丙烯酸酯压敏胶黏弹性与粘接性能关系研究
薛双乐，张绪刚，薛 刚，张 斌，孙明明，李坚辉
（黑龙江省科学院石油化学研究院，黑龙江哈尔滨 150040）
【摘 要】首先研究了功能单体丙烯酸（AA）/甲基丙烯酸羟丙酯（HPMA）的比例对压敏胶性能的影响，得出m(AA)∶m(HPMA)=6∶2时压敏胶的性能较为优异。之后以m(AA)∶m(HPMA)=6∶2的压敏胶液为基础，以乙酰丙酮铝（AlACA）为交联剂制备不同交联程度的丙烯酸酯压敏胶，并研究了其黏弹性与粘接性能的关系。研究结果表明：常温下压敏胶储能模量值在40~60 kPa左右，tan在0.5~0.7范围内，3%~8%左右的形变率及大于80%的形变回复率，弛豫时间在110~600 s左右，得到综合性能优异的压敏胶。
【关键词】丙烯酸酯压敏胶；交联；黏弹性；粘接性能
聚氨酯改性丙烯酸酯单体的制备及其醋丙共聚乳液胶粘剂的性能研究
关 涛，陈昌主，李元璐，邱元斌，林海峰，潘汉杰
(福建省建筑涂料企业重点实验室，三棵树涂料股份有限公司，福建莆田 351100)
【摘 要】以丙烯酸羟乙酯(HEA)、甲苯-2,4-二异氰酸酯（TDI）、2-乙基己醇为原料，制备了一种聚氨酯改性丙烯酸酯（PUA）杂化单体材料。对比研究了PUA单体与常规单体如丙烯酸(AA)、丙烯酰胺(AM)、丙烯酸羟丙酯(HPA)、醋酸乙烯酯(VAc)、丙烯酸异辛酯(2-EHA)等参与醋酸乙烯-丙烯酸丁酯混合单体共聚制备的醋丙乳液胶膜的耐水性、湿态剪切强度以及干态胶合强度。研究结果表明：AA、AM、HPA等亲水性强、极性高的单体共聚制备的醋丙乳液胶膜具有较好的干强度，但耐水性、湿强度差；VAc、2-EHA等单体共聚制备的乳液胶膜的耐水性相对较好，但干强度、湿膜强度较差。相比于上述常规单体，PUA单体参与共聚制备的醋丙乳液胶膜在桦木块上的湿态剪切强度以及在桦木块、铝条基材上粘接的干态强度方面拥有良好的兼顾效果，有望作为一种新的功能单体材料用于高性能聚醋酸乙烯酯乳液胶粘剂的制备。
【关键词】PUA杂化单体；乳液胶粘剂；聚醋酸乙烯酯；耐水
基于声发射检测的复合材料粘接铝合金结构失效模式研究
戴京涛1，刘浩东1，赵培仲1，苏洪波1，付亚峰2，曲利峰3
(1.中国人民解放军海军航空大学青岛校区，山东青岛 266041；2.中国人民解放军91286部队，山东青岛 266003；3.中国人民解放军驻167厂军事代表室，四川成都 610000)
【摘 要】通过湿铺方式制备了复合材料补片，并利用该补片开展了受损铝合金试样的粘接修复。然后基于声发射检测方法，对试件在拉伸试验中的失效过程进行动态监测，分析评估了复合材料粘接修理铝合金构件的性能及失效模式。研究结果表明：产生不同失效模式的主要原因是复合材料补片与损伤铝板之间的黏附强度和补片拉伸破坏强度的大小不一致；通过涂抹偶联剂或加热加压固化，可使试件的主要失效模式由界面破坏改善为混合破坏和补片破坏；发生混合破坏和补片破坏的试件相比发生界面破坏的试件的拉伸强度更大。
【关键词】复合材料；铝合金；声发射检测；拉伸强度；失效模式
[康达新材料（集团）股份有限公司，上海 201419]
【摘 要】为制备性能优异的冷藏集装箱用热熔压敏胶，研究了热熔压敏胶的各配方组分和性能影响因素。通过研究影响胶体性能的相关因素，如黏度、粘接强度、软化点等物理性能，对配方中应用到的3种弹性体、4种增黏树脂以及3种增塑剂种类、含量进行选择，以找到较佳配方组成。研究结果表明：当配方中增黏树脂为C5加氢石油树脂且含量为40%，增塑剂为环烷油且含量为20%，弹性体为SIS弹性体的混合体且总含量为33%时，所制备的冷藏集装箱用热熔压敏胶的的综合性能较好。另外，从本文研究的热熔压敏胶DSC曲线可以看出，热熔压敏胶胶体没有显示出明显的两相玻璃化转变温度。
【关键词】热熔压敏胶；弹性体；增黏树脂；增塑剂；冷藏集装箱
王娟娟1，余英丰1,2，景 华2,3，刘黎成2,3，徐子曦2,3
（1.聚合物分子工程国家重点实验室，复旦大学高分子科学系，上海 200433；2.南通康尔乐复合材料有限公司，江苏南通 226007；3.上海芯邦新材料科技有限公司，上海 201818）
【摘 要】随着微电子产业的发展，各种封装技术不断涌现，对于封装材料的内应力、导热性、电性能都提出了更高的要求。本文介绍了聚合物微电子封装的主要材料，包括环氧树脂、有机硅、聚酰亚胺。由于封装的无铅化发展以及高功率导致的散热需求，导电胶和热界面材料成为了在封装中研究的较多热门材料。根据产品的使用环境，通过加速试验（温度循环、高加速应力试验、疲劳试验等）可以评估封装的可靠性。为探索封装失效的原因，需要对产品进行失效分析。本文介绍了常用的失效分析技术，具体描述了倒装芯片的底填胶的失效分析，并根据失效原因对底填材料提出了性能要求。封装材料的冷热冲击和湿热稳定性是影响可靠性的重要因素，湿气会导致封装“爆米花效应”、电化学迁移等后果从而使器件失效。为此，本文探究了湿气对半导体器件的影响及扩散机理，并对影响材料吸水性能的因素（如极性、自由体积、材料微相分离等）进行了综述。最后，还对微电子封装材料的未来发展进行了展望。
【关键词】电子封装；导电胶；导热胶；可靠性分析；失效分析；湿热老化
（工业和信息化部电子第五研究所，广东广州 511370）
【摘 要】底部填充胶（Underfill）作为一种重要的集成电路封装电子胶粘剂，在先进封装如2.5D、3D封装中，用于缓解芯片封装中不同材料之间热膨胀系数不匹配带来的应力集中问题，进而提高器件封装可靠性。在各种底部填充材料中，环氧树脂基底部填充胶是最常用的，也是商业化最成熟的产品。然而，广泛使用的毛细管环氧基底部填充胶材料的导热系数较低，无法满足功率密度更高的下一代先进封装芯片不断增长的散热要求。尽管已经发明了许多提高环氧树脂导热系数的策略，但其作为性能要求复杂的底部填充材料的应用仍然很困难，优化用于倒装芯片封装用底部填充材料的热-电-机械性能仍然是一个巨大的挑战。本文回顾了导热环氧树脂基底部填充胶材料为满足关键散热要求而取得的最新进展。同时，为高功率密度电子器件的电子封装设计具有高导热高可靠性的底部填充材料提供思路。
苯乙烯-异戊二烯-苯乙烯（SIS）弹性体的改性进展
冯道硕1，王 杰1，王锦昌2，李辉阳2，张文文2，王 斌2，崔丽荣2，黄昊飞1，荣卫锋1，崔广军2
（1.山东理工大学化学化工学院，山东 淄博 255000；2.淄博鲁华泓锦新材料集团股份有限公司，山东 淄博 255411）
【摘 要】简要介绍了热塑性弹性体SIS的各种改性方法，并对每种改性方法的优缺点及应用进行了总结。SIS的改性主要包括引入极性单体与后聚合改性，前者是在SIS制备时引入具有特殊功能的单体，达到改性的目的；后者主要从物理与化学两方面进行介绍，物理方面主要采用机械掺混的方式，根据改性需求掺混搅拌具有相应需求功能的材料，完成改性；化学改性的方法主要有光化学反应、羟基化、环氧化、磺化和自由基接枝改性等。本文系统综述了热塑性弹性体SIS的改性研究进展及最新应用情况，并对SIS的未来进行总结展望。
（华东理工大学材料科学与工程学院，上海 200237）
【摘 要】聚氨酯（PU）作为世界上第六大常用的聚合物，在家具、建筑、汽车、航空航天和医疗健康等领域广泛应用。随着石油资源的枯竭、生态环境的恶化，聚氨酯的回收成为亟待解决的重要问题。填埋法作为最原始的回收方法，不仅占用土地，污染水土资源，且回收成本耗费大量人力物力；焚烧回收热量，也是回收聚氨酯材料的常用手段，但聚氨酯在焚烧过程中，极易产生有毒有害物质；物理回收，在实际回收工作中有大规模应用，但回收过程中需要较高的温度压力条件，导致此种回收方式存在较大限制。目前，大量研究表明，化学回收是最具前景的聚氨酯材料回收手段。本文详细论述了包括醇解、水解、氨解、热解、磷酸解和生物降解等在内的多种化学回收工艺，及其最新的研究进展。
Scientific Research Report
Study on the relationship between viscoelasticity and bonding properties of acrylate pressure sensitive adhesive
Xue Shuangle, Zhang Xugang, Xue Gang, Zhang Bin, Sun Mingming, Li Jianhui
（Institute of Petrochemistry Heilongjiang Academy of Sciences, Harbin 150040, Heilongjiang, China）
【Abstract】Firstly, the effects of the ratio of functional monomer acrylic acid (AA)/hydroxypropyl methacrylate (HPMA) on the performance of pressure sensitive adhesive were studied, and it was concluded that the performance of pressure sensitive adhesive was optimal when m(AA)∶m(HPMA)=6∶2. Then based on pressure sensitive adhesive solution with m(AA)∶m(HPMA)=6∶2, acrylate pressure sensitive adhesive with different degrees of crosslinking using aluminum acetylacetonate (AlACA) as crosslinking agent was prepared, and the relationship between its viscoelasticity and bonding properties was investigated. The research results showed that at normal temperature, the storage modulus of pressure sensitive adhesive was about 40-60 kPa, tanδ was in the range of 0.5-0.7, the deformation rate was about 3%-8% and the deformation recovery rate was more than 80%, and the relaxation time was about 110-600 s, then pressure sensitive adhesive with excellent comprehensive performance was obtained.
【Keywords】acrylate pressure sensitive adhesive; crosslinking; viscoelasticity; bonding property
Preparation of polyurethane modified acrylate monomer and performance of its vinyl acetate-acrylate copolymer emulsion adhesive
Guan Tao, Chen Changzhu, Li Yuanlu, Qiu Yuanbin, Lin Haifeng, Pan Hanjie
(Key Laboratory of Fujian Architectural Coatings Enterprise, SKSHU Paint Co., Ltd., Putian 351100, Fujian, China)
【Abstract】A kind of polyurethane modified acrylate (PUA) hybrid monomer material was prepared using hydroxyethyl acrylate (HEA), toluene diisocyanate (TDI), and 2-ethylhexanol as raw materials. The water resistance, wet shear strength and dry bonding strength of vinyl acetate-acrylate latex film prepared by PUA monomer and conventional monomers such as acrylic acid (AA), acrylamide (AM), hydroxypropyl acrylate (HPA), vinyl acetate (VAc), 2-ethylhexyl acrylate (2-EHA), which involved in the copolymerization of vinyl acetate-butyl acetate mixed monomers, were compared. The research results showed that the vinyl acetate-acrylate emulsion film prepared by copolymerization of monomers with strong hydrophilicity and high polarity, such as AA, AM and HPA, had good dry strength, but poor water resistance and wet strength. The water resistance of the emulsion film prepared by copolymerization of VAc, 2-EHA and other monomers was relatively good, but the dry strength and wet film strength were poor.Compared with the conventional monomers mentioned above, the vinyl acetate-butyl acetate emulsion film prepared by copolymerization of PUA monomer had good balance of wet shear strength on birch block and dry strength on birch block and aluminum strip substrate, which was expected to be used as a new functional monomer for the preparation of high-performance polyvinyl acetate emulsion adhesive.
【Keywords】PUA hybrid monomer; emulsion adhesive; polyvinyl acetate; water resistance
Development and Application
Study on failure mode ofcomposite bonded aluminum alloystructure based on acoustic emission detection
Dai Jingtao1, Liu Haodong1, Zhao Peizhong1, Su Hongbo1, Fu Yafeng2, Qu Lifeng3
（1.Naval Aviation University Qingdao Branch, Qingdao 266041, Shandong, China; 2.No.91286 Unit, People’s Liberation Army of China, Qingdao 266003, Shandong, China; 3.Military Representative Office in No.167 Factory, Chengdu 610000, Sichuan, China)
【Abstract】The composite patch was prepared by wet laying method, and the damaged aluminum alloy specimen was repaired by bonding with the patch. Then, based on the acoustic emission detection method, the failure process of the specimens in the tensile test was dynamically monitored, and the performance and failure mode of the composite bonding repair of aluminum alloy components were analyzed and evaluated. The research results showed that, the main reason for the different failure modes was that the bonding strength between the composite patch and the damaged aluminum plate was different from the tensile failure strength of the patch. The main failure modes of the specimen could be improved from interface failure to mixed failure and patch failure by applying coupling agent or heating and curing under pressure. The tensile strength of the specimen with mixed failure and patch failure was higher than that with interface failure.
【Keywords】composite material; aluminum alloy; acoustic emission detection; tensile strength; failure mode
Study on preparation and properties of hot melt pressure sensitive adhesive for reefer container
Dai Fei, Wei Guocai, Wei Jingjing
[Kangda New Materials (Group) Co., Ltd., Shanghai 201419, China]
【Abstract】In order to prepare hot melt pressure sensitive adhesive with excellent performance for reefer container, the formula components and properties of hot melt pressure sensitive adhesive were studied. By studying the relevant factors affecting the adhesive performance, such as viscosity, bonding strength, softening pointand other physical properties, the type and content of three kinds of elastomer, four kinds of tackifying resin and three kinds of plasticizer used in the formulation were selected, in order to find the optimum formula composition. The research results showed that in the formula, when the tackifying resin was C5 hydro petroleum resin with a content of 40%, the plasticizer was naphthenic oil with a content of 20%, and the elastomer was a mixture of SIS elastomer with a total content of 33%, the prepared hot melt pressure sensitive adhesive for reefer container had good comprehensive performance.In addition, from the DSC curve of hot melt pressure sensitive adhesive in this paper, it could be seen that the hot melt pressure sensitive adhesive did not exhibit obvious two-phase glass transition temperature.
【Keywords】hot melt pressure sensitive adhesive; elastomer; tackifying resin; plasticizer; reefer container
Special Topics and Review
Research progress in microelectronic packaging materials and their reliability
Wang Juanjuan1, Yu Yingfeng1,2, Jing Hua2,3, Liu Licheng2,3, Xu Zixi2,3
(1.State Key Laboratory of Molecular Engineering of Polymers, Department of Macromolecular
Science, Fudan University, Shanghai 200433, China; 2. Natong Kernel Co., Ltd., Nantong 226007, Jiangsu Province, China; 3. Shanghai Sci-bon Technology Co., Ltd., Shanghai 201818, China )
【Abstract】With the development of microelectronic industry, a variety of packaging technologies are emerging, which put forward higher requirements for the internal stress, thermal conductivity and electrical properties of packaging materials. In this paper, the main materials for polymer microelectronic packaging, including epoxy resin, silicone, and polyimide were introduced. Due to the development of lead-free packaging and the need for heat dissipation of high power, conductive adhesive and thermal interface materials had become the more popular materials in the packaging research. According to the use environment of the product, the reliability of packaging could be evaluated by accelerated test (temperature cycle, high accelerated stress test, fatigue test, etc.). In order to explore the causes of packaging failure, it was necessary to carry out failure analysis for the product. In this paper, the commonly used failure analysis technology was introduced, the failure analysis of the underfill adhesive of flip chip was specifically described, and the performance requirements for the underfill material were put forward according to the failure reasons. The cold/thermal shock and hygrothermal stability of packaging materials were important factors affecting the reliability, moisture could lead to package “popcorn effect”, electrochemical migration and other consequences, which would make the device fail. For this reason, in this paper, the effect and diffusion mechanism of moisture on semiconductor devices were explored, and the factors affecting the water absorption performance of materials (such as polarity, free volume, material micro-phase separation, etc.) were reviewed. Finally, the future development of microelectronic packaging materials was also prospected.
【Keywords】electronic packaging; conductive adhesive; thermal conductive adhesive; reliability analysis; failure analysis; damp-heat aging
Research progress of epoxy resin-based underfill with thermal conductivity
Li Yinle, Sun Zhaoning, Pang Chao, Zhang Zhixin, Zhao Zhenbo, Zhao Hao
(The Fifth Electronic Research Institute of Ministry of Industry and Information Technology, Guangzhou 511370, Guangdong, China)
【Abstract】Underfill, as an important electronic adhesive for integrated circuit packaging, is used in advanced packaging such as 2.5D and 3D packaging, to alleviate the problem of stress concentration caused by the mismatch of thermal expansion coefficients among different materials in chip packaging, thus improving the reliability of device packaging. Among all kinds of underfill materials, epoxy resin-based underfill is the most commonly used and the most commercially mature product. However, the widely used capillary epoxy underfill material has a low thermal conductivity, which cannot meet the growing heat dissipation requirements of the next generation of advanced packaging chips with higher power density. Although many strategies have been proposed to improve the thermal conductivity of epoxy resin, its application as underfill material with complex performance requirements is still difficult, and optimizing the thermal-electrical-mechanical properties of the underfill for flip chip packaging is still a huge challenge. In this paper, the latest progress of thermal conductive epoxy resin-based underfill to meet the key heat dissipation requirements was reviewed. At the same time, it provided ideas for the design of electronic packaging of high power density electronic devices with high thermal conductivity and high reliability of underfill materials.
【Keywords】underfill; epoxy resin; thermal conductivity
Progress in modification of styrene-isoprene-styrene (SIS) elastomer
Feng Daoshuo1,Wang Jie1, Wang Jinchang2, Li Huiyang2,Zhang Wenwen2, Wang Bin2, Cui Lirong2,Huang Haofei1, Rong Weifeng1, Cui Guangjun2
(1.School of Chemistry and Chemical Engineering, Shandong University of Technology, Zibo 255000, Shandong, China; 2.Zibo Luhua Hongjin New Material Group Co., Ltd., Zibo 255411, Shandong, China)
【Abstract】Various modification methods of thermoplastic elastomer SIS were briefly introduced, and the advantages, disadvantages and application of each modification method were summarized. The modification of SIS mainly included the introduction of polar monomers and post-polymerization modification. The former one was the introduction of monomers with special functions in the preparation of SIS to achieve the purpose of modification.The latter one was mainly introduced from both physical and chemical aspects. In the physical aspect, the mechanical blending method was mainly adopted, according to the modification requirements of blending and mixing materials with corresponding demanding functions to complete the modification. The chemical modification methods mainly included photochemical reaction, hydroxylation, epoxidation, sulfonation and free radical grafting modification, and etc.In this paper, the modification research progress and latest application of thermoplastic elastomer SIS were systematically reviewed, and the future outlook of SIS was summarized.
【Keywords】thermoplastic elastomer; SIS; modification
Progress in polyurethane recycling
Zhao Liang, Zhang Lijuan, Zhu Yun, Wang Guiyou
(School of Materials Science and Engineering, East China University of Science and Technology, Shanghai 200237, China)
【Abstract】Polyurethane (PU), as the sixth most commonly used polymer in the world, is widely used in the fields of furniture, architecture, automotive, aerospace and medical health. With the depletion of petroleum resources and the deterioration of ecological environment, the recycling of polyurethane has become an important problem to be solved urgently. As the most primitive recycling method, the way of landfill not only occupies land and pollutes water and soil resources, but also consumes a lot of manpower and material resources in the cost of recycling. Incineration to recover heat is also a common method for recycling polyurethane materials, but polyurethane is very easy to produce toxic and harmful substances during the incineration process. Physical recycling has large-scale application in actual recycling work, but it requires the condition of high temperature and pressure during the recycling process, which results in great restrictions on this recycling method. At present, a large number of studies have shown that chemical recycling is the most promising means of polyurethane material recycling. In this paper, a variety of chemical recycling processes including alcoholysis, hydrolysis, aminolysis, pyrolysis, phosphorylation and biodegradation, as well as the latest research progress were discussed in details.
【Keywords】polyurethane recycling; landfill; physical recycling; chemical recycling
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