Study On Synthesis And Properties Of Imidized Organosilicon Materials

With the continuous progress of science and technology,traditional silane coupling agents capable of meeting the needs of industry in the early years,are now increasingly unable to reach the industrial requirements.Especially in recent years,polymer materials tailored to the miniaturization of electronic components in various cutting-edge electronic equipment demand strong interfacial properties.Silane coupling agent has different properties in different directions,among which the most widely used is in electrolytic copper foil surface corrosion treatment.Electrolytic copper foil plays important role in signal and power transmission for all electronic devices,and widely appear in everyday life.However,the corrosion resistance of electrolytic copper foil itself is inadequate,and the traditional silane coupling agent cannot meet the anticorrosion requirements of electronic science and technology.Therefore,the modification of silane coupling agent has become an urgent problem.This thesis intends to modify the silane coupling agent by imide ring structure to transform the performance,depending on the excellent thermal stability of imide ring which has been applied in wide range of industries including aerospace,military and civil fields.According to the above background materials,we use imide ring to modify the organosilicon materials,so as to transfer good thermal stability,to impart good corrosion resistance,and comprehensively study their performance,especially their thermal properties.In general,the thesis includes the following research parts:Firstly,using BPADA as the starting raw material,the compound BPADA-AA containing imide ring was synthesized by reacting with allyl amine,followed by reacting with triethoxysilane to introduce imide ring to silane coupling agent BPADA-AA-TES as an imidized silane,which was structurally characterized and studied in terms of thermal properties.At the same time,using CBDA as the reaction starting material,the compound CBDA-AA containing imide ring was synthesized by imidization with allyl amine,and the structure and properties of CBDA-AA were characterized by IR,¹HNMR and ¹³CNMR measurements.However,the synthsized CBDA-AA is very difficult to dissolve,so the hydrosilylation reaction with triethoxysilane was not fulfilled.As a result,the thermal performance of BPADA-AA-TES was analyzed by TGA and DSC measurements,showing Tg at 155℃and the decomposition temperature at 431℃.Secondly,BPADA-AA-TES were prepared into hydrolytic membrane solutions with different concentrations,and the conductivity of hydrolytic membranes with different concentrations was tested to ascertain the best concentration ratio and the best hydrolysis time.Through the tests,we found that the optimal concentration ratio of silane:ethanol:water=5:90:5.The best hydrolysis time is 26h.The optimal hydrolysis time was verified by contact Angle test at different ratio.Experiments show that the maximum contact Angle is 97.8°when the concentration ratio is silane:ethanol:water=5:90:5,which is also in agreement with conductivity variation.BPADA-AA-TES was used to treat bare copper foil under the best proportion of hydrolysis liquid membrane,and the process consisted of immersing the EFC in the aqueous alcoholic liquids,and thermal cure to effect the condensation,followed by corrosion tests.By comparison,it has been found that imidized silane show robust corrosion inhibition for ECF.Despite slight difference in corrosion prevention between different concentration,all the formulations demonstrated adequate anti-corrosion performance.When the component ratio of hydrolytic solution of silane:ethanol:water=0:5 goes out when the best anti-corrosion effect.The corrosion effect and corrosion environment are also corelated,and the corrosion in alkaline environment is more readily to take place.Thirdly,BPADA-AA-TES was hydrolytically condensed into POSS structure,and its thermal performance was analyzed.TGA and DSC measurements showed that Tg was 211℃and decomposition temperature was 452℃,indicating that POSS network structure had higher thermal stability than BPADA-AA-TES.Meanwhile,the polymerization was carried by reacting the allyl imiminated compound BPADA-AA with 1,1,3,3-tetramethylsiloxane and generated a new imidized polysiloxane,which was characterized in terms of thermal properties.From TGA and DSC tests,Tg was detected at 251℃and decomposition temperature at 474℃,indicating that imide poly（imide siloxane）has better heat resistance than BPADA-AA-TES.