CN114269849A - 银粒子的制造方法、热固化性树脂组合物、半导体装置以及电气电子部件 - Google Patents
银粒子的制造方法、热固化性树脂组合物、半导体装置以及电气电子部件 Download PDFInfo
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- CN114269849A CN114269849A CN202080059294.9A CN202080059294A CN114269849A CN 114269849 A CN114269849 A CN 114269849A CN 202080059294 A CN202080059294 A CN 202080059294A CN 114269849 A CN114269849 A CN 114269849A
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- silver
- particles
- thermosetting resin
- silver particles
- resin composition
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 147
- 239000004332 silver Substances 0.000 title claims abstract description 147
- 229920001187 thermosetting polymer Polymers 0.000 title claims abstract description 83
- 239000011342 resin composition Substances 0.000 title claims abstract description 65
- 239000004065 semiconductor Substances 0.000 title claims description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 18
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- 239000011347 resin Substances 0.000 claims abstract description 47
- 239000011163 secondary particle Substances 0.000 claims abstract description 36
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- 150000001875 compounds Chemical class 0.000 claims description 40
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- 239000002002 slurry Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 18
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Abstract
本发明提供一种热固化性树脂组合物,其含有:(A)银粒子,由平均粒径为0.5~5.0μm的二次粒子构成,所述二次粒子由平均粒径为10~100nm的一次粒子凝集而成;以及(B)热固化性树脂。
Description
技术领域
本发明涉及银粒子的制造方法、热固化性树脂组合物、半导体装置以及电气电子部件。
背景技术
近年来,半导体元件的高效化正在推进,与此同时,半导体元件的发热量增加、驱动温度提高。另外,对接合材料要求高温条件下的可靠性以及散热性。作为接合材料的候选,可举出以往使用的焊料以及银膏。但是,由于它们的可靠性和散热性不充分因而无法应对,迫切希望提供适合高温动作的接合方法。例如,专利文献1中提出了通过低温烧成而表现出优异导电性的使用了银纳米粒子的银烧结(烧结)膏。
现有技术文献
专利文献
专利文献1:日本特开2013-142173号公报。
发明内容
发明要解决的问题
即,本发明涉及如下内容。
[1]一种热固化性树脂组合物,其含有:(A)银粒子,由平均粒径为0.5~5.0μm的二次粒子构成,所述二次粒子由平均粒径为10~100nm的一次粒子凝集而成;以及(B)热固化性树脂。
[2]一种半导体装置,其是通过含有上述[1]所述的热固化性树脂组合物的芯片粘接材料将半导体元件和基板粘接而成的。
[3]一种电气电子部件,其是通过含有上述[1]所述的热固化性树脂组合物的散热部件粘接用材料将散热部件和发热部件粘接而成。
[4]一种银粒子的制造方法,所述银粒子由平均粒径为0.5~5.0μm的二次粒子构成,该二次粒子由平均粒径为10~100nm的一次粒子凝集而成,所述制造方法具有:在含有银化合物的水溶液中添加氨水而得到银氨络合物溶液的工序;以及用还原性化合物将所述工序中得到的银氨络合物溶液中的银氨络合物进行还原,得到含银粒子的浆料的工序。
具体实施方式
下面,参照一个实施方式来详细说明本发明。
<热固化性树脂组合物>
本实施方式的热固化性树脂组合物包含:(A)银粒子,由平均粒径为0.5~5.0μm的二次粒子构成,所述二次粒子由平均粒径为10~100nm的一次粒子凝集而成;以及(B)热固化性树脂。
〔(A)银粒子〕
(A)成分的银粒子由平均粒径为0.5~5.0μm的二次粒子构成,该二次粒子由平均粒径为10~100nm的一次粒子凝集而成。
上述一次粒子的平均粒径小于10nm时,比表面积增大,热固化性树脂组合物的作业性有可能降低,上述一次粒子的平均粒径大于100nm时,烧结性有可能降低。根据这种观点,上述一次粒子的平均粒径可以为10~50nm,也可以为20~50nm。
上述一次粒子的平均粒径能够如下所述地测定,具体而言,能够通过实施例中记载的方法测定。
在60℃、120分钟的固化条件下,将银粒子嵌入环氧树脂。在加工电压为4.0kV、倾斜角度为80°且加工时间为1.5分钟的条件下,利用聚焦离子束(FIB)装置对其进行平面研磨。通过场发射型扫描电子显微镜(FE-SEM)在加速电压为1.0kV、倍率为10000~200000倍的条件下观察得到的球状银粒子的截面,从而测定200个银粒子的圆当量直径。利用图像分析软件对测定的200个银粒子的圆当量直径进行图像处理,并进行个数平均来求出。
另外,上述二次粒子的平均粒径小于0.5μm时,保存稳定性有可能降低,上述二次粒子的平均粒径大于5.0μm时,烧结性有可能降低。根据这种观点,上述二次粒子的平均粒径可以为0.5~3.0μm,也可以为1.0~3.0μm.
上述二次粒子的平均粒径是在使用激光衍射式粒度分布测定装置测定的粒度分布中累计体积为50%的粒径(50%粒径D50),具体而言,能够通过实施例中记载的方法进行测定。
(A)成分的银粒子是纳米尺寸的一次粒子凝集而成的二次粒子,由此,保持该一次粒子的表面所具有的高活性,在低温条件下具有二次粒子之间的烧结性(自烧结性)。另外,银粒子之间的烧结、以及银粒子和接合部件的烧结同时进行。因此,通过使用(A)成分的银粒子,能够得到热传导性优异且低热电阻、粘接特性优异的热固化性树脂组合物。
对(A)成分的银粒子的形状没有特别的限定,例如,可举出球状、薄片状(flake)等。(A)成分的银粒子的形状也可以为球状。
另外,(A)成分的银粒子可以为中空粒子,也可以为实心粒子,从低温烧结性的观点出发,也可以为中空粒子。此处,中空粒子是指粒子内部存在空隙的粒子。(A)成分的银粒子为中空粒子时,银粒子的中央部也可以存在空隙。另外,实心粒子是指粒子内部实质上不存在空间的粒子。
(A)成分的银粒子的振实密度可以为4.0~7.0g/cm3,可以为4.5~7.0g/cm3,也可以为4.5~6.5g/cm3。上述银粒子的振实密度为4.0g/cm3以上时,能够在热固化性树脂组合物中填充大量银粒子,上述银粒子的振实密度为7.0g/cm3以下时,能够降低热固化性树脂组合物中银粒子的沉降。
能够根据ASTM标准试验方法B 527,使用振实密度测定器来测定上述银粒子的振实密度,具体而言,能够通过实施例中记载的方法测定。
根据BET法求出的(A)成分的银粒子的比表面积可以为0.5~1.5m2/g,可以为0.5~1.2m2/g,也可以为0.6~1.2m2/g。上述银粒子的比表面积为0.5m2/g以上时,能够增加银粒子之间的接触,比表面积为1.5m2/g以下时,能够将热固化性树脂组合物低粘度化。
能够使用比表面积测定装置,通过基于氮吸附的BET单点法来测定上述银粒子的比表面积,具体而言,能够通过实施例中记载的方法测定。
(A)成分的银粒子还可以在烧成温度区域即150℃~300℃之间具有正的热膨胀系数。(A)银粒子的热膨胀系数可以为0.2~10.0ppm/℃,也可以为1.5~8.0ppm/℃。
在本发明中,对于银粒子的热膨胀系数,使用小型液压机(英国Specac公司制)对Ag粉银粒子施加1分钟的负荷200kgf,制作直径5mm且厚度1mm的圆柱型的颗粒型试样,使用热机械分析(TMA)装置(精工仪器株式会社(Seiko Instruments Inc.)制,商品名:TMASS150),在从常温(25℃)以升温速度20℃/分钟升温至350℃的条件下,对得到的所述试样测定热膨胀。然后,求出以25℃的颗粒长度为基准时的热膨胀系数,将其作为烧成温度区域即150℃~300℃之间的热膨胀系数。
另外,具有正线膨胀系数的银粒子的烧结起始温度是收缩开始的时刻、也就是热膨胀系数达到最大的时刻的温度。通常,其温度范围在150~300℃之间。
构成银烧结膏的银纳米粒子因烧结产生的收缩较大,在可靠性试验前后的热电阻的变化率较大。因此,需要收缩小、可靠性试验前后热电阻变化率小的银烧结膏。
对于(A)成分的银粒子,显示热膨胀系数时的温度在上述范围时,热固化性树脂组合物在烧结时银粒子膨胀,从而银粒子之间接触的机会增加,因此烧结性良好,能得到高热传导性。同时,由于起到抵消烧结时体积收缩的作用,因此热电阻的变化率变小。
热固化性组合物中的(A)成分的银粒子的含量可以为20~95质量%,也可以为40~90质量%。
热固化性组合物也可以含有除(A)成分的银粒子以外的银粒子。热固化性组合物含有除(A)成分的银粒子以外的银粒子时,热固化性组合物中的除(A)成分的银粒子以外的银粒子的含量可以为35质量%以下,可以为25质量%以下,可以为10质量%以下,也可以为5质量%以下。
((A)银粒子的制造方法)
(A)成分的银粒子的制造方法包括:在含有银化合物的水溶液中添加氨水而得到银氨络合物溶液的工序;以及用还原性化合物将所述工序中得到的银氨络合物溶液中的银氨络合物进行还原,得到含银粒子的浆料的工序。
(得到银氨络合物溶液的工序)
在本工序中,在含有银化合物的水溶液中添加氨水而得到银氨络合物溶液。
作为银化合物,可举出硝酸银、氯化银、乙酸银、草酸银、氧化银等。从在水中的溶解度的观点出发,银化合物可以为硝酸银、乙酸银。
相对于含有银化合物的水溶液中的每1mol银,氨的添加量可以为2~50mol,可以为5~50mol,也可以为10~50mol。氨的添加量为上述范围内时,能够将一次粒子的平均粒径设为上述范围内。
(得到含银粒子的浆料的工序)
在本工序中,用还原性化合物将所述工序中得到的银氨络合物溶液中的银氨络合物进行还原,得到含银粒子的浆料。
通过用还原性化合物将银氨络合物进行还原,银氨络合物中的银粒子的一次粒子凝集,形成在中央具有空隙的二次粒子(中空粒子)。
通过适当调整银氨络合物中的银量和还原性化合物的含量,能够控制上述一次粒子的凝集,从而能够使得到的二次粒子的平均粒径在上述范围内。
只要还原性化合物具有将银氨络合物还原并使银析出的还原力,就没有特别限定。作为还原性化合物,例如,可举出肼衍生物。作为肼衍生物,例如,可举出肼一水合物、甲基肼、乙基肼、正丙基肼、异丙基肼、正丁基肼、异丁基肼、仲丁基肼、叔丁基肼、正戊基肼、异戊基肼、新戊基肼、叔戊基肼、正己基肼、异己基肼、正庚基肼、正辛基肼、正壬基肼、正癸基肼、正十一烷基肼、正十二烷基肼、环己基肼、苯基肼、4-甲基苯基肼、苄基肼、2-苯基乙基肼、2-肼基乙醇、乙酰肼等。这些可以单独使用,也可以并用2种以上。
相对于银氨络合物中的每1mol银,还原性化合物的含量可以为0.25~20.0mol,可以为0.25~10.0mol,也可以为0.25~5.0mol。还原性化合物的含量为上述范围内时,能够使得到的二次粒子的平均粒径在上述范围内。
进一步,将银氨络合物还原时的银氨络合物溶液的温度可以为小于30℃,也可以为0~20℃。如果银氨络合物溶液的温度为该范围,能够控制上述一次粒子的凝集,并且能够使得到的二次粒子的平均粒径在上述范围内。
(将保护基导入银粒子的工序)
(A)成分的银粒子的制造方法可以具有:在得到所述含银粒子的浆料的工序之后,进一步在所述工序中得到的含银粒子的浆料中添加有机保护化合物,将保护基导入该银粒子的工序。
作为有机保护化合物,例如,可举出羧酸、胺、酰胺等。从提高分散性的观点出发,有机保护化合物可以为羧酸。
作为羧酸,例如,可举出甲酸、乙酸、丙酸、丁酸、戊酸、己酸、辛酸、辛酸、壬酸、癸酸、油酸、硬脂酸、异硬脂酸等一元羧酸;草酸、丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、二甘醇酸等二羧酸;苯甲酸、邻苯二甲酸、间苯二甲酸、对苯二甲酸、水杨酸、没食子酸等芳香族羧酸;乙醇酸、乳酸、丙醇二酸、苹果酸、甘油酸、羟基丁酸、酒石酸、柠檬酸、异柠檬酸等羟基酸等。
相对于1mol银粒子,有机保护化合物的配合量可以为1~20mmol,可以为1~10mmol,也可以为1~5mmol。有机保护化合物的配合量为1mmol以上时,银粒子能够分散在树脂中,有机保护化合物的配合量为20mmol以下时,银粒子不损害烧结性,能够分散在树脂中。
〔(B)热固化性树脂〕
只要(B)热固化性树脂是通常作为粘接剂用途使用的热固化性树脂,就能够没有特别限定地使用。上述热固化性树脂可以为液态树脂,也可以为室温(25℃)条件下为液态的树脂。作为上述热固化性树脂,可以为从氰酸酯树脂、环氧树脂、丙烯酸树脂和马来酰亚胺树脂中选出的至少一种。这些可以单独使用,也可以并用2种以上。
氰酸酯树脂是分子内具有-NCO基的化合物,是通过加热使-NCO基反应而形成三维网状结构并固化的树脂。具体而言,可举出1,3-二氰酸基苯、1,4-二氰酸基苯、1,3,5-三氰酸基苯、1,3-二氰酸基萘、1,4-二氰酸基萘、1,6-二氰酸基萘、1,8-二氰酸基萘、2,6-二氰酸基萘、2,7-二氰酸基萘、1,3,6-三氰酸基萘、4,4’-二氰酸基联苯、双(4-氰酸基苯基)甲烷、双(3,5-二甲基-4-氰酸基苯基)甲烷、2,2-双(4-氰酸基苯基)丙烷、2,2-双(3,5-二溴-4-氰酸基苯基)丙烷、双(4-氰酸基苯基)醚、双(4-氰酸基苯基)硫醚、双(4-氰酸基苯基)砜、三(4-氰酸基苯基)亚磷酸酯、三(4-氰酸基苯基)磷酸酯、以及通过酚醛清漆树脂与卤化氰的反应而得到的氰酸酯类等。另外,也能够使用通过对这些多官能团氰酸酯树脂的氰酸酯基进行三聚而形成的具有三嗪环的预聚物。该预聚物,通过例如以无机酸、路易斯酸等酸、醇钠、叔胺类等碱、碳酸钠等盐类为催化剂并使上述多官能团氰酸酯树脂单体进行聚合而得到的。
作为氰酸酯树脂的固化促进剂,能够使用一般公知的物质。例如,可举出辛酸锌、辛酸锡、环烷酸钴、环烷酸锌、乙酰丙酮铁等有机金属络合物;氯化铝、氯化锡、氯化锌等金属盐;三乙胺、二甲基苄胺等胺类,但并不限定于这些。这些固化促进剂能够使用1种或混合使用2种以上。
环氧树脂是在分子内具有1个以上的缩水甘油基的化合物,是通过加热使缩水甘油基反应而形成三维网状结构并固化的树脂。上述环氧树脂也可以为1分子中含有2个以上的缩水甘油基的化合物。这是因为,缩水甘油基仅为1个的化合物即使反应也不能表现出充分的固化物特性。1分子中包含2个以上的缩水甘油基的化合物能够通过将具有2个以上的羟基的化合物进行环氧化而得到。作为这种化合物,可举出双酚A、双酚F、联苯酚等双酚化合物或这些的衍生物、氢化双酚A、氢化双酚F、氢化联苯酚、环己二醇、环己烷二甲醇、环己烷二乙醇等具有脂环结构的二醇或这些的衍生物;将丁二醇、己二醇、辛二醇、壬二醇、癸二醇等脂肪族二醇或这些的衍生物等环氧化而成的双官能团化合物;将具有三羟苯基甲烷骨架、氨基苯酚骨架的化合物等环氧化而成的三官能团化合物;将苯酚酚醛清漆树脂、邻甲酚酚醛清漆树脂、苯酚芳烷基树脂、联苯芳烷基树脂、萘酚芳烷基树脂等环氧化而成的多官能团化合物等,但并不限于这些。另外,为使热固化性树脂组合物在室温(25℃)条件下为膏状,上述环氧树脂也可以是以单独或以混合物的形式在室温(25℃)条件下为液态的化合物。也可以像通常进行的那样使用反应性稀释剂。作为反应性稀释剂,可举出苯基缩水甘油醚、甲苯基缩水甘油醚等单官能团的芳香族缩水甘油醚类、脂肪族缩水甘油醚类等。
作为环氧树脂的固化剂,例如,可举出脂肪族胺、芳香族胺、双氰胺、二酰肼化合物、酸酐、酚醛树脂等。作为二酰肼化合物,可举出己二酸二酰肼、十二烷酸二酰肼、间苯二甲酸二酰肼、对氧基苯甲酸二酰肼等羧酸二酰肼等。作为酸酐,可举出邻苯二甲酸酐、四氢邻苯二甲酸酐、六氢邻苯二甲酸酐、桥-亚甲基四氢邻苯二甲酸酐、十二烯基琥珀酸酐、马来酸酐与聚丁二烯的反应物、马来酸酐与苯乙烯的共聚体等。
进一步,为了促进固化,能够配合固化促进剂,作为环氧树脂的固化促进剂,可举出咪唑类、三苯基膦或四苯基膦及它们的盐类、二氮杂双环十一碳烯等胺系化合物及其盐类等。固化促进剂可以为2-甲基咪唑、2-乙基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、2-苯基-4-甲基-5-羟甲基咪唑、2-苯基-4,5-二羟甲基咪唑、2-C11H23-咪唑、2-甲基咪唑与2,4-二氨基-6-乙烯基三嗪的加成物等咪唑化合物。也可以为熔点180℃以上的咪唑化合物。
作为丙烯酸树脂,例如,可举出2-羟乙基(甲基)丙烯酸酯、2-羟丙基(甲基)丙烯酸酯、3-羟丙基(甲基)丙烯酸酯、2-羟丁基(甲基)丙烯酸酯、3-羟丁基(甲基)丙烯酸酯、4-羟丁基(甲基)丙烯酸酯、1,2-环己二醇单(甲基)丙烯酸酯、1,3-环己二醇单(甲基)丙烯酸酯、1,4-环己二醇单(甲基)丙烯酸酯、1,2-环己烷二甲醇单(甲基)丙烯酸酯、1,3-环己烷二甲醇单(甲基)丙烯酸酯、1,4-环己烷二甲醇单(甲基)丙烯酸酯、1,2-环己烷二乙醇单(甲基)丙烯酸酯、1,3-环己烷二乙醇单(甲基)丙烯酸酯、1,4-环己烷二乙醇单(甲基)丙烯酸酯、甘油单(甲基)丙烯酸酯、甘油二(甲基)丙烯酸酯、三羟甲基丙烷单(甲基)丙烯酸酯、三羟甲基丙烷二(甲基)丙烯酸酯、季戊四醇单(甲基)丙烯酸酯、季戊四醇二(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、新戊二醇单(甲基)丙烯酸酯等具有羟基的(甲基)丙烯酸酯以及使这些具有羟基的(甲基)丙烯酸酯与二羧酸或其衍生物反应而得到的具有羧基的(甲基)丙烯酸酯等。作为此处能够使用的二羧酸,例如,可举出草酸、丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、马来酸、富马酸、邻苯二甲酸、四氢邻苯二甲酸、六氢邻苯二甲酸以及这些的衍生物等。
另外,作为丙烯酸树脂,可举出分子量为100~10000的聚醚、聚酯、聚碳酸酯、聚(甲基)丙烯酸酯等具有(甲基)丙烯酰基的化合物;具有羟基的(甲基)丙烯酸酯;具有羟基的(甲基)丙烯酰胺等。
马来酰亚胺树脂为1分子内包含1个以上的马来酰亚胺基的化合物,是通过加热使马来酰亚胺基反应从而形成三维网状结构并固化的树脂。作为马来酰亚胺树脂,例如,可举出N,N’-(4,4’-二苯基甲烷)双马来酰亚胺、双(3-乙基-5-甲基-4-马来酰亚胺苯基)甲烷、2,2-双[4-(4-马来酰亚胺苯氧基)苯基]丙烷等双马来酰亚胺树脂。马来酰亚胺树脂可以为通过二聚酸二胺与马来酸酐的反应而得到的化合物;通过马来酰亚胺基乙酸、马来酰亚胺基己酸这样的马来酰亚胺化氨基酸与多元醇的反应而得到的化合物。上述马来酰亚胺化氨基酸通过使马来酸酐与氨基乙酸或氨基己酸反应而得到。作为上述多元醇,可以为聚醚多元醇、聚酯多元醇、聚碳酸酯多元醇、聚(甲基)丙烯酸酯多元醇,也可以为不含芳香族环的多元醇。
相对于(A)银粒子100质量份,(B)热固化性树脂的含量可以为1~20质量份,也可以为5~18质量份。(B)热固化性树脂为1质量份以上时,能够得到热固化性树脂带来的粘接性,(B)热固化性树脂为20质量份以下时,能够控制银成分的比例降低,能够充分确保高热传导性,能够提高散热性。另外,有机成分不会过多,能够抑制光和热引起的劣化,其结果是,能够提高发光装置的寿命。
热固化性组合物中的(A)银粒子与(B)热固化性树脂的合计含量可以为30~99质量%,也可以为50~98质量%。
〔(C)稀释剂〕
从作业性的观点出发,本实施方式的热固化性树脂组合物还可以含有(C)稀释剂。作为(C)稀释剂,例如可举出丁基卡必醇、乙酸溶纤剂、乙基溶纤剂、丁基溶纤剂、丁基溶纤剂乙酸酯、丁基卡必醇乙酸酯、二乙二醇二甲醚、二丙酮醇、N-甲基-2-吡咯烷酮(NMP)、二甲基甲酰胺、N,N-二甲基乙酰胺(DMAc)、γ-丁内酯、1,3-二甲基-2-咪唑啉酮、3,5-二甲基-1-金刚烷胺(DMA)等。这些可以单独使用,也可以并用2种以上。
在本实施方式的热固化性树脂组合物含有(C)稀释剂时,相对于(A)银粒子100质量份,所述(C)稀释剂的含量可以为3~20质量份,可以为4~15质量份,也可以为4~10质量份。(C)稀释剂的含量为3质量份以上时,能够通过稀释来进行低粘度化,(C)稀释剂的含量为20质量份以下时,能够控制本实施方式的热固化性树脂组合物固化时的空隙的产生。
〔其他成分〕
本实施方式热固化性树脂组合物除了以上各成分以外,根据需要也能够含有通常配合在这种组合物中的橡胶、硅酮等低应力化剂;偶联剂;消泡剂;表面活性剂;颜料、染料等着色剂;各种阻聚剂;抗氧化剂;溶剂;其他各种添加剂。这些各添加剂均可以使用1种,也可以混合2种以上使用。
本实施方式的热固化性树脂组合物能够通过将上述(A)银粒子、(B)热固化性树脂、根据需要含有的(C)稀释剂和各种添加剂充分混合后,进一步利用分散机、捏合机、三辊研磨机等进行混炼处理,然后进行脱泡来制备。
本实施方式的热固化性树脂组合物的固化物的热传导率可以为35W/mK以上,也可以为40W/mK以上。
本实施方式的热固化性树脂组合物的固化物的热电阻可以为0.5K/W以下,也可以为0.3K/W以下。
上述热传导率以及热电阻能够分别通过实施例中记载的方法来测定。
本实施方式的热固化性树脂组合物的粘度可以为70~200Pa·s,也可以为100~200Pa·s。
上述粘度为使用E型粘度计(3°锥角)在25℃条件下测定的值。具体而言,能够通过实施例中记载的方法测定。
本实施方式的热固化性树脂组合物由于能够得到低粘度、分散性和粘接特性良好、热传导性优异、低热电阻、体积收缩小且低应力性优异的固化物,因此能够作为元件粘接用芯片粘接材料、散热部件粘接用材料等使用。
<半导体装置以及电气电子部件>
本实施方式的半导体装置通过含有上述热固化性树脂组合物的芯片粘接材料将半导体元件和基板粘接而成。另外,本实施方式的电气电子部件是通过含有上述热固化性树脂组合物的散热部件粘接用材料将散热部件和发热部件粘接而成。因此,本实施方式的半导体装置及电气电子部件的可靠性优异。
半导体元件可以为公知的半导体元件,例如,可举出晶体管、二极管等。进一步,作为上述半导体元件,可举出LED等发光元件。另外,对发光元件的种类没有特别的限定,例如,也可举出通过MOBVC法等在基板上形成InN、AlN、GaN、InGaN、AlGaN、InGaAlN等氮化物半导体作为发光层而成的元件。
另外,作为元件支撑部件,可举出通过铜、镀铜的铜、PPF(预镀引线框架)、玻璃环氧树脂、陶瓷等材料形成的支撑部件。
通过使用本实施方式的芯片粘接材料,半导体元件还能够与未经金属镀处理的基材接合。与以往相比,如此得到的半导体装置在安装后对温度循环的连接可靠性显著提高。另外,由于电阻值足够小,经时变化小,因此,具有即使长时间驱动输出的经时减少也少且寿命也长的优点。
作为发热部件,可以为上述半导体元件或具有该半导体元件的部件,也可以为除此之外的发热部件。作为除半导体元件以外的发热部件,可举出光拾取器、功率晶体管等。另外,作为散热部件,可举出散热器(heat sink)、散热片(heat spreader)等。
如上所述,通过使用上述散热部件粘接用材料将散热部件粘接于发热部件,能够将发热部件中产生的热从散热部件高效地释放到外部,能够抑制发热部件的温度上升。此外,发热部件和散热部件可以通过散热部件粘接用材料直接粘接,也可以将其他热传导率高的部件夹在中间而间接地粘接。
实施例
下面,通过实施例具体地说明本发明,但是本发明并不受这些示例任何限定。
(银粒子的制造)
[合成例1]
将40g硝酸银溶解于10L的离子交换水中,制备硝酸银水溶液,向其中添加浓度26质量%的氨水203mL并搅拌,得到银氨络合物水溶液。将该水溶液设定为液温10℃,一边搅拌一边用60秒滴加20质量%的肼一水合物水溶液28mL,使银粒子析出,得到含银粒子的浆料。向该浆料中加入相对于银量为1质量%的油酸,搅拌10分钟。将该浆料过滤,对滤渣进行水洗、甲醇清洗,以60℃、24小时在真空环境下干燥,得到一次粒子的平均粒径为20nm、二次粒子的平均粒径为1.1μm、最大热膨胀系数为+5.5ppm/℃、振实密度为5.4g/cm3、比表面积为1.2m2/g的银粒子。
此外,用场发射型扫描电子显微镜(FE-SEM)(日本电子株式会社(JEOL社)制的JSM-6700F)观察得到的银粒子的截面,确认该银粒子是中央具有空隙的中空粒子。
[合成例2]
将40g硝酸银溶解于10L的离子交换水中,制备硝酸银水溶液,向其中添加浓度26质量%的氨水203mL并搅拌,得到银氨络合物水溶液。将该水溶液设定为液温10℃,一边搅拌一边用60秒滴加20质量%的肼一水合物水溶液18mL,使银粒子析出,得到含银粒子的浆料。向该浆料中加入相对于银量为1质量%的油酸,搅拌10分钟。将该浆料过滤,对滤渣进行水洗、甲醇清洗,以60℃、24小时在真空环境下干燥,得到一次粒子的平均粒径为20nm、二次粒子的平均粒径为1.5μm、最大热膨胀系数为+7.0ppm/℃、振实密度为5.2g/cm3、比表面积为1.1m2/g的银粒子。
[合成例3]
将40g硝酸银溶解于10L的离子交换水中,制备硝酸银水溶液,向其中添加浓度26质量%的氨水203mL并搅拌,得到银氨络合物水溶液。将该水溶液设定为液温10℃,一边搅拌一边用60秒滴加20质量%的肼一水合物水溶液12mL,使银粒子析出,得到含银粒子的浆料。向该浆料中加入相对于银量为1质量%的油酸,搅拌10分钟。将该浆料过滤,对滤渣进行水洗、甲醇清洗,以60℃、24小时在真空环境下干燥,得到一次粒子的平均粒径为20nm、二次粒子的平均粒径为2.6μm、最大热膨胀系数为+7.4ppm/℃、振实密度为5.0g/cm3、比表面积为1.0m2/g的银粒子。
用下述方法对合成例1~3中得到的银粒子进行评价。
[一次粒子的平均粒径]
在上述各合成例中得到的银氨络合物水溶液1020mL中,用60秒滴加20质量%的肼一水合物水溶液2.8mL,进行固液分离,用纯水洗涤得到的固体物,以60℃、24小时在真空环境下进行干燥而得到银粒子,使用该银粒子进行一次粒子的平均粒径的测定。
如下所述地测定上述一次粒子的平均粒径。
在60℃、120分钟的固化条件下,将银粒子嵌入环氧树脂CLR(美国标乐公司(Buehler Ltd.)制)。用聚焦离子束(FIB)装置(日本电子株式会社(JEOL社)制的JEM-9310FIB)在加工电压为4.0kV、倾斜角度为80°、加工时间为1.5分钟的条件下对其进行平面研磨。用场发射型扫描电子显微镜(FE-SEM)(日本电子株式会社(JEOL社)制的JSM-6700F)在加速电压为1.0kV、倍率为10000~200000倍的条件下观察得到的球状银粒子的截面,从而测定了200个银粒子的圆当量直径。利用图像分析软件ImageJ(美国国立卫生研究所(National Institutes of Health)制)对测定的200个银粒子的圆当量直径进行图像处理,进行个数平均来求出。
[二次粒子的平均粒径]
二次粒子的平均粒径,根据使用激光衍射式粒度分布测定装置(株式会社岛津制作所制造,商品名:SALAD-7500nano)测定的粒度分布中累计体积为50%的粒径(50%粒径D50)来求出。
[热膨胀系数]
使用小型油压机(英国Specac公司制造)对银粒子施加1分钟的负荷200kgf,得到了直径5mm且厚度1mm的圆柱型的颗粒型试样。使用热机械分析(TMA)装置(精工仪器株式会社(Seiko Instruments Inc.)制,商品名:TMA SS150),在从常温(25℃)以升温速度20℃/分钟升温至350℃的条件下对其测定热膨胀,求出以25℃的颗粒长度为基准时的热膨胀系数,将在烧成温度区域即150℃~300℃之间最大的热膨胀系数作为最大热膨胀系数。
[振实密度]
基于ASTM标准试验方法B527,利用振实密度测定器(Tap-Pak Volumeter,美国赛默飞世尔科技公司制),以振动容器内的银粒子的每单位体积的质量(单位:g/cm3)来测定振实密度(TD)。
[比表面积]
以60℃脱气10分钟后,使用比表面积测定装置(Monosorb,美国康塔(Quanatachrome)公司制),通过基于氮吸附的BET单点法来测定比表面积。
[实施例1~8、比较例1~5]
按照表1的配方将各成分混合,用三辊磨机进行混炼,得到热固化性树脂组合物。用后述的方法对得到的热固化性树脂组合物进行评价。将其结果示于表1。需要说明的是,在表1中,空栏表示未配合。
实施例和比较例中使用的表1中记载的各材料如下所示。
〔(A)银粒子〕
·(A1):合成例1中得到的银粒子(一次粒子的平均粒径:20nm;二次粒子的平均粒径:1.1μm;最大热膨胀系数:+5.5ppm/℃;振实密度:5.4g/cm3;比表面积:1.2m2/g)
·(A2):合成例2中得到的银粒子(一次粒子的平均粒径:20nm;二次粒子的平均粒径:1.5μm;最大热膨胀系数:+7.0ppm/℃;振实密度:5.2g/cm3;比表面积:1.1m2/g)
·(A3):合成例3中得到的银粒子(一次粒子的平均粒径:20nm;二次粒子的平均粒径:2.6μm;最大热膨胀系数:+7.4ppm/℃;振实密度:5.0g/cm3;比表面积:1.0m2/g)
〔除(A)成分以外的银粒子〕
·TC-505C(德力本店株式会社制;商品名;平均粒径:1.93μm;最大热膨胀系数:-0.1ppm/℃;振实密度:6.25g/cm3;比表面积:0.65m2/g)
·Ag-HWQ 1.5μm(福田金属箔粉工业株式会社制;商品名;平均粒径:1.8μm;最大热膨胀系数:-0.6ppm/℃;振实密度:3.23g/cm3;比表面积:0.5m2/g)
·AgC-221PA(福田金属箔粉工业株式会社制;商品名;平均粒径:7.5μm;最大热膨胀系数:-0.1ppm/℃;振实密度:5.7g/cm3;比表面积:0.3m2/g)
·DOWA Ag纳米粉末-1(DOWA电子株式会社(DOWAエレクトロニクス(株))制;商品名;平均粒径:20nm;最大热膨胀系数:-0.1ppm/℃)
·DOWA Ag纳米粉末-2(DOWA电子株式会社(DOWAエレクトロニクス(株))制;商品名;平均粒径:60nm;最大热膨胀系数:-0.1ppm/℃)
〔(B)热固化性树脂〕
·环氧树脂:(三菱化学株式会社制;商品名;YL983U)
·丙烯酸树脂(KJ化学株式会社(KJケミカルズ(株))制;商品名:HEAA(注册商标))
·双酚F(本州化学工业株式会社制;商品名;双酚F)
〔(C)稀释剂〕
·丁基卡必醇(东京化成工业株式会社制)
〔其他成分〕
·咪唑(四国化成工业株式会社制;商品名:Curezol 2P4MHZ-PW)
·二枯基过氧化物(日本油脂株式会社制;商品名:Percumyl(注册商标)D)
<评价方法>
[热传导率]
测定器:LFA-502(京都电子工业株式会社制)
测定方法:激光闪光法
根据JIS R 1611-1997,使用上述测定器,通过激光闪光法来测定热固化性树脂组合物的固化物的热传导率。
[体积电阻率]
通过丝网印刷法将热固化性树脂组合物涂布于玻璃基板(厚度1mm)以使其厚度为30μm,以190℃、60分钟使其固化。使用产品名称“MCP-T600”(三菱化学株式会社制),通过四端子法对得到的配线测定体积电阻率。
[粘度]
使用E型粘度计(东机工业株式会社制;产品名称:VISCOMETER-TV22;应用锥板型转子:3°×R17.65)测定温度25℃且转速0.5rpm条件下的值。
[触变指数]
使用E型粘度计(东机工业株式会社制;产品名称:VISCOMETER-TV22;应用锥板型转子:3°×R17.65),在温度25℃条件下分别测定转速0.5rpm以及2.5rpm时的粘度,用粘度比(以0.5rpm测定的粘度/以2.5rpm测定的粘度)表示。
[适用期]
测定热固化性树脂组合物放置在25℃的恒温槽内时的粘度增稠至初始粘度的1.5倍以上为止的天数。
[热电阻]
使用热固化性树脂组合物将5mm×5mm的接合面设有金蒸镀层的热电阻用TEG芯片安装于表面镀有Ag的铜基板,以190℃、60分钟进行固化来制作半导体封装。使用明导国际日本公司(Mentor Graphics Japan Co.,Ltd.)制的热电阻测定装置“T3Ster”在室温(25℃)条件下测定所述半导体封装的接合部的热电阻。
[翘曲]
使用热固化性树脂组合物,将8mm×8mm的接合面设有金蒸镀层的背面镀金的硅芯片安装于表面镀有Ag的铜基板,以190℃、60分钟使其固化来制作半导体封装。使用作为测定装置的投影波纹测定装置(ThermoireAXP:美国Akrometrix制),按照电子信息技术工业协会标准的JEITA ED-7306在室温(25℃)条件下测定半导体封装的封装翘曲。具体而言,将测定区域的基板面的全部数据的通过最小二乘法算出的虚拟平面作为基准面,将距离该基准面的垂直方向的最大值为A且最小值为B时的|A|+|B|的值(共面性)作为封装翘曲值。
[冷热循环试验]
使用热固化性树脂组合物,将8mm×8mm的接合面设有金蒸镀层的背面镀金的硅芯片安装于表面镀有Ag的铜框架,进行190℃、60分钟的加热固化(OV固化)。对其进行冷热循环处理(将从-55℃升温至150℃、接着冷却至-55℃的操作作为1个循环,将其循环2000次),通过超声波显微镜(FineSAT II;日立解决方案株式会社(Hitachi Power Solutions Co.,Ltd.)制)观察处理后芯片有无剥离,按照下述基准来评价。
(判定基准)
A:无剥离
C:有剥离
表1
使用了含有(A)银粒子(凝集粒子)的热固化性树脂组合物的实施例1~8均为低粘度且分散性优异。该树脂组合物固化物的热传导率高、翘曲少。另外,使用上述热固化性树脂组合物得到的半导体封装与芯片或基材的接合部的热电阻均小,冷热循环试验后也观察不到芯片的剥离,具有优异的粘接性。因此,通过使用本实施方式的热固化性树脂组合物,能够得到可靠性优异的半导体装置和电气电子部件。
对于使用了含有非凝集体的银粒子的热固化性树脂组合物的比较例1,该树脂组合物的固化物的翘曲小,热传导率良好。但是,相对于银粒子之间的烧结,比较例1的银粒子与芯片或基材的烧结难以进行,因此,与芯片或基材的接合部的热电阻大。另外,银粒子的比表面积小,在接合界面通过树脂粘接,冷热循环试验中的粘接性良好。
对于使用了含有非凝集体的银粒子的热固化性树脂组合物的比较例2和3,该树脂组合物的固化物的翘曲均小。但是,比较例2和3的烧结性差、热传导率低、体积电阻和热电阻高。
对于使用了含有银纳米粒子的热固化性树脂组合物的比较例4和5,与上述实施例的凝集粒子相比,该树脂组合物中含有的保护分子的量多,由于烧结后保护分子挥发,该树脂组合物的固化物的体积收缩变大,因此翘曲大。另外,由于上述树脂组合物中的保护分子的比率多,因此银的绝对量少,虽然烧结性良好,但热传导率与上述凝集粒子相比更低。另外,由于是纳米粒子,所以比表面积大,上述树脂组合物的粘度高,作业性(涂敷性)差。
权利要求书(按照条约第19条的修改)
1.一种热固化性树脂组合物,其中,其含有:(A)银粒子,由平均粒径为0.5~5.0μm的二次粒子构成,所述二次粒子由平均粒径为10~100nm的一次粒子凝集而成;以及(B)热固化性树脂,所述(A)银粒子是粒子内部存在空隙的粒子。
2.如权利要求1所述的热固化性树脂组合物,其中,所述(A)银粒子的振实密度为4.0~7.0g/cm3,且通过BET法求出的比表面积为0.5~1.5m2/g。
3.如权利要求1或2所述的热固化性树脂组合物,其中,所述(A)银粒子的150℃~300℃之间的热膨胀系数为正。
4.如权利要求1~3中任一项所述的热固化性树脂组合物,其中,相对于所述(A)银粒子100质量份,所述(B)热固化性树脂的含量为1~20质量份。
5.如权利要求1~4中任一项所述的热固化性树脂组合物,其中,所述(B)热固化性树脂为从氰酸酯树脂、环氧树脂、丙烯酸树脂以及马来酰亚胺树脂中选出的至少1种。
6.如权利要求1~5中任一项所述的热固化性树脂组合物,其中,还含有(C)稀释剂,相对于所述(A)银粒子100质量份,所述(C)稀释剂的含量为3~20质量份。
7.一种半导体装置,其中,其通过含有权利要求1~6中任一项所述的热固化性树脂组合物的芯片粘接材料将半导体元件和基板粘接而成。
8.一种电气电子部件,其中,其通过含有权利要求1~6中任一项所述的热固化性树脂组合物的散热部件粘接用材料将散热部件和发热部件粘接而成。
9.一种银粒子的制造方法,其中,所述银粒子由平均粒径为0.5~5.0μm的二次粒子构成,所述二次粒子由平均粒径为10~100nm的一次粒子凝集而成,所述制造方法具有:在含有银化合物的水溶液中添加氨水而得到银氨络合物溶液的工序;以及用还原性化合物将所述工序中得到的银氨络合物溶液中的银氨络合物进行还原,得到含银粒子的浆料的工序。
10.如权利要求9所述的银粒子的制造方法,其中,在所述得到银氨络合物溶液的工序中,相对于含有银化合物的水溶液中的每1mol银,氨水的添加量为2~50mol。
11.如权利要求9或10所述的银粒子的制造方法,其中,在所述得到含银粒子的浆料的工序中,相对于银氨络合物中的每1mol银,还原性化合物的含量为0.25~20.0mol,银氨络合物溶液的温度为小于30℃。
12.如权利要求9~11中任一项所述的银粒子的制造方法,其中,所述还原性化合物为肼衍生物。
13.如权利要求9~12中任一项所述的银粒子的制造方法,其中,在所述得到含银粒子的浆料的工序之后,还具有在所述工序中得到的含银粒子的浆料中添加有机保护化合物并将保护基导入所述银粒子的工序。
Claims (13)
1.一种热固化性树脂组合物,其中,其含有:(A)银粒子,由平均粒径为0.5~5.0μm的二次粒子构成,所述二次粒子由平均粒径为10~100nm的一次粒子凝集而成;以及(B)热固化性树脂。
2.如权利要求1所述的热固化性树脂组合物,其中,所述(A)银粒子的振实密度为4.0~7.0g/cm3,且通过BET法求出的比表面积为0.5~1.5m2/g。
3.如权利要求1或2所述的热固化性树脂组合物,其中,所述(A)银粒子的150℃~300℃之间的热膨胀系数为正。
4.如权利要求1~3中任一项所述的热固化性树脂组合物,其中,相对于所述(A)银粒子100质量份,所述(B)热固化性树脂的含量为1~20质量份。
5.如权利要求1~4中任一项所述的热固化性树脂组合物,其中,所述(B)热固化性树脂为从氰酸酯树脂、环氧树脂、丙烯酸树脂以及马来酰亚胺树脂中选出的至少1种。
6.如权利要求1~5中任一项所述的热固化性树脂组合物,其中,还含有(C)稀释剂,相对于所述(A)银粒子100质量份,所述(C)稀释剂的含量为3~20质量份。
7.一种半导体装置,其中,其通过含有权利要求1~6中任一项所述的热固化性树脂组合物的芯片粘接材料将半导体元件和基板粘接而成。
8.一种电气电子部件,其中,其通过含有权利要求1~6中任一项所述的热固化性树脂组合物的散热部件粘接用材料将散热部件和发热部件粘接而成。
9.一种银粒子的制造方法,其中,所述银粒子由平均粒径为0.5~5.0μm的二次粒子构成,所述二次粒子由平均粒径为10~100nm的一次粒子凝集而成,所述制造方法具有:在含有银化合物的水溶液中添加氨水而得到银氨络合物溶液的工序;以及用还原性化合物将所述工序中得到的银氨络合物溶液中的银氨络合物进行还原,得到含银粒子的浆料的工序。
10.如权利要求9所述的银粒子的制造方法,其中,在所述得到银氨络合物溶液的工序中,相对于含有银化合物的水溶液中的每1mol银,氨水的添加量为2~50mol。
11.如权利要求9或10所述的银粒子的制造方法,其中,在所述得到含银粒子的浆料的工序中,相对于银氨络合物中的每1mol银,还原性化合物的含量为0.25~20.0mol,银氨络合物溶液的温度为小于30℃。
12.如权利要求9~11中任一项所述的银粒子的制造方法,其中,所述还原性化合物为肼衍生物。
13.如权利要求9~12中任一项所述的银粒子的制造方法,其中,在所述得到含银粒子的浆料的工序之后,还具有在所述工序中得到的含银粒子的浆料中添加有机保护化合物并将保护基导入所述银粒子的工序。
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JP2014235942A (ja) * | 2013-06-04 | 2014-12-15 | Dowaエレクトロニクス株式会社 | 接合材およびその接合材を用いて電子部品を接合する方法 |
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