【作者】 付志强；

【导师】 刘峰； 林森；

【作者基本信息】 南昌大学 ， 化学， 2016， 硕士

【摘要】 随着科技的发展,曾经很好满足工业需求的传统结构的硅烷偶联剂也越来越显得力不从心,特别是最近几年来,复合材料、电子工业的迅速发展和电子产品的小型化及个性化,对硅烷偶联剂的性能提出了新的要求,不同的应用领域对硅烷偶联剂的性能要求也不同,因此改进新型的硅烷偶联剂也成为一个很迫切的课题。聚酰亚胺(PI)是一类含有酰亚胺环结构单元有机聚合物,具有高耐热性(达400℃以上)、广泛的温度使用范围(-200℃至300℃)和良好的机械、电性能以及无毒性等优点在广泛运用于航空航天微电子等领域,被誉为“解决问题的能手”。电子信息产业高速发展的今天,电解铜箔是重要的电子工业原材料,有着电子产品信号与电力传输、沟通的“神经网络”的美誉。然而传统铜箔防氧化工艺以+6价铬酸盐为基础,对人体以及环境的造成危害,因此寻求一种对人体以及环境绿色友好的表面处理工艺显得尤为迫切。基于以上研究背景,我们研究从合成高耐热酰亚胺改性硅烷偶联剂,并将其用于电解铜箔的表面防氧化处理。具体来说,我们从以下四个方面进行了研究:第一,以双酚A(Bisphenol A,简称BA)为底物合成酸酐双酚A二酸酐(BAAD)和氢化双酚A(Hydrogenated Bisphenol A,简称HBA)为底物合成的酸酐氢化双酚A二酸酐(HBA-AD)。这两种酸酐与3,3’,4,4’-联苯四甲酸二酐(BPDA)、4,4’-(六氟)二邻苯二甲酸酐(6FDA)分别为反应起始物,经过与烯丙基胺进行酰亚胺化反应和与三乙氧基硅烷进行硅氢加成反应,将酰亚胺环与硅烷偶联剂两者有机结合起来,合成了四种经酰亚胺环改性后的硅烷偶联剂(分别为BA-AD-AATES,HBA-AD-AA-TES,BPDA-AA-TES,6FDA-AA-TES),并对这些物质的结构和基本性能进行了表征。第二,将这四种经酰亚胺环改性后的硅烷偶联剂BA-AD-AA-TES,HBA-ADAA-TES,BPDA-AA-TES,6FDA-AA-TES各自配置成不同浓度水解成膜液进行预处理电解铜箔,通过电化学阻抗谱图以及动电位极化曲线谱图分别对这4种不同浓度硅烷水解成膜液预处理铜箔防腐蚀性能进行了研究,探讨最佳水解液浓度。第三,用四种经酰亚胺环改性后的硅烷偶联剂BA-AD-AA-TES,HBA-AD-AA-TES,BPDA-AA-TES,6FDA-AA-TES以及商品化的3-三乙氧基甲硅烷丙胺(γ-APS)和双-(3-γ-三乙氧基硅基丙基)四硫化物(A-1289)各自配置水解成膜液进行预处理电解铜箔,通过动电位极化曲线谱图以及电化学阻抗谱图比较研究了这四种经酰亚胺环改性后的硅烷偶联剂和另外两种商品化的硅烷偶联剂预处理电解铜箔在0.1mol/L氯化钠溶液中的防腐蚀情况。第四,用6FDA-AA-TES和BA-AD-AA-TES两种酰亚胺环改性的硅烷偶联剂为基础,在其水解液中掺杂纳米二氧化硅,研究其对铜箔的电化学防腐蚀性能。更多还原

【Abstract】 With the development of science and technology,silane coupling agents,industrial demand has been very good to meet more and more conventional structure appeared to be inadequate,especially in recent years,the miniaturization of the composite material,the rapid development of the electronics industry and electronic products and personalized the silane coupling agents performance raised new demands of different applications of the silane coupling agents performance requirements are also different,so new improved silane coupling agents has become a very urgent task.Polyimide(PI)is a class of imide ring structural units of the organic polymer,which has high heat resistance(more than 400 ℃),wide temperature range(-200 ℃ to 300 ℃)and good mechanical,electrical properties,non-toxicity and so on.PIs are widely used in aerospace and other fields of microelectronics,which are known as "problem solver."Today,in the rapid development of the electronic information industry,electrolytic copper foil is an important industrial raw material.With the signals and power transmission of the electronic products,which has the reputation of “Neural Networks”.However,the traditional copper anti-oxidation process is based on chromate(+6),that could cause harm to human body and environment.Therefore,sought a green environment-friendly surface treatment is particularly urgent.Based on the above background,we study the synthesis of high heat imidemodified silane coupling agents,and a surface anti-oxidation treatment for electrolytic copper foil.Specifically,we studied the following four aspects:First,bisphenol A(which is short for BA)as a substrate anhydride synthesis of bisphenol A dianhydride(BA-AD)and hydrogenated bisphenol A(which is short for HBA)as a substrate anhydride synthesis of Hydrogenated bisphenol A anhydride(HBA-AD).Both anhydrides and 3,3’,4,4’-biphenyltetracarboxylic dianhydride(BPDA),4,4’-(hexafluoro)diphthalic anhydride(6FDA)were reaction starting materials,through imidization reaction with allylamine and hydrosilylation reaction with triethoxysilane,so that combine the silane and the imide ring.Four silane coupling agents which are modified by the imide ring are synthesized(respectively for the BA-AD-AA-TES,HBA-AD-AA-TES,BPDA-AA-TES,6FDA-AA-TES),and these structures and basic material properties were characterized.Second,these four silane coupling agents that modified by the imide ring BA-ADAA-TES,HBA-AD-AA-TES,BPDA-AA-TES,6FDA-AA-TES each configured different concentrations of hydrolysis pretreatment liquid film forming electrolytic copper foil.Four different concentrations of these film-forming liquid hydrolysis pretreatment of copper corrosion by electrochemical impedance spectra and polarization curves were energy spectra were studied.Ib order to explore the best hydrolyzate concentration.Third,the four silane coupling agents modified by imide ring BA-AD-AA-TES,HBA-AD-AA-TES,BPDA-AA-TES,6FDA-AA-TES and commercialization 3-triethoxysilyl propylamine(γ-APS)and bis-(3-γ-triethoxysilylpropyl)tetrasulfide(A-1289)are respectively arranged hydrolysis pretreatment electroless copper deposition solution foil,a comparative study of four silane coupling agents modified imide ring and two other commercially available silane coupling pretreatment copper spectrum by polarization curves and electrochemical impedance spectra foil 0.1mol/ L NaCl solution corrosion conditions.Fourth,6FDA-AA-TES and BA-AD-AA-TES two kinds of imide ring-modified silane coupling agents based in its hydrolyzate doped nano-silica,study electrochemical anticorrosion foil.更多还原