gage & Tool Co. as described in ASTM D3359. A crosshatch pattern is made through the film to the substrate. Pressure-sensitive tape is applied over the crosshatch cut. Tape is removed by pulling it off rapidly back over itself at close to an angle of $180^{\\circ}$ . Adhesion is assessed on a 0–5 scale. Then the adhesion test was examined before the anti-fogging tests at $25^{\\circ}\\mathsf{C}$ and under relative humidity $30\\%$ . \n\nThe surface hardness of the cured film was measured by using graphite pencils of increasing hardness as described in ASTM D 3363-74. Pendulum hardness (ASTM D4366-84) was measured as the time taken for the oscillations of a pendulum to reduce from $6^{\\circ}$ to $3^{\\circ}$ (König ref. 707KP from Sheen). The gloss of the coating was",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 12,
|
||||
"chunk": "# 3. Results and discussion",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 13,
|
||||
"chunk": "# 3.1. Curing behavior of UV-UAO \n\nThe UV-curing behavior of the synthesized UV-UAO was compared with that of SK cytech EBECRYL-series urethane acrylate oligomers commonly used in UV-curable systems by Photo-DSC. The photo-DSC exotherms for the photopolymerization of EB 8210, EB 9260, and UA-UAO are illustrated in Fig. 1. The filled circles, open circles, and filled downward triangles are the measured heat flow of EB 8210, EB 9260, and UV-UAO, respectively. From the peak symmetry, induction time, and the time to peak maximum, one can obtain information such as the optimum ratio of monomer to oligomer, the photoinitiator efficiency, and the curing rate [7]. The amounts of heat released, induction time, peak to maximum, and the ultimate percentage conversions derived from Fig. 1 are collected in Table 1. \n\n \nFig. 1. Photo-DSC exothermic curves for the photopolymerization of EB 8210, EB 9260, and UV-UAO. \n\nTable 1 Data from photo-DSC studies on EB 8210, EB 9260, and UV-UAO (IT, induction time; PM, time to peak maximum). \n\n\n<html><body><table><tr><td>Sample</td><td>Functionality</td><td>Mw (g/mol)</td><td>△H (J/g)</td><td>IT (s)</td><td>PM (s)</td><td>Conversion (%)</td></tr><tr><td>EB8210</td><td>4</td><td>600</td><td>310</td><td>1.00</td><td>1.98</td><td>83</td></tr><tr><td>EB 9260</td><td>3</td><td>1500</td><td>163</td><td>1.08</td><td>1.98</td><td>58</td></tr><tr><td>AF-UAO</td><td>3</td><td>830</td><td>154</td><td>1.10</td><td>2.58</td><td>53</td></tr></table></body></html> \n\nTable 2 Curing Parameters of UV-cured AF coatings. \n\n\n<html><body><table><tr><td>Sample</td><td>AF1</td><td>AF2</td><td>AF3</td><td>AF4</td></tr><tr><td>UV-UAO content (%)</td><td>55</td><td>60</td><td>65</td><td>70</td></tr><tr><td> H(J/g)</td><td>302</td><td>298</td><td>287</td><td>208</td></tr><tr><td>Induction Time (sec)</td><td>1.12</td><td>1.00</td><td>0.96</td><td>1.02</td></tr><tr><td>Time to Peak Maximum (sec)</td><td>2.76</td><td>1.98</td><td>1.92</td><td>2.34</td></tr><tr><td>Conversion (%)</td><td>75</td><td>74</td><td>70</td><td>59</td></tr></table></body></html> \n\nAs expected, the results show (Table 1) that tetra functional EB 8210 with low molecular weight has the shortest induction time and the shortest time to peak maximum as well as the highest value of $\\Delta{\\sf H}$ , indicating the fastest reaction system. Meanwhile, the synthesized UV-UAO and EB 9260 have a similar value for induction time, and UV-UAO has the longest time to peak maximum. In addition, the conversion of the UV-UAO is lower than that of EB 8210 and EB 9260, as shown by the lower value of $\\Delta{\\sf H}$ . This may be a result of the steric effect of quaternary ammonium salts. As shown, although the photopolymerization efficiency of the UV-UAO is lower than that of the commercially available EB 8210, it is similar to that of EB 9260 under the same experimental conditions. Therefore, it is obvious that the synthesized UV-UAO is suitable for practical use in UV coating formulations as the oligomer. \n\nAt this point, it is necessary to investigate the effects of UV-UAO concentration on the curing behavior of the UV-curable coating formulations. The photo-DSC exotherms for photopolymerization containing variable concentrations of UV-UAO in the coating formulations are shown in Fig. 2; while the amount of the measured heat flow, the induction time, the time to peak maximum, and the ultimate percentage conversion are collected in Table 2. \n\nHeat flow and percentage conversion decrease as the concentration of UV-UAO increases (Fig. 2 and Table 2); however, the AF3 containing $65\\%$ of UV-UAO has the shortest induction time and the shortest peak maximum, indicating that the initial curing rate is faster than that of the other AF samples. Although the mechanism for this improved initial curing rate is not clear yet, it can be tentatively explained as follows: The addition of UV-UAO into the UV coating formulation increases slightly the viscosity of the AF coating formulation. In general, it is known that increasing the viscosity of the coating decreases the oxygen diffusion into the coating and improves the surface cure [8]. Therefore, it could be expected that the improved curing rate may be attributed to oxygen inhibition. In addition, there is a sudden drop in curing properties as the UV-UAO concentration is increased above $65\\%$ . It is supposed that there are potential incompatibility problems with other components present in the coating formulation. \n\n \nFig. 2. Photo-DSC exotherms for the photopolymerization of formulations AF1-AF4. \n\n \nFig. 3. Steam anti-fog test of uncoated PC (left) and formula AF 3 coated PC (right).",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 14,
|
||||
"chunk": "# 3.2. Antifogging properties \n\nIn order to investigate the anti-fog properties of the prepared UV-cured anti-fog (AF) coatings containing variable concentrations of UV-UAO in the coating formulations, the water contact angle and AF tests of UV-cured AF coatings were examined under a variety of different fogging conditions and the results are summarized in Table 3. The neat PC surface is relatively hydrophobic with a high water contact angle of $74^{\\circ}$ , and the AF test shows a fog appearance (Figs. 3 and 4). After applying a UV-cured AF coating on PC, the water contact angle drops markedly from $58^{\\circ}$ to $5^{\\circ}$ as the content of UV-UAO in the formulation increases from $55\\%$ to $70\\%$ (Table 3). Especially, the AF 3 and AF4 with $65\\%$ and $70\\%$ of UV-UAO in the formulation exhibited lower static water contact angle values $\\mathrm{\\cdot}\\mathrm{AF}3=6^{\\circ}$ , ${\\mathsf{A F}}4=5^{\\circ}$ ) than the AF 1 and AF 2, suggesting that the addition of the UV-UAO into the coating formulation was effective for increasing the surface hydrophilicity of the hydrophobic PC substrate. The hydrophilic OH group and quaternary ammonium salts of UV-UAO were expected to provide excellent anti-fog capability to the coating film because both groups are able to imbibe water on the surface layer, and this hydrophilic surface decreases the water droplet contact angle and provides the anti-fog performance. \n\nTable 3 Anti-fog test and coating properties of UV-cured AF coatings. \n\n\n<html><body><table><tr><td colspan=\"2\">Sample</td><td>AF1</td><td>AF2</td><td>AF3</td><td>AF4</td></tr><tr><td rowspan=\"2\">Contact Angle（°）</td><td>Initial</td><td>58</td><td>50</td><td>6</td><td>5</td></tr><tr><td>After water soaking</td><td>56</td><td>49</td><td>5</td><td>Partly detached</td></tr><tr><td rowspan=\"2\">Antifog performance</td><td>Cold-fog test</td><td>fogging</td><td>Some -fogging</td><td>Anti-fog</td><td>Anti-fog</td></tr><tr><td>Steam-fog test</td><td>fogging</td><td>Some -fogging</td><td>Anti-fog</td><td>Anti-fog</td></tr><tr><td colspan=\"2\">Pendulum Hardness</td><td>208</td><td>213</td><td>228</td><td>203</td></tr><tr><td colspan=\"2\">Pencil Hardness</td><td>1H</td><td>1H </td><td>2H</td><td>1H</td></tr><tr><td colspan=\"2\">Gloss</td><td>133.5</td><td>134.8</td><td>135.2</td><td>135.5</td></tr><tr><td colspan=\"2\">Adhesion/cross-cuta</td><td>0</td><td>0</td><td>0</td><td>3</td></tr></table></body></html>\n\na 0: The edges of the cuts are completely smooth; none of the squats of the lattice are detached, 3: A cross-cut area significantly greater than $15\\%$ , but not significantly greater than $35\\%$ , is affected. \n\n \nFig. 4. Cold anti-fog test of uncoated PC (left) and AF 3 coated PC (right) after removal from $-20^{\\circ}C$ freezer to humid environment. \n\nIn practice, the durability of AF coatings is of major concern, in addition to the initial water wettability, particularly when the coating is to be used in high humidity conditions. In this regard, in order to test anti-fog durability, various AF coatings were soaked in water for an extended period of time. It was found that AF 4 with $70\\%$ UV-UAO content cannot withstand long-term water soaking with the AF layer of the AF 4 detaching partly from the PC substrate after being immersed in water for 1 day at $25^{\\circ}\\mathsf C$ whereas AF 3 with good water wettability and anti-fog performance retains its outstanding anti-fog durability (Table 3). \n\nThe anti-fog performance of the AF 3 coatings is shown by the steam-fog test and the cold-fog test, and AF 1 and AF 2 do not exhibit acceptable anti-fog performance (Table 3). In the case of AF 4, excellent anti-fog ability was observed in the initial stages; however, it did not provide anti-fog durability. In contrast, AF 3 provided excellent antifogging capability under a variety of different fogging environments. In the steam fog test, the formula AF 3 coated PC (right part) was seen clearly and retained good transparency; however, the uncoated PC (left part) fogged immediately (Fig. 3). A more aggressive cold-fog test was performed by placing the AF 3 coated PC and the uncoated PC in a freezer at $-20^{\\circ}C$ for 1 h. Both samples were then removed into a humid environment. The uncoated PC (left part) was wholly fogged; however, the AF 3 coated PC (right part) remained fog free (Fig. 4). \n\n \nFig. 5. FTIR-ATR spectra of UV-cured AF films at the film-air interfaces: (a) AF 1 (UV-UAO 55 wt.%); (b) AF 2 (UV-UAO 60 wt.%); (c) AF 3 (UV-UAO 65 wt.%). \n\nHenceforth we will not discuss AF 4 because its anti-fog properties and conversion from Photo-DSC are outside the specification required in this paper.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 15,
|
||||
"chunk": "# 3.3. Coating properties and degree of surface curing \n\nSince pencil hardness and pendulum hardness are determined primarily by structural parameters such as cross-link density, it is appropriate to consider the cross-link density of the samples [9,10]. It is known that PC is relatively soft and tough with a pencil hardness $<2\\tt B$ . After being coated with AF coating formulation containing UV-UAO, its hardness was raised to 2H (AF 3 coating), which is sufficiently high for general purposes. Among the UV-cured AF coatings, AF 3 exhibited the highest pendulum and pencil hardness compared with the other AF coatings (Table 3), suggesting that the cross-link density of the AF 3 is higher than that of the other AF coatings. \n\nIn order to confirm the above results, the unreacted acrylic double bonds at the film-air interface of the UV-cured AF coating films were measured by FTIR-ATR, and the results showed clearly (Fig. 5) \n\nthat the intensity at $811\\mathrm{cm}^{-1}$ decreases with increasing amounts of UV-UAO. Since the infrared band at $811\\mathrm{cm}^{-1}$ is attributable to the $C{\\mathrm{-}}\\mathrm{H}$ deformation mode of the acryl groups, it can be concluded that the addition of UV-UAO into the formulation increases the degree of surface curing. These FTIR-ATR results are in very good agreement with the results of the pencil and pendulum hardness tests. \n\nIn light of these results, it is evident that adding UV-UAO at $65\\%$ results in a cured film that achieves a good balance between anti-fog properties and hardness, two characteristics that are often difficult to achieve at the same time. \n\nWe then turned to other coating properties such as gloss and adhesion. All of the UV-cured AF films containing UV-UAO (except that with $70\\mathrm{wt\\%}$ of UV-UAO) exhibited excellent adhesive properties for PC (Table 3). Since adhesion was related to the ion content, the higher ion content in the UV-cured AF films may increase the ion strength, which may improve the adhesion between the film and the PC substrate. In addition, increasing the UV-UAO concentration from 55 wt. $\\%$ to 70 wt. $\\%$ produced no detectable difference in gloss (Table 3).",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 16,
|
||||
"chunk": "# 4. Conclusions \n\nThis work demonstrates that UV-UAO is a useful oligomer that can provide excellent anti-fog properties for a UV-cured coating under a variety of environmental conditions. Surfaces coated with a coating formulation containing UV-UAO are capable of spreading and absorbing water, thereby preventing fog formation on the optical substrate. Specially, AF 3 containing UV-UAO 65 wt. $\\%$ in a coating formulation achieves a good balance between anti-fog properties and surface hardness. This UV curable anti-fog coating with UV-UAO also offers desirable product features such as simple wet chemical application methods and a fast curing process for maximum process yields.",
|
||||
"category": " Conclusions"
|
||||
},
|
||||
{
|
||||
"id": 17,
|
||||
"chunk": "# References \n\n[1] J.A. Howarter, J.P. Youngblood, Macromol. Rapid Commun. 29 (2008) 455–466. \n[2] L. Maechler, C. Sarra-Bournet, P. Chevallier, N. Gherardi, G. Laroche, Plasma Chem. Plasma Process. 31 (2011) 175–187. \n[3] N. Nuraje, R. Asmatulu, R.E. Cohen, M.F. Rubner, Langmuir 27 (2011) 782–791. \n[4] F.C. Cebeci, Z. Wu, L. Zhai, R.E. Cohen, M.F. Rubner, Langmuir 22 (2006) 2856–2862. \n[5] C.C. Chang, F.H. Huang, H.H. Chang, T.M. Don, C.C. Chen, L.P. Cheng, Langmuir 28 (2012) 17193–17201. \n[6] Y. Yuan, R. Liu, C. Wang, J. Luo, X. Liu, Prog. Org. Coat. (2014) 785–789. \n[7] J.W. Hong, H.W. Lee, J. Korean Ind. Eng. Chem. 5 (1994) 860. \n[8] R. Schwalm, UV Coating: Basics, Recent Development and New Applications, 2007, pp. 179–184. \n[9] H.K. Kim, Y.B. Kim, J.D. Cho, J.W. Hong, Prog. Org. Coat. 48 (2003) 34–42. \n[10] H.K. Kim, H.T. Ju, J.W. Hong, Eur. Polym. J. 39 (2003) 2235–2241.",
|
||||
"category": " References"
|
||||
}
|
||||
]
|
||||
@@ -0,0 +1,92 @@
|
||||
[
|
||||
{
|
||||
"id": 1,
|
||||
"chunk": "# Synthesis of UV-curable acrylate polymer containing sulfonic groups for anti-fog coatings \n\nYan Yuan, Ren Liu, Chunlin Wang, Jing Luo, Xiaoya Liu ∗ \n\nThe Key Laboratory of Food Colloids and Biotechnology, Ministry of Education, School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122, China",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 2,
|
||||
"chunk": "# a r t i c l e i n f o \n\nArticle history: \nReceived 5 November 2013 \nReceived in revised form \n10 December 2013 \nAccepted 1 January 2014 \nAvailable online 23 January 2014 \nKeywords: \nUV-curable \nSulfonic group \nAcrylate \nAnti-fog",
|
||||
"category": " Abstract"
|
||||
},
|
||||
{
|
||||
"id": 3,
|
||||
"chunk": "# a b s t r a c t \n\nA series of UV curable hydrophilic acrylate polymers containing sulfonic acid group was prepared via free radical copolymerization using 2-acrylamido-2-methyl propane sulfonic acid (AMPS) as hydrophilic monomer, which were used as prepolymers for anti-fog coatings. The expected structures were confirmed by FT-IR, $^1\\mathrm{H}$ NMR and gel permeation chromatography (GPC). These UV-curable acrylate polymers were then mixed with reactive diluents and photoinitiator to form coating formulas. Various substrates were coated with these formulas and cured under UV exposure to obtain transparent coatings with good adhesion and hardness. The anti-fog properties of UV-cured coating were measured by contact angle test and anti-fog test. The results showed that the AMPS content in prepolymer had a great influence on the anti-fog properties of UV-cured coating. The formula was optimized and the corresponding UV-curing anti-fog coating was manufactured. The test results indicated that the coatings showed good mechanical properties, great optical transparency and excellent anti-fog performance. \n\n$\\mathfrak{C}$ 2014 Elsevier B.V. All rights reserved.",
|
||||
"category": " Abstract"
|
||||
},
|
||||
{
|
||||
"id": 4,
|
||||
"chunk": "# 1. Introduction \n\nWater vapor can condense on solid surface at a certain temperature or humidity, and water on surface forms little droplets if the solid surface has a very high surface energy. Therefore the light is refracted and scattered by water droplets and the transparent materials turn hazy, which causes fogging problems. Many optical devices are suffering from fogging problems, such as eyeglasses, mirrors, windshields and many other devices in special fields [1–4]. There are two efficient ways to solve the problem. One is to heat the device to make water vapor non-condensing, and the other is to provide the solid surface with wetting characteristics such as hydrophilicity [5] or even super hydrophilicity [6]. Although the former method is efficient, the cost of energy limits its wide application. \n\nHydrophilic surfaces that have contact angles with water of less than $40^{\\circ}$ are often explored as anti-fog coatings. The main reason is that condensing water droplets on this type of surface can rapidly spread into a uniform and non-light-scattering water film [7,8]. In this case, although condensation still occurs, the surface remains optically clear. The key to this approach is the use of materials which can strongly interact with water molecules and/or have a high capacity to absorb water. Hydrophilic polymeric systems containing hydroxyl groups $(\\mathrm{-OH})$ , amino group $\\left(\\mathrm{-NH}_{2}\\right).$ , carboxyl group ( COOH) or sulfonic group $(-S0_{3}\\mathrm{H})$ are often utilized in antifog formulas [9,10]. However, the preparation of optical quality thin-film coatings with these hydrophilic functionalities exhibiting both good coating characteristics and mechanical durability is still a great challenge. \n\nHerein, a new coating system with good anti-fog properties and mechanical properties was presented. This new coating system was based on a UV-curable hydrophilic polymer which was prepared via free radical copolymerization with 2-acrylamido-2- methyl propane sulfonic acid (AMPS) as hydrophilic monomer. After UV-curing, the resultant coating exhibited good anti-fog properties as well as good mechanical properties.",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 5,
|
||||
"chunk": "# 2. Experimental",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 6,
|
||||
"chunk": "# 2.1. Materials \n\nMethyl methacrylate (MMA), 2-ethylhexyl acrylate (EHA), 2-hydroxyethyl methacrylate (HEMA), 2-acrylamido-2-methyl propane sulfonic acid (AMPS), isophorone diisocyanate (IPDI), $^{2,2^{\\prime}}$ - azobisisobutyronitrile (AIBN), potassium hydroxide (KOH), methyl alcohol (MeOH), dibutyltin dilaurate (DBTDL), 4-methoxyphenol (MEHQ), acetic ether (EAc), N,N-dimethylformamide (DMF) were all purchased from Sinopharm Chemical Reagent Co., Ltd. (Shanghai, China). \n\n \nScheme 1. The synthetic route of IU-PHEMA. \n\n1-Hydroxycyclohexyl phenyl ketone (HCPK), 1,6-hexanediol diacrylate (HDDA), ethoxylated trimethylolpropane triacrylate (EOTMPTA), trifunctional acid ester (CD9051), phosphate (w190) were all supplied by Jiangsu Kuangxin Photosensitivity Newmaterial Stock Co., Ltd. (Wuxi, China).",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 7,
|
||||
"chunk": "# 2.2. Synthesis of prepolymer \n\nAn isocyanate-containing unsaturated monomer named as HIp was prepared via nucleophilic addition of IPDI and HEMA. The molar ratio of two reactants was 1:1 and the temperature was maintained at $40^{\\circ}\\mathsf C$ . \n\nA series of sulfo-group-containing acrylate copolymers (PHEMA) were synthesized via free radical copolymerization of AMPS, HEMA, EHA and MMA. AIBN-initiated bulk copolymerizations of monomers were carried out at $90^{\\circ}\\mathsf C.$ . The concentration of AIBN was fixed equal to $2\\times10^{-3}$ mol per mol of all monomers. The prepared PHEMA then reacted with Hip to introduce urethane groups and cross-linkable double bonds into the side chain of polymer, which led to a UV-curable copolymer named as U-PHEMA. Finally, the IU-PHEMA, a prepolymer for antifog coating, was obtained by ionization of U-PHEMA with KOH–methanol solution. The whole synthetic route is shown in Scheme 1. \n\nIn the experiment, a series of IU-PHEMA prepolymers were prepared to investigate the influence of AMPS content on anti-fog properties. Table 1 shows the amount of each component used in the reaction. \n\nTable 1 Composition of IU-PHEMA in copolymerization. \n\n\n<html><body><table><tr><td>No.</td><td>HEMA</td><td>EHA</td><td>MMA</td><td>AMPS</td><td>IPDI</td><td>HEMA</td><td>AMPS%</td></tr><tr><td>IU-PHEMA01</td><td>21.95</td><td>24.72</td><td>11.24</td><td>1.00</td><td>25.00</td><td>16.01</td><td>1%</td></tr><tr><td>IU-PHEMA03</td><td>21.95</td><td>22.72</td><td>11.24</td><td>3.00</td><td>25.00</td><td>16.01</td><td>3%</td></tr><tr><td>IU-PHEMA05</td><td>21.95</td><td>20.72</td><td>11.24</td><td>5.00</td><td>25.00</td><td>16.01</td><td>5%</td></tr><tr><td>IU-PHEMA07</td><td>21.95</td><td>18.72</td><td>11.24</td><td>7.00</td><td>25.00</td><td>16.01</td><td>7%</td></tr><tr><td>IU-PHEMA08</td><td>21.95</td><td>17.72</td><td>11.24</td><td>8.00</td><td>25.00</td><td>16.01</td><td>8%</td></tr><tr><td>IU-PHEMA10</td><td>21.95</td><td>15.72</td><td>11.24</td><td>10.00</td><td>25.00</td><td>16.01</td><td>10%</td></tr></table></body></html>",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 8,
|
||||
"chunk": "# 2.3. Preparation of anti-fog coating \n\nThe IU-PHEMA was mixed with photoinitiator and reactive diluents to obtain formulas. HDDA and EOTMPTA were chosen as the reactive diluents to increase the double bond content, and CD9051 and w190 were used to improve the adhesion of formula on glass. Then the formula was coated on clean substrates to obtain a transparent film. The compositions of all formulas were shown in Table 2.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 9,
|
||||
"chunk": "# 2.4. Measurements \n\nThe number-average molecular weight $(M_{\\mathfrak{n}})$ and molecular weight distribution or polydispersity index PDI $(M_{\\mathrm{W}}/M_{\\mathrm{n}})$ of the polymers were determined at $25^{\\circ}\\mathsf{C}$ with WATERS GPC-1515(GPC), using DMF as eluent at a flow rate of $1.0\\mathrm{mL}\\mathrm{min}^{-1}$ . The molecular weight and polydispersity index data were compared against broad standards of PEG. FT-IR spectra were recorded with a Bomem FTLA 2000-104 using the potassium bromide (KBr) disk sampling technique. $^1\\mathrm{H}$ NMR spectrum for IU-PHEMA was obtained by an AVANCE III ${400}\\mathrm{MHz}$ Digital NMR spectrometer at $25^{\\circ}\\mathsf C$ , using DMSO-d6 as solvent. \n\nTable 2 Composition of UV-curable anti-fog coatings. \n\n\n<html><body><table><tr><td>Formula</td><td>Resin</td><td>Resin content</td><td>HDDA</td><td>EOTMPTA</td><td>CD9051</td><td>Phosphate</td><td>HCPK</td></tr><tr><td>FA1</td><td>IU-PHEMA01</td><td>70</td><td>10</td><td>10</td><td>5</td><td>2</td><td>3</td></tr><tr><td>FA2</td><td>IU-PHEMA03</td><td>70</td><td>10</td><td>10</td><td>5</td><td>2</td><td>3</td></tr><tr><td>FA3</td><td>IU-PHEMA05</td><td>70</td><td>10</td><td>10</td><td>5</td><td>2</td><td>3</td></tr><tr><td>FA4</td><td></td><td>70</td><td>10</td><td>10</td><td>5</td><td>2</td><td>3</td></tr><tr><td>FA5</td><td></td><td>50</td><td>20</td><td>20</td><td>5</td><td>2</td><td>3</td></tr><tr><td>FA6</td><td>IU-PHEMA07</td><td>40</td><td>25</td><td>25</td><td>5</td><td>2</td><td>3</td></tr><tr><td>FA7</td><td></td><td>30</td><td>30</td><td>30</td><td>5</td><td>2</td><td>3</td></tr><tr><td>FA8</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td></tr><tr><td></td><td>IU-PHEMA08</td><td>5040</td><td>2025</td><td>2025</td><td>５５</td><td>２2</td><td>33</td></tr><tr><td>FA10</td><td></td><td>50</td><td>20</td><td>20</td><td>5</td><td>2</td><td>3</td></tr><tr><td>FA11</td><td>IU-PHEMA10</td><td>40</td><td>25</td><td>25</td><td>5</td><td>2</td><td>3</td></tr></table></body></html> \n\nContact angles were measured using a DATA physics OCA40 contact angle goniometer equipped with an environmental chamber. Three drops of water were used for each measurement, and the average contact angle values were reported. Samples for testing were cured on a slide. \n\nThe coatings are prepared on one side of clean substrates and cured under UV lamp. One part of each substrate is coated and the other part is uncoated. Then samples are held above hot water $(80^{\\circ}\\mathsf{C})$ for 15 s, which is called the anti warm fog test. \n\nAs comparison, an anti cold fog test is done as follows. The coatings are prepared on both sides of clean substrates and cured under UV lamp. One part of each substrate side is coated and the other part is uncoated. Then the samples are put into a $-15^{\\circ}\\mathsf C$ refrigerator for $10\\mathrm{min}$ and taken out in a $50\\%$ humidity environment. \n\nTo evaluate the oil resistance of samples, coated panels were immersed in oleic acid at room temperature. To examine the chemical resistance, samples were immersed in $0.5\\mathrm{mol}\\mathrm{L}^{-1}\\mathrm{H}_{2}\\mathrm{S}0_{4}$ , $\\boldsymbol{1}\\mathrm{mol}\\mathrm{L}^{-1}$ NaOH and $50\\%$ ethanol, respectively.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 10,
|
||||
"chunk": "# 3. Results and discussion",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 11,
|
||||
"chunk": "# 3.1. Characterizations of U-PHEMA \n\nThe FT-IR spectra of PHEMA, HIp and U-PHEMA are shown in Fig. 1. From Fig. 1(a), the absorption peaks of $\\mathsf{C}{=}\\mathsf{C}$ at $1640\\mathsf{c m}^{-1}$ and $\\scriptstyle{\\mathrm{H-C=}}$ at $810\\mathrm{cm}^{-1}$ disappear, which is an evidence that all the monomers have reacted during the copolymerization. Besides, the peak of $s{=}0$ at about $1400\\mathrm{cm}^{-1}$ is observed, indicating the introduction of sulfonic group in the polymer. From Fig. 1(b), the appearance of the characteristic peaks of $\\mathsf{C}{=}\\mathsf{C}$ at $1640\\mathsf{c m}^{-1}$ and $810\\mathrm{cm}^{-1}$ indicates HEMA has successfully reacted with IPDI. As shown in Fig. 1(c), the disappearance of peak at $2236\\mathrm{cm}^{-1}$ indicates the successful reaction between $-\\mathsf{N C O}$ in HIp and $-\\mathsf{O H}$ in PHEMA. What is more, the presence of $\\mathsf{C}{=}{\\mathsf{C}}$ at $1640\\mathrm{cm}^{-1}$ and $\\scriptstyle{\\mathrm{H-C=}}$ at $810\\mathrm{cm}^{-1}$ indicates that photo-crosslinkable double bond has been successfully introduced into the polymer. Fig. 2 shows the $^1\\mathrm{H}$ NMR spectrum of U-PHEMA. The peak a at $7.9\\mathrm{ppm}$ is related to group of $-N\\mathsf{H}-$ , peaks b at 6.1 ppm and $5.8\\mathsf{p p m}$ are assigned to the ${\\mathrm{HC}}{=}{\\mathrm{CH}}$ , and peak c, d and e belong to $\\scriptstyle0=\\mathsf{C}-\\mathsf{C}-\\mathsf{H}$ in the structure of polymer. Based on the above results, it can be concluded that U-PHEMA has been successfully synthesized. \n\n \nFig. 1. FT-IR spectra of PHEMA (a), HIp (b), and U-PHEMA (c).",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 12,
|
||||
"chunk": "# 3.2. Glass transition temperature of IU-PHEMA \n\nFig. 3 shows the DSC curves of IU-PHEMA with different AMPS content. It can be observed that AMPS content does not have any effects on the glass transition temperature of IU-PHEMA. It can be explained by that the amount of AMPS is not enough to influence the glass transition temperature.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 13,
|
||||
"chunk": "# 3.3. Anti-fog test of IU-PHEMA \n\nTable 3 shows the anti-fog test of UV-cured anti-fog coatings. An overview of Tables 2 and 3 shows that the anti-fog ability of coatings is affected by two major factors. One is the amount of AMPS in IU-PHEMA prepolymers, and the other one is the content of IU-PHEMA in formulas. When the amount of AMPS in IU-PHEMA is above $7\\%$ and the amount of IU-PHEMA in formulas is above $50\\%$ , the coatings exhibit the anti-fog performance. During the UV-curing process, it is likely that the sulfonic groups are trapped in the polymer network, which makes the surface of the film less hydrophilic. Therefore the content of AMPS in prepolymer and the content of prepolymer in formulas have to reach a certain value to ensure sufficient sulfo-group on the surface. Fig. 4 shows the anti-fog tests of formula FA8 on PC plate. It shows that the part with anti-fog coating left keeps good transparency both in anti warm and cold fog tests, which demonstrates the coating prepared by formula FA8 provides the anti-fog performance. \n\n \nFig. 2. $^1\\mathrm{H}$ NMR spectrum of U-PHEMA. \n\nTable 3 The anti-fog test of UV-cured anti-fog coatings. \n\n\n<html><body><table><tr><td>Formula</td><td>FA1</td><td>FA2</td><td>FA3</td><td>FA4</td><td>FA5</td><td>FA6</td><td>FA7</td><td>FA8</td><td>FA9</td><td>FA10</td><td>FA11</td></tr><tr><td>Water contact angle</td><td>75</td><td>72</td><td>66</td><td>9.4</td><td>12.4</td><td>54</td><td>59</td><td>11.2</td><td>57</td><td>10.6</td><td>63</td></tr><tr><td>Anti-fog test</td><td>Fogging</td><td>Fogging</td><td>Fogging</td><td>Anti-fog</td><td>Anti-fog</td><td>Fogging</td><td>Fogging</td><td>Anti-fog</td><td>Fogging</td><td>Anti-fog</td><td>Fogging</td></tr></table></body></html> \n\n \nFig. 3. DSC curves of IU-PHEMA with different AMPS content.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 14,
|
||||
"chunk": "# 3.4. Mechanical properties of UV-cured anti-fog coatings \n\nTable 4 gives the film properties of UV-cured anti-fog coatings. Three different transparent substrates (PMMA, PC and glass) were used in the test. It can be seen that the UV-cured coatings exhibit great adhesion and good resistance on various substrates except glass. Although the hydroxyl groups in the IU-PHEMA prepolymer make formulas interact with substrates surface more easily, the surface of glass is so smooth that few resins show a good adhesion on it. The hardness of the coating is an important factor affecting the abrasion and scratch resistance. Hard coatings give better scratch resistance, and abrasion resistance is also affected by surface friction. From Table 4, it is shown that the pencil and pendulum hardness increased with the increasing amount of reactive diluents. The enhancement in hardness can be attributed from the enhanced crosslinking density of the film, which results in higher reactive diluents content in the UV-curing formula. The above results demonstrate that the UV-curing coating with proper formula provides great coating characteristics. \n\n \nFig. 5. UV–vis spectra of three different plates with and without UV-cured coatings.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 15,
|
||||
"chunk": "# 3.5. Transparency of UV-cured anti-fog coatings \n\nTransparency is a key indication for films of anti-fog coatings. Bad transparency limits the film application in optical instruments fields [8]. To evaluate the optical transmission, the UV-cured coatings on various substrates were investigated in the wavelength range of $300{-}800\\mathrm{nm}$ . Fig. 5 shows UV–vis spectra of three different plates with and without UV-cured coatings. For all three substrates, a slight decrease in transmittance with UV-cured coating indicated good transparency of the UV-cured coatings. Besides, the images of the UV-cured coatings on various substrates were also shown in Fig. 6. A clear observation showed that all the prepared UV-cured coatings are totally transparent. Both of the results demonstrate that UV-cured anti-fog coatings with IU-PHEMA have good optical transparency and they can be potential used in transparent optical instruments fields. \n\n \nFig. 4. Anti-fog tests of formulation FA8 on PC plate. (a) Anti warm fog test and (b) anti cold fog test. The left part of the plate is coated with the anti-fog coating and the right one is without. \n\nTable 4 The film properties of UV-curing formula of IU-PHEMA. \n\n\n<html><body><table><tr><td>Formula</td><td>Substrate</td><td>Adhesion/cross-cut</td><td>Pencil hardness</td><td>Pendulum hardness (s)</td><td>Acid resistance</td><td>Alkali resistance</td><td>Ethanol resistance</td><td>Oleic acid resistance</td></tr><tr><td>FA7</td><td>Glass</td><td>２２</td><td>3H</td><td>96</td><td><3 days</td><td><3 days</td><td><3 days</td><td><3 days</td></tr><tr><td>FA6</td><td>Glass</td><td></td><td>3H</td><td>79</td><td><3 days</td><td><3 days</td><td><3 days</td><td><3 days</td></tr><tr><td>FA5</td><td>Glass</td><td>2</td><td>2H</td><td>69</td><td><3 days</td><td><3 days</td><td><3 days</td><td><3 days</td></tr><tr><td></td><td>Glass</td><td>2</td><td>2H</td><td>44</td><td><3 days</td><td><3 days</td><td><3 days</td><td><3 days</td></tr><tr><td>FA4</td><td>PC-plate</td><td>0</td><td>2H</td><td>43</td><td>>10 days</td><td>>10 days</td><td>>10 days</td><td>>10 days</td></tr><tr><td></td><td>PMMA-plate</td><td>0</td><td>2H</td><td>49</td><td>>10 days</td><td>>10 days</td><td>>10 days</td><td>>10 days</td></tr><tr><td>FA8</td><td>PC-plate</td><td>0</td><td>2H</td><td>72</td><td>>10 days</td><td>>10 days</td><td>>10 days</td><td>>10 days</td></tr><tr><td>FA9</td><td>PC-plate</td><td>0</td><td>2H</td><td>83</td><td>>10 days</td><td>>10 days</td><td>>10 days</td><td>>10 days</td></tr><tr><td>FA10</td><td>PC-plate</td><td>0</td><td>2H</td><td>66</td><td>>10 days</td><td>>10 days</td><td>>10 days</td><td>>10 days</td></tr><tr><td>FA11</td><td>PC-plate</td><td>0</td><td>3H</td><td>85</td><td>>10 days</td><td>>10 days</td><td>>10 days</td><td>>10 days</td></tr></table></body></html> \n\n \nFig. 6. The images of three different plates with and without UV-cured coatings. The upper are substrates with UV-cured coating and the lower are clean substrates: (a) glass, (b) PC plate, and (c) PMMA plate.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 16,
|
||||
"chunk": "# 4. Conclusion \n\nIn this article, a new series of UV-curable hydrophilic polyacrylate containing sulfonic groups were synthesized. When the content of AMPS in the prepolymer was over $7\\%$ and the content of prepolymer in the formula was at least $50\\%$ , the UV-cured coatings could achieve anti-fog properties. Also, the formula coated on PC, PMMA and glass plates showed great mechanical properties and good transparency except for bad adhesion on glass plate.",
|
||||
"category": " Conclusions"
|
||||
},
|
||||
{
|
||||
"id": 17,
|
||||
"chunk": "# Acknowledgements \n\nThis work was supported by the National Nature Science Foundation of Jiangsu Province (No. BK20130153) and the Fundamental Research Funds for the Central Universities (No. JUSRP1021).",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 18,
|
||||
"chunk": "# References \n\n[1] L. Maechler, C. Sarra-Bournet, P. Chevallier, N. Gherardi, G. Laroche, Plasma Chem. Plasma Process. 31 (2011) 175–187. \n[2] H.D. Hwang, C.H. Park, J.I. Moon, H.J. Kim, T. Masubuchi, Prog. Org. Coat. 72 (2011) 663–675. \n[3] S.J. Dain, A.K. Hoskin, C. Winder, D.P. DingsdagdOphthal, Physiol. Opt. 19 (1999) 357–361. \n[4] P. Chevallier, S. Turgeon, C. Sarra-Bournet, R. Turcotte, G. Laroche, Appl. Mater. Int. 3 (2011) 750–758. \n[5] N. Nuraje, R. Asmatulu, R.E. Cohen, M.F. Rubner, Langmuir 27 (2011) 782–791. \n[6] R. Wang, K. Hashimoto, A. Fujishima, M. Chikuni, E. Kojima, A. Kitamura, M. Shimohigoshi, T. Watanabe, Nature 338 (1997) 431–432. \n[7] F.C. Cebeci, Z. Wu, L. Zhai, R.E. Cohen, M.F. Rubner, Langmuir 22 (2006) 2856–2862. \n[8] J.A. Howarter, J.P. Youngblood, Macromol. Rapid Commun. 29 (2008) 455–466. \n[9] D. Radloff, C. Boeffel, H.W. Spiess, Macromolecules 29 (1996) 1528–1534. \n[10] Y.K. Lai, Y.X. Tang, J.J. Gong, D.G. Gong, L.F. Chi, C.J. Lin, Z. Chen, J. Mater. Chem. 22 (2012) 7420–7426.",
|
||||
"category": " References"
|
||||
}
|
||||
]
|
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[
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{
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"id": 1,
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"chunk": "# UV-Curable Anti-Fog 医 Coatings \n\nA t c ertain t emperature aand h um d ty, water vap or i n a ir c ondenses on s olid surfaces. Because water has much higher surface energy t han most solid surfaces, the c ondensed w ater u sually t akes t he form of s mall d roplets, which scatter light and cause haziness. Fogging is a severe problem for a lot of optical devices, such as lenses, m irrors, w indshields and visors et al. Basically, there are two ways to avoid hazy water condensation. One i s t o c ontrol t he t emperature a nd h umidity s o t hat water c ondensation c an n ot hap pen. F or exa mple, s ome devices use heating elements to keep the temperature high enough th at w ater c annot c ondense; s ome d evices a re purged by inert gases or dry air to remove moisture. These approaches are very effective, but consume energy and they are ex pensive. The ot her approach i s t o u se a nti-fog c oatings on t he optical devices. A nti-fog c oatings c an p revent hazy water condensation and maintain the optical clarity. Obviously, this is a better approach, because anti-fog coatings are cheaper and consume no energy to operate. Considering the anti-fog mechanism, it is possible to categorize anti-fog coatings into three types. \n\nType I: The coatings remove water condensation by absorbing liquid water into the coating. Type I c oatings can b e s aturated whe n moi sture lev el i s t oo h igh, a nd do not respond to water condensation quickly; therefore they are not very effective. \n\nType I I: The c oatings lo wer t he s urface e nergy of water, a nd the condensed water evenly wets the surface. Usually, Type II anti-fog coatings carry extractable surfactants.1 W hen wa ter co ndenses o n t he coa ting surface, t he s urfactants di ssolve in to t he li quid w ater and br ing down its surface energy so that water w ill wet the s urface ev enly. T ype I I c oatings w ork e ffectively a s long a s e nough s urfactants c an b e ex tracted i nto w ater; however, surfactants can be washed away by water, and Type II anti-fog coatings will lose their anti-fog property gradually. I n ad dition, b ecause it t akes t ime fo r w ater t o dissolve surfactants, Type II coatings will not respond to water condensation very quickly. When suddenly exposed to high humidity, some Type II coatings can immediately get fogged and it will take some time for them to turn clear. \n\nType I II: The se c oatings ha ve a s uper-hydrophilic surface. Water has a very low contact angle, less than $5^{\\circ}$ , on s uperhydrophilic s urfaces, a nd w ater c ondensed on a s uper-hydrophilic s urface w ill ev enly s pread ou t v ery quickly. No s urfactants ne ed t o b e ex tracted f rom t he super-hydro hilic coatings; t ey work instantly with little d lay ttime. Sup er-hydrophilic c oatings2 p erform b tter than the other two types of anti-fog coatings. \n\nIn this paper, we discuss UV-curable super-hydrophilic anti-fog c oatings. UV -curable an ti-fog c oatings3 c an b e cured i nstantaneously. They c onsume le ss e nergy t o produce and, more importantly, they can be produced in a roll-to-roll process at high speed.",
|
||||
"category": " Introduction"
|
||||
},
|
||||
{
|
||||
"id": 2,
|
||||
"chunk": "# Experimental \n\nSilica na noparticles, a s a 1 $\\ensuremath{\\mathrm{0-15}}\\ensuremath{\\mathrm{n~m~p~}}$ article s ize, $3\\:0\\%$ dispersion in m ethanol, w ere u sed e ither dir ectly wi thout modification o r w ere m odified b y p olyethylene g lycolmodified silane and acrylate/methacrylate-modified silanes.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 3,
|
||||
"chunk": "# Synthesis of Polyethylene Glycol-Modified Silane \n\nMonomethyl ether polyethylene glycol (mPEG) $(\\mathrm{Mw}=1100)$ ) was dissolved in toluene and the mixture was dried. At room temperature a nd u nder n itrogen, a mola r e quivalent (with respect to the mPEG) of 3-isocyantopropyl trimethoxysilane was added drop wise to the reaction mixture. A few d rops of dibutyl tin dilaurate were added as a c atalyst. The r eaction mixture w as t hen s tirred c ontinuously fo r $24\\mathrm{h}$ at $5\\ 0^{\\mathrm{{o}}}\\mathrm{{C}}$ . The r eaction w as mon itored by i nfrared s pectroscopy; the is ocyanate s ignal is a $\\mathrm{t}2271\\mathrm{cm}^{-1}$ . U pon c ompletion, approximately t wo t hirds of t he t oluene w as r emoved by rotary evap oration a nd t he m PEG t rimethoxysilane w as precipitated into hexane and washed several times. The resulting s olid w as d ried a nd cha racterized by 1 H N MR. Reaction yields of $>90\\%$ were obtained.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 4,
|
||||
"chunk": "# Silica Nanoparticle Surface Modification \n\nThe s urface of s ilica na noparticles w as f unctionalized with mPEG triethoxysilane and 3-(trimethoxysilyl)propyl \n\n \nFIGURE 1 | Polycarbonate sheet (left) and PET sheet (right) coated by a roll-to-roll process. \n\nTABLE 1 | Modification of silica nanoparticles. \n\n\n<html><body><table><tr><td rowspan=\"3\">Material</td><td colspan=\"2\">Modified Silicon Oxide Particle</td></tr><tr><td></td><td></td></tr><tr><td>A</td><td>B</td></tr><tr><td>Silicon oxide nanoparticles, 30% solid in methanol</td><td>29.0</td><td>28.8</td></tr><tr><td>3-(trimethoxysilyl)propyl acrylate</td><td>1.1</td><td></td></tr><tr><td>3-(trimethoxysilyl)propyl methacrylate</td><td></td><td>1.1</td></tr><tr><td>mPEG trimethoxysilane</td><td>2.1</td><td>3.0</td></tr><tr><td>Hydroquinone monoethyl ether</td><td>0.02</td><td>0.02</td></tr><tr><td>Methanol (solvent)</td><td>67.7</td><td>67.1</td></tr><tr><td>Total</td><td>100</td><td>100</td></tr></table></body></html> \n\nTABLE 2 | Anti-fog coating formulation. \n\n\n<html><body><table><tr><td rowspan=\"2\">Material</td><td colspan=\"4\">Formulation</td></tr><tr><td>C (%)</td><td>D (%)</td><td>E (%)</td><td>F (%)</td></tr><tr><td>Silicon oxide nanoparticle</td><td></td><td>20.4</td><td>-</td><td></td></tr><tr><td>Modified silicon oxide particle A</td><td>28.9</td><td>-</td><td>-</td><td>28.9</td></tr><tr><td>Modified silicon oxide particle B</td><td></td><td>-</td><td>29.7</td><td></td></tr><tr><td>PEG diacrylate</td><td>6.8</td><td>5.1</td><td></td><td>6.8</td></tr><tr><td>PEG dimethacrylate</td><td>-</td><td>-</td><td>7.0</td><td></td></tr><tr><td>Sulfo propyl acrylate potassium salt</td><td>0.3</td><td>0.2</td><td>-</td><td></td></tr><tr><td>Sulfo propyl methyacrylate potassium salt</td><td></td><td></td><td>0.3</td><td>-</td></tr><tr><td>Water</td><td>2.4</td><td>1.8</td><td>2.5</td><td>2.4</td></tr><tr><td>Irgacure184</td><td>0.4</td><td>0.3</td><td>0.3</td><td>0.4</td></tr><tr><td>Methanol (solvent)</td><td>61.3</td><td>72.2</td><td>60.4</td><td>61.6</td></tr><tr><td>Total</td><td>100</td><td>100</td><td>100</td><td>100</td></tr></table></body></html> \n\nTABLE 3 | Rating of anti-fogging performance. \n\n\n<html><body><table><tr><td>Antifogging Performance</td><td>Rating</td><td>Annotations</td></tr><tr><td>No</td><td>1</td><td>Zero visible, poor light transmission</td></tr><tr><td>No</td><td>2</td><td>Zero visible, poor light transmission</td></tr><tr><td>Poor</td><td>4</td><td>Poorvisible</td></tr><tr><td>Fair</td><td>6</td><td>Discontinuous film of water</td></tr><tr><td>Good</td><td>8</td><td>Discontinuous film of water, mostly transparent</td></tr><tr><td>Excellent</td><td>10</td><td>Completely transparent</td></tr></table></body></html> \n\nTABLE 4 | Performance of the anti-fog coatings. \n\n\n<html><body><table><tr><td rowspan=\"2\"></td><td colspan=\"2\">Anti-Fogging Rating</td></tr><tr><td>Before Water Wash</td><td>After Water Wash*</td></tr><tr><td>Formulation C</td><td>10</td><td>10</td></tr><tr><td>Formulation D</td><td>10</td><td>10</td></tr><tr><td>Formulation E</td><td>10</td><td>10</td></tr><tr><td>Formulation F</td><td>2</td><td>2</td></tr></table></body></html>\n\n\\* The coated samples were washed with water for 10 seconds. \n\nTABLE 5 | Properties of anti-fog coatings produced by roll-to-roll process. \n\n<html><body><table><tr><td>Properties</td><td>Value</td></tr><tr><td>Pencil hardness</td><td>H on PET, 2B on polycarbonate</td></tr><tr><td>Refractive index</td><td>1.48</td></tr><tr><td>Thickness</td><td>6 μm</td></tr><tr><td>Transmittance (%)</td><td>93.4</td></tr><tr><td>Clarity</td><td>99.8</td></tr><tr><td>Yellownessindex</td><td>No change from the uncoated substrate</td></tr><tr><td>Haze</td><td>0.27</td></tr><tr><td>Steelwoolabrasion*△Haze</td><td>1.87</td></tr></table></body></html>\n\n$\\ast_{250~9}$ load, #0000 steel wool, 10 double rub, and then measure haze value \n\nacrylate or 3- (trimethoxysilyl)propyl methacrylate. Table 1 sho ws t he a mount of e ach c omponent u sed i n t he reaction. The m ixtures were stirred at r oom temperature overnight to finish the reaction.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 5,
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||||
"chunk": "# Coating Formulation \n\nFormulations were prepared by mixing modified or unmodified s ilicon o xide na noparticles w ith r eactive diluents, polyethylene glycol diacrylate $\\mathrm{(Mw=575~g~moF^{1}}$ ), sulfopropyl ac rylate p otassium salt, a nd a phot oinitiator, 1-hydroxycyclohexyl b enzophenone. The s ulfopropyl acrylate potassium salt was added as a s olution in water. The exact weights used for coatings are shown in Table 2. All the liquid coatings have a solid content of about $12\\%$ . \n\nCoatings were applied on PE T or p olycarbonate she ets using # 16 w ire w ound r od. The c oatings w ere d ried for ha lf a m inute, a nd t hen c ured u nder a $3\\ \\mathrm{~00~W~p~}$ er inch me rcury vap or la mp at a do se of 1 J/ $\\mathrm{cm}^{2}$ in a nitrogen at mosphere. The t hicknesses of t he c ured coatings were ab out $5\\mathrm{m}$ icrometers. The c oated s amples were cha racterized by c ross-hatch ad hesion t est, p encil hardness, optical properties and steel wool scratch test.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 6,
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||||
"chunk": "# Results and Discussion \n\nAll c ured c oatings ha ve $100\\%$ ad hesion on t reated PE T and polycarbonate substrate, $99\\%$ optical clarity and over $90\\%$ transmittance. The anti-fog properties of the coatings were t ested by hold ing a c oated substrate for 15 seconds above warm water at $50^{\\circ}\\mathrm{C}$ . The c oating p erformance i s rated to the degree of fogging/transparency. If the coating fogs c ompletely, ha ving n o t ransparency, it i s rat ed a s 1. I f t he c oating do es n ot fog at a ll, s taying c ompletely transparent, it is rated as 10. A complete description of the rating and degree of fogging is given in Table 3. \n\nAnti-fog p erformance o f c oatings i s li sted in T able 4. A ll t he c oatings w ith t he s ulfonate s alt ha ve p erfect anti-fog p roperties; t he c oating w ithout s ulfonate s alt has p oor an ti-fog p roperties. Typ ically, i onic gr oups are mo re h ydrophilic t han e thylene g lycol g roups, a nd that is p robably th e r eason th at c oatings c ontaining sulfonate s alt h ave b etter p erformance in t he f ogging test. B ecause a ll t he c omponents a re c rosslinked i nto a p olymer ne twork, a fter t he c oatings w ere w ashed by water t heir a nti-fog p erformance d id n ot cha nge. It a lso has n o e ffect on a nti-fog p erformance whe ther ac rylates or met hacrylates w ere u sed. H owever, met hyacrylates polymerize much slower than acrylates. When coating E i s cured i n a ir, t he c oating i s very t acky b ecause of t he oxygen inhibition. There is no obvious difference between coating C and coating E, when they are cured in nitrogen. \n\nThe mo dification of s ilica na noparticles ha s n o e ffect on a nti-fog p erformance of t he c oatings. B ecause t he modified s ilica n anoparticles ar e c ovalently link ed in to the p olymer ne twork, t he mo dified s ilica na noparticles should g ive t he c oating b etter s cratch r esistance. Si nce silica nanoparticles without modification can already give good mechanical properties, surface modification of silica nanoparticles is not always necessary. \n\nThe c oating w ith n on-modified s ilica p articles w as applied by a roller coater on flexible PET and polycarbonate sheet. The c oating w as ap plied a nd c ured c ontinuously at $5\\mathrm{m}$ /min i n a r oll-to-roll p rocess. A s sho wn i n T able 5 a nd Figure 1 , t he c oated t ransparent she ets ha ve g ood op tical a nd mechanical properties and uniform thickness. \n\n \n\nAnti-fog coatings were also tested at both high and low temperatures, a nd t hey w orked v ery w ell b etween - $20~^{\\mathrm{o}}\\mathrm{C}$ and $90^{\\mathrm{{o}}}\\mathrm{{c}}$ . A s sho wn i n F igure 2 , a p iece of $\\mathrm{\\Deltap}$ artially c oated polycarbonate plat e w as plac ed on a c up of $90^{\\mathrm{{o}}}\\mathrm{{C}}$ c offee. The plate w as i nitially at r oom t emperature. Whe n it w as ex posed to the moisture from $90~^{\\mathrm{~o~c~}}$ coffee, the uncoated area was immediately fogged, while the coated area always stayed clear. In t he lo w-temperature t est, t he c oated s amples w ere c ooled down t o - $20^{\\mathrm{o}}\\mathrm{C}$ , a nd t hen w ere ex posed t o $60\\%$ h umidity room temperature air. The coated area stayed clear, while the uncoated area was quickly fogged.",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 7,
|
||||
"chunk": "# Conclusion \n\nUV-curable anti-fog coatings were developed. The coatings comprise i norganic na noparticles a nd U V-curable h ydrophilic materials. The c oatings c an p revent fogg ing at t emperatures between $-20{}^{\\mathrm{o}}\\mathrm{C}$ a nd $90^{\\mathrm{{o}}}\\mathrm{{c}}$ . The c oatings sho w exc ellent op tical clarity, good hardness and scratch resistance. \u0002",
|
||||
"category": " Conclusions"
|
||||
},
|
||||
{
|
||||
"id": 8,
|
||||
"chunk": "# References \n\n1 Radisch, Helmer; Scholz, Werner. US Patent, 4,609,688. 2 Cebeci, F .Ç.; W u, Z .; Z hai, L .; C ohen, R .E.; R ubner, M .F. Langmuir 2006, 22, 2856-2862. 3 Meijers, Guido, Thies, Jens Christoph; Nijenhuis, Atze Jan. International Patent Application, 2009, WO 2009/118415. \n\nThis p aper w as p resented a t t he R adTech 20 10 T echnology E xpo a nd Co nference, Baltimore, MD, www.radtech.org. \n\n",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 9,
|
||||
"chunk": "# Elcometer 456 Coating Thickness Gauge. One gauge–A world full of applications. \n\nThe key to the superiority of the 456 is its measurement system featuring a range of interchangeable probes \n\nAll Ferrous models will accept ANY Ferrous 456 probe \nAll Non-Ferrous models will accept ANY Non-Ferrous 456 probe \nAll Dual FNF models will accept ANY 456 probe High speed accurate readings Three memory options–Basic, Standard,Top Easy to use menu driven display-available in 22 languages Standard and pre-defined calibration options \nIntegral and separate probe options \n\nUS & Canada 800.521.0635 $\\cdot$ www.elcometer.com \n\nCopyright of Paint & Coatings Industry is the property of BNP Media and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use.",
|
||||
"category": " Materials and methods"
|
||||
}
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||||
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"chunk": "# ADVANCED MATERIALS \n\nSupporting Information \n\nfor Adv. Mater., DOI: 10.1002/adma.202002710 \n\nWet-Style Superhydrophobic Antifogging Coatings for Optical Sensors \n\nJongsun Yoon, Min Ryu, Hyeongjeong Kim, Gwang-Noh Ahn, Se-Jun Yim, Dong-Pyo Kim,\\* and Hyomin Lee\\* \n\nCopyright WILEY-VCH Verlag GmbH & Co. KGaA, 69469 Weinheim, Germany, 2020.",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 2,
|
||||
"chunk": "# Supporting Information",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 3,
|
||||
"chunk": "# Wet-Style Superhydrophobic Antifogging Coatings for Optical Sensors \n\nJongsun Yoon, Min Ryu, Hyeongjeong Kim, Gwang-Noh Ahn, Se-Jun Yim, Dong-Pyo Kim\\*, and Hyomin Lee\\*",
|
||||
"category": " Abstract"
|
||||
},
|
||||
{
|
||||
"id": 4,
|
||||
"chunk": "# WILEY-VCH",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 5,
|
||||
"chunk": "# Experimental Section",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 6,
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||||
"chunk": "# Materials \n\nChitosan (CHI, low molecular weight), Carboxymethyl cellulose (CMC, $\\mathrm{Mw}=250{,}000\\ \\mathrm{g}$ $\\mathrm{mol^{-1}}.$ ), Cationic silica nanoparticles LUDOX® CL ( $30\\mathrm{wt}\\%$ $\\mathrm{SiO}_{2}$ suspension in water, average particle size of $12\\ \\mathrm{nm}$ , and specific surface area of $220{\\mathrm{~m}}^{2}{\\mathrm{~g}}^{-1}.$ ), Anionic silica nanoparticles LUDOX® HS-40 ( $40\\ \\mathrm{wt}\\%$ $\\mathrm{SiO}_{2}$ suspension in water, average particle size of $12\\ \\mathrm{nm}$ , and specific surface area of $220{\\mathrm{~m}}^{2}{\\mathrm{~g}}^{-1}.$ ), Silicone oil (viscosity $10~\\mathrm{cSt}$ at $25~^{\\circ}\\mathrm{C}$ ), Acetic acid, and 2-Hydroxy-2-methylpropiophenone (Darocur 1173) were purchased from Sigma-Aldrich (Korea). Negative photoresist (SU-8 50, Microchem), Perfluoropolyether (PFPE)-urethane methacrylate (Fluorolink® MD700, Solvay), and Polydimethylsiloxane (PDMS, Sylgard® 184, Dow Corning) were used for lithography. Sand (40-100 mesh) was purchased from Acros Organics. Glass slides $76\\times26\\times1~\\mathrm{mm}$ ) were purchased from Marienfeld. \n\nPolymer-Silica Nanocomposite Fabrication via Layer-by-Layer Assembly: Sequential stacking of polymer and nanoparticle layers were performed using a StratoSequence 8 spin dipper (nanoStrata Inc.), controlled by StratoSmart operating software. The concentrations of CHI, CMC, positive charged $\\mathrm{SiO}_{2}$ , and negative charged $\\mathrm{SiO}_{2}$ in the dipping solutions were 1 $\\mathrm{mg\\ml^{-1}}$ , $1~\\mathrm{mg~ml^{-1}}$ , $0.03\\%$ (w/w), and $0.03\\%$ (w/w), respectively. For CHI, $0.3\\%$ (v/v) acetic acid (Sigma-Aldrich) was added prior to dissolving the polymer and was filtered with $5~{\\upmu\\mathrm{m}}$ pore filter (Millex®) after stirring overnight. Deionized water ( $18.2~\\mathrm{M}\\Omega\\cdot\\mathrm{cm}$ at $25~^{\\circ}\\mathrm{C}$ ) was used for all aqueous solutions. The dipping time in each solutions was $10~\\mathrm{min}$ followed by three rinsing steps (2, 1, and $1\\mathrm{min}^{\\cdot}$ ) in deionized water. The polymeric reservoir, (CHI/CMC)n ( $\\mathrm{\\dot{n}=}$ number of bilayers) was produced by alternately dipping in CHI and CMC solutions with rinsing steps in between. The polymer-silica nanocomposite was prepared by additionally depositing two complementary interacting nanoparticles on the polymeric reservoir.",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 7,
|
||||
"chunk": "# WILEY-VCH \n\nCold-Fog Transition Test: The cold-fog transition test described in Figure 1e and Figure 1f was performed by incubating glasses coated with various types of films in a $-15^{\\circ}\\mathrm{C}$ freezer for 12 hours and subsequent transfer to ambient lab conditions ( $21~^{\\circ}\\mathrm{C}$ , $35\\%$ RH). The cold-fog transition test described in Figure 3b and Figure 3e was conducted by contacting the coated glasses with a Peltier plate $\\left(-20^{\\circ}\\mathrm{C}\\right)$ for 1 minute and exposure to an ambient condition $(25^{\\circ}\\mathrm{C}$ , $22\\%$ RH) for 10 seconds. The optical photographs were obtained by a digital microscope (AM4113, Dino-Lite). For the observation of surface-induced fog, an inverted microscope (Eclipse Ti2, Nikon) was used. The cold-fog transition test described in Figure S5 was performed by incubating micro-pillar assembled polymer-silica nanocomposite in a $4~^{\\circ}\\mathrm{C}$ freezer for 1 hour and subsequent transfer to a temperature and humidity condition of $50~^{\\circ}\\mathrm{C}$ , $55\\%$ RH. \n\nLow Surface Energy Micro-Pillar Array Transfer on the Polymer-Silica Nanocomposite via Two-Step Lithography: To transfer the micro-pillar array, SU-8 pillar array was fabricated using typical lithography with a negative photoresist (SU-8 50). PDMS was poured onto the master and cured in an oven set at $70~^{\\circ}\\mathrm{C}$ for 3 hours. Then, photocurable PFPE polymer precursor containing $4\\%$ (w/w) Darocur 1173 was poured into the PDMS microwell and the excess was removed using a razorblade. Prior to attachment and curing, the polymer-silica nanocomposite was infused with a silicone oil to avoid PFPE film formation on the polymersilica nanocomposite. UV with an intensity of $20\\mathrm{mW}\\mathrm{cm}^{-2}$ was irradiated for 5 min to induce photocuring of the independent PFPE pillars. The residue was washed off with acetone. \n\nOther Measurements: The thickness of the films were characterized using profilometry (Dektak XT, Bruker). The Fourier transform infrared (FT-IR) spectra were collected using FT-IR spectroscopy (PerkinElmer) in transmittance mode. The X-ray photoelectron spectroscopy (XPS) spectra were obtained at the 4D beamline in the Pohang Accelerator",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 8,
|
||||
"chunk": "# WILEY-VCH \n\nLaboratory (PAL). The refractive index of the polymer and the silica layer was measured using spectroscopic ellipsometry (M-2000, J.A. Woollam). The water contact angles were measured using goniometry (SmartDrop, FemtoBiomed Inc.). The transmission spectra of the substrates were measured by spectrophotometer (UV-1800, Shimadzu) with a scanning rate of $50\\mathrm{nm\\sec^{-1}}$ . To demonstrate the utility of the wet-style superhydrophobic antifogging coating, an image sensor (Pixy2) was used to identify the specific colors in various simulated conditions. \n\n \nFigure S1. (a) The thickness of the polymeric reservoir with respect to the number of bilayers (n) of (CHI/CMC). (b) Transmission spectra of the polymeric reservoir, $(\\mathrm{CHI/CMC)_{n}}$ . \n\n \nFigure S2. XPS spectra of the polymer-silica nanocomposite (blue line) and polymeric reservoir (green line) (a) O 1s spectra, (b) Si 2p spectra. \n\n \nFigure S3. (a) The thickness of the polymer-silica nanocomposites with respect to the number of bilayers (n) of $\\mathrm{(SiO_{2}/S i O_{2}}$ ). (b) Transmission spectra of the polymer-silica nanocomposites, $\\mathrm{(CHI/CMC)_{30}(S i O_{2}/S i O_{2})_{n}}$ . \n\n \nFigure S4. FT-IR spectra of the (a) individual materials used in the wet-style superhydrophobic antifogging coating and (b) the coating in each step during the assembly. \n\n \nFigure S5. (a) A plot showing the water advancing (black bar), and receding (red bar) contact angles of the wet-style superhydrophobic antifogging coatings after exposure to various solvents for 1 hour (micro-pillar interval/diameter value of 4.0). (b) Optical photographs taken after transfer to an environmental chamber equilibrated at $50~^{\\circ}\\mathrm{C}$ , $55\\%$ RH from a $4^{\\circ}\\mathrm{C}$ refrigerator for the wet-style superhydrophobic antifogging coatings treated with various solvents. The scale bar is $1\\mathrm{cm}$ . \n\n \nFigure S6. Scanning electron microscopy (SEM) images of the substrates after two-step lithography. (a) Bare glass. (b) Polymeric reservoir. (c) Silica nanoporous film. (d) Polymersilica nanocomposite coated glass. The scale bar is $100\\upmu\\mathrm{m}$ . \n\n \nFigure S7. Transmission spectra of the wet-style superhydrophobic antifogging coatings with respect to the micro-pillar interval to diameter ratio $(I/D)$ with a fixed micro-pillar diameter of $25\\upmu\\mathrm{m}$ .",
|
||||
"category": " Materials and methods"
|
||||
},
|
||||
{
|
||||
"id": 9,
|
||||
"chunk": "# WILEY-VCH \n\n \nFigure S8. Optical micrograph of the wet-style superhydrophobic antifogging coating before and after removal of the contaminant (sand, 40-100 mesh) via self-cleaning. The scale bar is $100\\upmu\\mathrm{m}$ . \n\n \nFigure S9. Transmission spectra of the various films under ambient condition (before) and in a fogging condition (after).",
|
||||
"category": " Results and discussion"
|
||||
},
|
||||
{
|
||||
"id": 10,
|
||||
"chunk": "# Supporting Movies \n\nMovie S1. The application of the wet-style superhydrophobic antifogging coating on a curved surface. \n\nMovie S2. Mechanical durability test of the wet-style superhydrophobic antifogging coating. \n\nMovie S3. Water droplet repellency of the wet-style superhydrophobic antifogging coating under the fogging condition.",
|
||||
"category": " Results and discussion"
|
||||
}
|
||||
]
|
||||
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||||
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||||
"chunk": "Supporting Information",
|
||||
"category": " References"
|
||||
},
|
||||
{
|
||||
"id": 2,
|
||||
"chunk": "# Preparation of Antifog Hard Coatings Based on CarboxyFunctionalized Polyhedral Oligomeric Silsesquioxane Crosslinked with Oligo(ethylene glycol)s \n\nJun Nakagawa, Seiya Morinaga, and Yoshiro Kaneko\\* \n\nGraduate School of Science and Engineering, Kagoshima University, Kagoshima 890-0065, Japan \n\n\\*Corresponding author, E-mail: ykaneko@eng.kagoshima-u.ac.jp (Y. Kaneko) \n\n \nFigure S1. $\\mathrm{^{1}H}$ NMR spectrum of POSS-C in DMSO- $\\cdot d_{6}$ . The chemical shifts were referenced to DMSO (δ 2.5). \n\n \nFigure S2. $^{29}\\mathrm{Si}$ NMR spectrum of POSS-C in DMSO- $.d_{6}$ at $40^{\\circ}\\mathrm{C}$ . A small amount Cr(acac)3 was added as a relaxation agent. The chemical shifts were referenced to TMS (δ 0.0). \n\n<html><body><table><tr><td>HO H n</td><td>n=1</td><td>n=2</td><td>n=3</td><td>n=4</td><td>n=5</td><td>n=6</td></tr><tr><td>COOH OH (POSS-C) (OEG) 5 ： 1</td><td>goshima University goshima University goshima University</td><td>goshima University goshima Universil goshima University</td><td>ima University ima University</td><td>shima University shima University shima University</td><td>shima University shima University shima University</td><td>oshima University oshima University oshima University</td></tr><tr><td>COOH OH (POSS-C) (OEG) 2 1</td><td>Kagoshima Univer Kagoshima Univ agoshima Unive</td><td>Kagoshima Univ Kagoshima Uni</td><td>Universi</td><td>oshima shima University shima Univers</td><td>goshima Universit goshin goshimaUniver</td><td>agoshima Univers agoshima Univers agoshima Univers</td></tr><tr><td>COOH OH (POSS-C) (OEG) 1 1</td><td>Kagoshima Unive agoshima Univer Kagoshima Unive</td><td>agoshima Univ agoshima Uni agoshima Unive</td><td>agoshima Univer agoskima Univers</td><td>goshima Unive 0</td><td>hima Univ</td><td>Kagoshima Univ Kagoshima Univ</td></tr></table></body></html> \n\n \nFigure S3. Appearance of POSS-C/OEG coatings. \nFigure S4. UV-Vis spectra of a glass substrate and POSS-C/OEG coating $(n=4$ , $\\mathrm{COOH}{\\mathrm{:OH}}=2{:}1\\$ ). \n\n \nFigure S5. (a) SEM image and (b) EDX pattern of POSS-C/OEG coating $(n=4$ , $\\mathrm{COOH}{\\mathrm{:OH}}=2{:}1$ ). \n\n \nFigure S6. Photo of the equipment used for antifogging evaluation.",
|
||||
"category": " Materials and methods"
|
||||
}
|
||||
]
|
||||
7
task2/task2-chunks/ap4c00912_si_001.json
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7
task2/task2-chunks/ap4c00912_si_001.json
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@@ -0,0 +1,7 @@
|
||||
[
|
||||
{
|
||||
"id": 1,
|
||||
"chunk": "# Supporting Information \n\nRobust UV-Curable Dual-Cross-Linked Coating with Increased Transparency, Long-Term Antifogging, and Efficient Antibacterial Performances \n\nLina Zhang [1,3], Kai Feng\\*[1], Yizhe Liu [1,2], Fangrong Wu [1], Yubo Liu [1,2], Bo $\\mathrm{Yu}^{[2]}$ Xiaowei Pei [1,2], Lijia Liu[3], Chunhong Zhang[3] Yang $\\mathrm{Wu}^{*[1,2,4]}$ , Feng Zhou [2] [1] Yantai Zhongke Research Institute of Advanced Materials and Green Chemical Engineering, Shandong Laboratory of Advanced Materials and Green Manufacturing at Yantai, Yantai, Shandong 264006, PR China. \n[2] State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Science, Lanzhou, Gansu 730000, PR China. \n[3] Yantai Research Institute of Harbin Engineering University, Yantai, Shandong 264006, PR. China. \n[4] Qingdao Centre of Resource Chemistry and New Materials, Qingdao, Shandong \n\n266100, PR China. \n\nCorresponding Authors: Yang Wu, Email: yangwu@licp.cas.cn Kai Feng, Email: kaifeng@amgm.ac.cn \n\n \nFigure S1. The fine spectrum of nitrogen and bromine of PET and pMDHAB−AA \n\ncopolymer. \n\n \nFigure S2. DTG curves of pDMAEMA−AA copolymer and pMDHAB−AA copolymer. \n\n \nFigure S3. The cross-sectional SEM images of pMDHAB−AA coating. \n\n \nFigure S4. AFM images of PET surface. \n\n \n\nFigure S5. (a) The thermal weight loss of different crosslinked coatings. (b) DTG curves of different crosslinked coatings. \n\n \nFigure S6. Transmittance of pMDHAB−AA coatings after different dry-wet alternate \n\nanti-fog test cycles with hot-vapor method. \n\n \nFigure S7. (a) Bending tests of a pMDHAB-AA coating. (b) The transmittance of the \n\ncoating after bent 100 times. (c) Optical microscope image before coating bending. (d) Optical microscope image after coating bending.",
|
||||
"category": " Results and discussion"
|
||||
}
|
||||
]
|
||||
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