导电银胶的研究与制备
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摘要
本论文研究了导电银胶的制备及性能。首先叙述了导电银胶的组成和各成分的选取原则，通过理论分析及实验，确定了热固型导电银胶的成分为：环氧树脂、酸酐类固化剂、改性咪唑类化合物为促进剂、5μm片状银粉为导电填料，并研究其电磁屏蔽性能。对热塑型导电银胶进行研究，确定其成分为：乙基纤维素、松油醇或二乙二醇单丁醚醋酸酯、银粉为导电填料，并将此导电银胶应用于柔性基底上。
对热固型银导电胶的基体树脂组成及固化性能进行讨论，并测试了其导电性、剪切强度、电磁屏蔽等性能。采用小电流电阻测试仪对导电银胶的导电性进行了测试，当银粉质量分数大于75%时，导电银胶的体积电阻率可达10-4数量级；采用数显电子万能试验机对导电银胶的粘接强度进行测试，当银粉填充量为60%时，导电银胶拉伸剪切强度为15.75MPa；采用电磁屏蔽暗室对导电银胶的电磁屏蔽性能进行测试，所配制的导电银胶屏蔽效能最高达51dB。研究了基体树脂各组分与导电银胶固化速度和适用期的关系，结果表明：促进剂用量为树脂基体的适用期和固化时间的主要影响因子，促进剂多，适用期变短，同时固化时间也会缩短；促进剂少，适用期变长，同时固化时间也会变长。同时研究了银粉形态和填充量对银导电胶性能的影响，研究表明：银粒子为片状时粒子间接触面积大，导电胶体电阻率最低；银粉填充量大，导电银胶固化后体积电阻率低，但同时粘接强度下降；随着银粉含量增加，屏蔽效能也增大，屏蔽效能还与涂层厚度有关。
对热塑型导电银胶的组成、制备及性能进行研究。通过对热塑型基体树脂的研究，确定乙基纤维素为热塑型导电银胶的高分子树脂，溶剂选用松油醇和二乙二醇单丁醚醋酸酯，且溶剂与高分子树脂的最佳量化比为4:1。研究热塑型导电银胶的印刷性能，选用非接触式印刷方式，网板选用不锈钢网板，承印材料为高分子膜。当溶剂与乙基纤维素的质量比为4:1时，导电银胶均易分散便于研磨，且印刷时易通过网孔，成线平整均一。研究了稀释剂对导电银胶的作用，结果表明：稀释剂在工艺涂布上能够改进导电银胶的印刷性能，对电阻值的影响具有不确定性。探索了三辊轧机制备导电银胶的工艺，结果表明：三辊轧机的混合效果优于手工制备。
本论文对热固型、热塑型导电银胶进行了初步的实验研究，为今后导电银胶产品的推出奠定了理论和实验基础。
The preparation and performance of the silver conductive adhesive were studied in thispaper. The silver conductive adhesive components and its selection principle were describedat first. Through theoretical analysis and experiments, the components of thermosetting silverconductive adhesive were confirmed: epoxy resin, acid anhydride curing agent, modifiedimidazole compounds used as curing accelerator,5μm flake silver powder used as conductivefiller. The thermoplastic silver conductive adhesive was also discussed. And it was made up of:ethyl cellulose, terpineol or two ethylene glycol monobutyl ether, and silver powder.
The components and curing properties of thermosetting silver conductive adhesivematrix were discussed, and its conductivity, adhesion strength and electromagnetic shieldingperformance were tested. The conductivity of silver conductive adhesive was tested by smallcurrent resistance tester, when the mass fraction of silver powder is more than75%, theresistivity can reach10-4cm; the adhesion strength of silver conductive adhesive was testedby digital electronic universal testing machine, and when the content of silver powder is60%,the tensile shear strength is15.75MPa; the electromagnetic shielding performance of silverconductive adhesive was tested by electromagnetic shielding room, and the shieldingeffectiveness can reach51dB. The relationship among the components of resin matrix andcuring speed and applicable term of silver conductive adhesive was studied. The resultsshowed that: the amount of curing accelerator is the main influence factor of resin matrixapplicable term and curing time. When the amount of accelerant is large, the applicationperiod is shorten, at the same time curing time will be shortened; with less accelerant, thesilver conductive adhesive is suitable for longer periods, at the same time, its curing time willbe longer. The influence of powder morphology and filling volume of silver on silverconductive adhesive properties was studied. The results show: the flake silver particles havelarge contact area, the conductive adhesive has lowest resistivity; with large silver content, thesilver conductive adhesive has low volume resistivity after cured, but at the same timeadhesion strength decreased; the shielding effectiveness increased with the silver contentincreased. Shielding effectiveness was also influenced by coating thickness.
The components, preparation and performance of the thermoplastic silver conductiveadhesive were studied. Based on the thermal plastic resin research, ethyl cellulose was chosenas thermoplastic conductive polymer resin; terpineol and two ethylene glycol monobutyl etherwere chosen as solvents. The optimal quantization ratio of solvent and polymer resin was4:1.The printing performance of thermoplastic silver conductive adhesive was studied.Non-contact printing method was chosen. The screen was stainless steel screen, and printingmaterials was polymeric membrane. When the ratio of solvent and ethyl cellulose mass was4:1, the silver conductive adhesive was dispersed easily and easy to grind, and easy to printthrough the mesh to form a smooth line. The effect of diluent on silver conductive adhesiveshowed that: in the process of coating can be improved by diluent, but the resistance value ofthe effect was uncertainty. The process of silver conductive adhesive with of three roller millwas explored, and the results show that the mixing effect of three roller mill is better than themanual preparation.
In this paper, thermosetting and thermoplastic silver conductive adhesive were studied. Andtheoretical and experimental basis were founded.
对热固型银导电胶的基体树脂组成及固化性能进行讨论，并测试了其导电性、剪切强度、电磁屏蔽等性能。采用小电流电阻测试仪对导电银胶的导电性进行了测试，当银粉质量分数大于75%时，导电银胶的体积电阻率可达10-4数量级；采用数显电子万能试验机对导电银胶的粘接强度进行测试，当银粉填充量为60%时，导电银胶拉伸剪切强度为15.75MPa；采用电磁屏蔽暗室对导电银胶的电磁屏蔽性能进行测试，所配制的导电银胶屏蔽效能最高达51dB。研究了基体树脂各组分与导电银胶固化速度和适用期的关系，结果表明：促进剂用量为树脂基体的适用期和固化时间的主要影响因子，促进剂多，适用期变短，同时固化时间也会缩短；促进剂少，适用期变长，同时固化时间也会变长。同时研究了银粉形态和填充量对银导电胶性能的影响，研究表明：银粒子为片状时粒子间接触面积大，导电胶体电阻率最低；银粉填充量大，导电银胶固化后体积电阻率低，但同时粘接强度下降；随着银粉含量增加，屏蔽效能也增大，屏蔽效能还与涂层厚度有关。
对热塑型导电银胶的组成、制备及性能进行研究。通过对热塑型基体树脂的研究，确定乙基纤维素为热塑型导电银胶的高分子树脂，溶剂选用松油醇和二乙二醇单丁醚醋酸酯，且溶剂与高分子树脂的最佳量化比为4:1。研究热塑型导电银胶的印刷性能，选用非接触式印刷方式，网板选用不锈钢网板，承印材料为高分子膜。当溶剂与乙基纤维素的质量比为4:1时，导电银胶均易分散便于研磨，且印刷时易通过网孔，成线平整均一。研究了稀释剂对导电银胶的作用，结果表明：稀释剂在工艺涂布上能够改进导电银胶的印刷性能，对电阻值的影响具有不确定性。探索了三辊轧机制备导电银胶的工艺，结果表明：三辊轧机的混合效果优于手工制备。
本论文对热固型、热塑型导电银胶进行了初步的实验研究，为今后导电银胶产品的推出奠定了理论和实验基础。
The preparation and performance of the silver conductive adhesive were studied in thispaper. The silver conductive adhesive components and its selection principle were describedat first. Through theoretical analysis and experiments, the components of thermosetting silverconductive adhesive were confirmed: epoxy resin, acid anhydride curing agent, modifiedimidazole compounds used as curing accelerator,5μm flake silver powder used as conductivefiller. The thermoplastic silver conductive adhesive was also discussed. And it was made up of:ethyl cellulose, terpineol or two ethylene glycol monobutyl ether, and silver powder.
The components and curing properties of thermosetting silver conductive adhesivematrix were discussed, and its conductivity, adhesion strength and electromagnetic shieldingperformance were tested. The conductivity of silver conductive adhesive was tested by smallcurrent resistance tester, when the mass fraction of silver powder is more than75%, theresistivity can reach10-4cm; the adhesion strength of silver conductive adhesive was testedby digital electronic universal testing machine, and when the content of silver powder is60%,the tensile shear strength is15.75MPa; the electromagnetic shielding performance of silverconductive adhesive was tested by electromagnetic shielding room, and the shieldingeffectiveness can reach51dB. The relationship among the components of resin matrix andcuring speed and applicable term of silver conductive adhesive was studied. The resultsshowed that: the amount of curing accelerator is the main influence factor of resin matrixapplicable term and curing time. When the amount of accelerant is large, the applicationperiod is shorten, at the same time curing time will be shortened; with less accelerant, thesilver conductive adhesive is suitable for longer periods, at the same time, its curing time willbe longer. The influence of powder morphology and filling volume of silver on silverconductive adhesive properties was studied. The results show: the flake silver particles havelarge contact area, the conductive adhesive has lowest resistivity; with large silver content, thesilver conductive adhesive has low volume resistivity after cured, but at the same timeadhesion strength decreased; the shielding effectiveness increased with the silver contentincreased. Shielding effectiveness was also influenced by coating thickness.
The components, preparation and performance of the thermoplastic silver conductiveadhesive were studied. Based on the thermal plastic resin research, ethyl cellulose was chosenas thermoplastic conductive polymer resin; terpineol and two ethylene glycol monobutyl etherwere chosen as solvents. The optimal quantization ratio of solvent and polymer resin was4:1.The printing performance of thermoplastic silver conductive adhesive was studied.Non-contact printing method was chosen. The screen was stainless steel screen, and printingmaterials was polymeric membrane. When the ratio of solvent and ethyl cellulose mass was4:1, the silver conductive adhesive was dispersed easily and easy to grind, and easy to printthrough the mesh to form a smooth line. The effect of diluent on silver conductive adhesiveshowed that: in the process of coating can be improved by diluent, but the resistance value ofthe effect was uncertainty. The process of silver conductive adhesive with of three roller millwas explored, and the results show that the mixing effect of three roller mill is better than themanual preparation.
In this paper, thermosetting and thermoplastic silver conductive adhesive were studied. Andtheoretical and experimental basis were founded.
引文
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[4] Rao Y, Lu D, Wong C P. Int J Adhesion Adhesives,2004,24:449
[5] Liong S, Wong C P. International Symposium on Advanced Packaging Mater,2001:13
[6] Li L, Morris J E. IEEE Transactions on CPMT Part A,1997,20(1):3
[7] WOJCIECHOWSKI D,VANFLETEREN J,REESE E, etal. Electro-conductive adhesivesfor high density package and flip-chip interconnections. MicroelectronicsReliability,2000,40(7):1215～1226.
[8] WU ZHEN-HUA, LI JIAN-ZHI, DOUGLAS T, et al. Study of processing variableson the electrical resistivity of conductive adhesives. International Journalof Adhesion and Adhesives,2009,29(5):488～494.
[9] Wong C P，Lu D，Meyers L，etal. Fundamental study of electrically conductiveadhesives (ECAs).1997.Norrkoping，Sweden:IEEE，Piscataway，NJ，USA
[10] MIR I，KUMAR D. Recent advances in isotropic conductive adhesives forelectronics packaging applications．International Journal of Adhesion andAdhesives，2008，28(7):362～371
[11]吴人洁.复合材料.天津:天津大学出版社，2000.158～160
[12] Li Y，Wong C P. Recent advances of conductive adhesives as a lead-freealternative in electronic packaging: Materials，processing，reliability andapplication. Materials Science and Engineering: R: Reports，2006，51(l-3):l～35
[13]代凯，施利毅，方建慧，等.导电胶粘剂的研究进展.材料导报，2006,20（3）：116～118
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