CN114269494A - 银粒子、银粒子的制造方法、膏组合物、半导体装置以及电气电子部件 - Google Patents
银粒子、银粒子的制造方法、膏组合物、半导体装置以及电气电子部件 Download PDFInfo
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- CN114269494A CN114269494A CN202080059308.7A CN202080059308A CN114269494A CN 114269494 A CN114269494 A CN 114269494A CN 202080059308 A CN202080059308 A CN 202080059308A CN 114269494 A CN114269494 A CN 114269494A
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- Prior art keywords
- silver
- silver particles
- acid
- particles
- paste composition
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- 239000002245 particle Substances 0.000 title claims abstract description 153
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 129
- 239000004332 silver Substances 0.000 title claims abstract description 129
- 239000000203 mixture Substances 0.000 title claims description 50
- 239000004065 semiconductor Substances 0.000 title claims description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 239000011164 primary particle Substances 0.000 claims abstract description 22
- 150000001875 compounds Chemical class 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 32
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 22
- -1 amine carboxylate salt Chemical class 0.000 claims description 21
- 229940100890 silver compound Drugs 0.000 claims description 14
- 150000003379 silver compounds Chemical class 0.000 claims description 14
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- 230000001681 protective effect Effects 0.000 claims description 9
- 238000006722 reduction reaction Methods 0.000 claims description 8
- 239000007791 liquid phase Substances 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 5
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- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 4
- 150000003973 alkyl amines Chemical class 0.000 claims description 3
- 238000000889 atomisation Methods 0.000 claims description 3
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- 238000004438 BET method Methods 0.000 claims description 2
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- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 description 20
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- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 5
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- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
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Classifications
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- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
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- B22F7/064—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts using an intermediate powder layer
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Abstract
本发明提供银粒子,该银粒子具有:银粉;以及由比该银粉更小的一次粒子构成的银层。
Description
技术领域
本发明涉及银粒子、银粒子的制造方法、糊组合物、半导体装置和电气电子部件。
背景技术
近年来,半导体元件的高效化不断推进,与此相伴,半导体元件的发热量增加、驱动温度提高。另外,接合材料要求高温条件下的可靠性和放热性。作为接合材料的候选,可举出以往一直使用的焊料和银膏,但是由于可靠性和放热性不足因而无法应对,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
即,本发明涉及以下内容。
[1]一种银粒子,其具有:银粉;以及由比该银粉更小的一次粒子构成的银层。
[2]一种银粒子的制造方法,其具有通过液相还原法进一步在(A)银粉的表面形成银层的工序。
[3]一种膏组合物,其含有上述[1]或[2]所述的银粒子。
[4]一种半导体装置,其使用上述[3]所述的膏组合物接合而成。
[5]一种电气电子部件,其使用上述[3]所述的膏组合物接合而成。
具体实施方式
下面,参照一个实施方式详细说明本发明。
需要说明的是,在本发明中,“(甲基)丙烯酸酯”是指丙烯酸酯和/或甲基丙烯酸酯。
<银粒子>
本实施方式的银粒子具有:银粉;以及由比该银粉更小的一次粒子构成的银层。
对构成上述银粒子的母体的银粉没有特别的限定,例如,能够使用通过雾化法、电解法、化学还原法、粉碎法/捣碎法、等离子体旋转电极法、均匀液滴喷雾法、热处理法等公知的方法制备的银粉。从控制粒径以及粒子形状的观点出发,上述银粉也可以为通过雾化法、电解法或化学还原法制备而成的银粉。
另外,也能够使用市售品,具体而言,可举出Ag-HWQ(福田金属箔粉工业株式会社制,D50=1.8μm,球状)、SL01(三井金属矿业株式会社制,D50=1.23μm,不定形状)等。这些可以单独使用,也可以并用2种以上。
上述银粉的平均粒径可以为0.5μm以上且30μm以下,可以为大于0.5μm且20μm以下,也可以为1μm以上且20μm以下。另外,对形状没有特别的限定,可举出球状、板形、薄片状(flake)、鳞片状、树枝状、棒状、线状、不定形状等。
需要说明的是,上述银粉的平均粒径是在使用激光衍射式粒度分布测定装置等测定的粒度分布中累计体积为50%的粒径(50%粒径D50)。
例如,用还原性化合物将银化合物还原,从该银化合物中游离的银的一次粒子凝集而形成上述银层。
作为上述银化合物,可以为从硝酸银、氯化银、乙酸银、草酸银以及氧化银中选出的至少1种,从水中的溶解度的观点出发,也可以为硝酸银、乙酸银。
只要上述还原性化合物具有将银化合物还原并使银析出的还原力,就没有特别限定。
作为上述还原性化合物,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。
上述一次粒子的平均粒径可以为10~100nm,可以为10~50nm,也可以为20~50nm。上述一次粒子的平均粒径为10nm以上时,比表面积不会过大,能够提高膏的作业性,平均粒径为100nm以下时,烧结性良好。
上述一次粒子的平均粒径能够通过对用场发射型扫描电子显微镜(FE-SEM)来观察利用聚焦离子束(FIB)装置切断的球状银粒子的截面而测定的200个银粒子的粒径进行个数平均来求出。具体而言,能够通过实施例中记载的方法进行测定。
上述银粒子的平均粒径可以为0.5~5.0μm,可以为0.5~3.0μm,也可以为1.0~3.0μm。上述银粒子的平均粒径为0.5μm以上时,保存稳定性良好,平均粒径为5.0μm以下时,烧结性良好。
上述银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。
上述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,能够在膏中填充大量银粒子,振实密度为7.0g/cm3以下时,能够降低银粒子在膏中的沉降。
上述银粒子的振实密度能够使用振实密度测定器进行测定,具体而言,能够通过实施例中记载的方法进行测定。
上述银粒子的通过BET法求出的比表面积可以为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,上述银粒子的比表面积为1.5m2/g以下时,能够使膏低粘度化.
能够使用比表面积测定装置并通过基于氮吸附的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。
<银粒子的制造方法>
本实施方式的银粒子的制造方法具有:通过液相还原法在(A)银粉的表面进一步形成银层的工序(以下,简称为银层形成工序)。
在银层形成工序中,在液相中混合(A)银粉、(B)银化合物以及(C)还原性化合物。
(A)银粉、(B)银化合物以及(C)还原性化合物能够分别使用上述<银粒子>项目中说明的物质。
从络合物的稳定性的观点出发,上述(B)银化合物也可以为银氨络合物溶液。
对银氨络合物溶液没有特别限定。通常,通过将银化合物溶解在氨水中得到(例如,参照日本特开2014-181399号公报),但也可以在银化合物中加入胺化合物后,使其溶解在醇中来制备。
相对于含有(B)银化合物的水溶液中的每1mol银,上述氨的添加量可以为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,能够将从银化合物中游离的银的一次粒子的平均粒径设为上述范围内。
利用(C)还原性化合物将上述银氨络合物溶液中的银氨络合物还原,得到含银粒子的浆料。
通过利用(C)还原性化合物将银氨络合物还原,使银从银氨络合物中游离,在(A)银粉的周围形成该银的一次粒子凝集而成的二次粒子,形成本实施方式的银粒子。
通过适当调整银氨络合物中的银量、(C)还原性化合物的含量以及添加的(A)银粉的平均粒径,能够控制上述一次粒子的凝集,能够将得到的二次粒子(银粒子)的平均粒径设为上述范围内。
相对于银氨络合物中的每1mol银,(C)还原性化合物的含量可以为0.25~20mol,可以为0.25~10mol,也可以为1.0~5.0mol。
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。
通过在如上所述得到的含银粒子的浆料中进一步添加(D)有机保护化合物,能够将保护基导入上述含银粒子的浆料中的银粒子。
作为(D)有机保护化合物,例如,可举出羧酸、烷基胺、羧酸胺盐、酰胺等。从粒子的稳定性的观点出发,(D)有机保护化合物可以为从羧酸、烷基胺以及羧酸胺盐中选出的至少1种,从提高分散性的观点出发,也可以为羧酸。
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。这些可以单独使用,也可以并用2种以上。
相对于1mol银粒子,(D)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。
(混合物的形成)
在反应容器中混合(A)银粉、(B)银化合物以及(C)还原性化合物,进一步根据需要混合(D)有机保护化合物。对这些化合物的混合的顺序没有特别的限定,可以按照任何顺序将上述化合物混合。
通过本实施方式的银粒子的制造方法而得到的银粒子为纳米尺寸的银的一次粒子在银粉的表面凝集而成的二次粒子,从而维持上述银的一次粒子表面具有的高活性,在低温条件下具有二次粒子之间的烧结性(自烧结性)。另外,银粒子之间的烧结和银粒子以及接合部件的烧结同时进行。因此,通过使用上述银粒子,能够得到热传导性以及粘接特性优异的膏组合物。
<膏组合物>
本实施方式的膏组合物包含上述银粒子。因此,本实施方式的膏组合物为低粘度且分散性良好,能够得到粘接特性以及热传导性优异,且体积收缩小且低应力性优异的固化物。本实施方式的膏组合物能够作为元件粘接用芯片粘接材料、放热部件粘接用材料等使用。
本实施方式的膏组合物通过包含热固化性树脂,能够形成具有适度的粘度的粘接材料(膏)。
只要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。作为氰酸酯树脂,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,为使作为膏组合物在室温(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。上述固化促进剂例如可以为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。
相对于银粒子100质量份,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。热固化性树脂为1质量份以上时,能够充分得到热固化性树脂带来的粘接性,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,能够提高放热性。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。
从作业性的观点出发,本实施方式的膏组合物还可以含有稀释剂。作为稀释剂,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。
在本实施方式的膏组合物含有稀释剂时,相对于银粒子100质量份,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。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,稀释剂的含量为20质量份以下时,能够控制本实施方式的膏组合物固化时的空隙的产生。
本实施方式的膏组合物除了以上的各成分以外,根据需要也能够含有通常配合在这种组合物中的固化促进剂;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;聚合引发剂;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。
本实施方式的膏组合物能够通过将上述银粒子、根据需要含有的热固化性树脂、稀释剂和各种添加剂充分混合后,进一步通过分散机、捏合机、三辊研磨机等进行混炼处理,然后进行脱泡来制备。
本实施方式的膏组合物的固化物的热传导率可以为35W/m·K以上,也可以为40W/m·K以上。
上述热传导率能够通过实施例中记载的方法测定。
本实施方式的膏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。
<半导体装置以及电气电子部件>
本实施方式的半导体装置以及电气电子部件使用上述膏组合物接合而成,因此可靠性优异。
本实施方式的半导体装置是使用上述膏组合物将半导体元件粘接在作为元件支撑部件的基板上而成。即,此处,膏组合物作为芯片粘接材料使用,通过该芯片粘接材料将半导体元件和基板粘接并固定。
此处,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。
通过使用上述芯片粘接材料,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。
另外,本实施方式的电气电子部件使用上述膏组合物将放热部件粘接于发热部件而成。即,此处,膏组合物作为放热部件粘接用材料使用,通过该膏组合物将放热部件和发热部件粘接并固定。
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,作为放热部件,可举出放热器(heat sink)、散热器(heat spreader)等。
如上所述,通过使用上述放热部件粘接用材料将放热部件粘接于发热部件,能够通过放热部件将发热部件所产生的热高效地释放到外部,能够抑制发热部件的温度上升。此外,发热部件和放热部件可以通过放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的任何限定。
(银粒子的制造)
[合成例1]
将40g的硝酸银(东洋化学工业株式会社制)溶解在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。将银粉(产品名称:Ag-HWQ 1.5μm;福田金属箔粉工业株式会社制;平均粒径:1.8μm)50g投入到该水溶液中,制成银粉分散的银氨络合物水溶液。将其设为液温10℃,一边搅拌一边用60秒滴加20质量%的肼一水合物水溶液(林纯药工业株式会社制)28mL,使银在银粉的表面析出,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(东京化成工业株式会社制),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,得到银粒子1。
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1的截面,确认了该银粒子1为银在银粉的周围凝集并在该银粉的表面形成有银层。另外,形成银层的银的一次粒子的平均粒径为20nm,该一次粒子凝集而成的二次粒子的平均粒径为1.9μm,得到的银粒子1的振实密度为5.7g/cm3,比表面积为1.0m2/g。
[合成例2]
将40g的硝酸银(东洋化学工业株式会社制)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。将银粉(产品名称:AgS1.0;德力本店株式会社制;平均粒径:1.59μm)50g投入到该水溶液中,制成银粉分散的银氨络合物水溶液。将其设为液温10℃,一边搅拌一边用60秒滴加20质量%的肼一水合物水溶液(林纯药工业株式会社制)28mL,使银在银粉的表面析出,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(东京化成工业株式会社制),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,得到银粒子2。
[合成例3]
将40g的硝酸银(东洋化学工业株式会社制)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。将银粉(产品名称:AgS2.0;德力本店株式会社制;平均粒径:2.45μm)50g投入到该水溶液中,制成银粉分散的银氨络合物水溶液。将其设为液温10℃,一边搅拌一边用60秒滴加20质量%的肼一水合物水溶液(林纯药工业株式会社制)28mL,使银在银粉的表面析出,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(东京化成工业株式会社制),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,得到银粒子3。
[合成例4]
将40g的硝酸银(东洋化学工业株式会社制)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。将银粉(产品名称:AgS1.0;德力本店株式会社制;平均粒径:1.59μm)50g投入到该水溶液中,制成银粉分散的银氨络合物水溶液。将其设为液温10℃,一边搅拌一边用60秒滴加20质量%的肼一水合物水溶液(林纯药工业株式会社制)20mL,使银在银粉的表面析出,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(东京化成工业株式会社制),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,得到银粒子4。
用下述的方法对合成例1~4中得到的银粒子1~4进行评价。将其结果示于表1。
[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小时在真空环境下干燥得到银粒子,使用该银粒子进行一次粒子的平均粒径的测定。
对通过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)观察利用聚焦离子束(FIB)装置(日本电子株式会社(JEOL社)制的JEM-9310FIB)切断的球状银粒子的截面而测定的200个银粒子的粒径进行个数平均,从而求出一次粒子的平均粒径。
[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),来求出二次粒子的平均粒径。
[振实密度]
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。
表1
合成例1 | 合成例2 | 合成例3 | 合成例4 | |
银粒子1 | 银粒子2 | 银粒子3 | 银粒子4 | |
一次粒子的平均粒径[nm] | 20 | 20 | 20 | 30 |
二次粒子的平均粒径[μm] | 1.9 | 2.2 | 2.7 | 2.0 |
振实密度[g/cm<sup>3</sup>] | 5.7 | 5.0 | 5.51 | 5.25 |
比表面积[m<sup>2</sup>/g] | 1.0 | 1.2 | 0.8 | 0.9 |
[实施例1~9、比较例1~4]
按照表2的配比将各成分混合,用三辊磨机进行混炼,得到膏组合物。用后述的方法对得到的膏组合物进行评价。将其结果示于表2。需要说明的是,在表2中,空栏表示未配合。
实施例和比较例中使用的表2中记载的各材料如下所示。
[银粒子X]
·(银粒子1):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:1.9μm)
·(银粒子2):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:2.2μm)
·(银粒子3):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:2.7μm)
·(银粒子4):合成例4中得到的银粒子(一次粒子的平均粒径:30nm;二次粒子的平均粒径:2.0μm)
[通过除本实施方式的银粒子的制造方法以外的制造方法得到的银粒子(银粒子Y)]
·TC-505C(德力本店株式会社制;商品名;平均粒径:1.93μm;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;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;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)
·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)
[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 Chemicals Corporation)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)
[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膏组合物的固化物的热传导率。
[体积电阻率]
通过丝网印刷法将膏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)来测定温度为25℃且转速为0.5rpm条件下的值。
[适用期]
测定膏组合物放置在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。
[翘曲]
在室温(25℃)条件下测定半导体封装的封装翘曲,该半导体封装是使用膏组合物将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,并以190℃、60分钟进行固化来制作的。测定装置使用投影波纹测定装置(ThermoireAXP:美国Akrometrix制),按照电子信息技术工业协会标准的JEITA ED-7306进行测定。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设为A且最小值设为B时的|A|+|B|的值(共面性)作为封装翘曲值。
[冷热循环试验]
使用膏组合物,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,制备半导体封装。对该半导体封装进行冷热循环处理(将从-55℃升温至150℃、然后冷却至-55℃的操作设为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 PowerSolutions Co.,Ltd.)制)观察处理后芯片有无剥离,按照下述基准进行评价。
(判定基准)
A:无剥离
C:有剥离
表2
使用了含有本发明的银粒子的膏组合物的实施例1~9均为低粘度且分散性优异。可知该膏组合物的固化物的热传导率高且翘曲少。另外,可知使用上述膏组合物得到的半导体封装均在冷热循环试验后未观察到芯片的剥离,具有优异的粘接性。
Claims (11)
1.一种银粒子,其中,其具有:银粉;以及由比该银粉更小的一次粒子构成的银层。
2.如权利要求1所述的银粒子,其中,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。
3.一种银粒子的制造方法,其中,其具有通过液相还原法进一步在(A)银粉的表面形成银层的工序。
4.如权利要求3所述的银粒子的制造方法,其中,在所述工序中,在液相中将(A)银粉、(B)银化合物以及(C)还原性化合物混合。
5.如权利要求3或4所述的银粒子的制造方法,其中,所述(A)银粉通过雾化法、电解法或化学还原法来制备。
6.如权利要求4或5所述的银粒子的制造方法,其中,所述(B)银化合物为从硝酸银、氯化银、乙酸银、草酸银以及氧化银中选出的至少1种。
7.如权利要求3~6中任一项所述的银粒子的制造方法,其中,在所述工序中,进一步添加(D)有机保护化合物。
8.如权利要求7所述的银粒子的制造方法,其中,所述(D)有机保护化合物为从羧酸、烷基胺以及羧酸胺盐中选出的至少1种。
9.一种膏组合物,其中,其含有权利要求1或2所述的银粒子。
10.一种半导体装置,其中,其使用权利要求9所述的膏组合物接合而成。
11.一种电气电子部件,其中,其使用权利要求9所述的膏组合物接合而成。
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2005146408A (ja) * | 2003-10-22 | 2005-06-09 | Mitsui Mining & Smelting Co Ltd | 微粒銀粒子付着銀粉及びその微粒銀粒子付着銀粉の製造方法 |
CN101106048A (zh) * | 2006-06-28 | 2008-01-16 | 东丽株式会社 | 荧光体浆料及显示器的制造方法 |
TW201623638A (zh) * | 2014-12-19 | 2016-07-01 | 普蘭特太陽能光電公司 | 基於銀奈米粒子之複合太陽能金屬化漿料 |
Family Cites Families (11)
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JP2004107728A (ja) * | 2002-09-18 | 2004-04-08 | Ebara Corp | 接合材料及び接合方法 |
KR100719993B1 (ko) * | 2003-09-26 | 2007-05-21 | 히다치 가세고교 가부시끼가이샤 | 혼합 도전 분말 및 그의 이용 |
JP4674375B2 (ja) * | 2005-08-01 | 2011-04-20 | Dowaエレクトロニクス株式会社 | 銀粒子粉末の製造法 |
JP4624222B2 (ja) * | 2005-09-13 | 2011-02-02 | 戸田工業株式会社 | 導電部形成用粒子 |
JP5164239B2 (ja) * | 2006-09-26 | 2013-03-21 | Dowaエレクトロニクス株式会社 | 銀粒子粉末、その分散液および銀焼成膜の製造法 |
JP6001861B2 (ja) | 2012-01-11 | 2016-10-05 | 株式会社ダイセル | 銀ナノ粒子の製造方法及び銀ナノ粒子、並びに銀塗料組成物 |
JP5785532B2 (ja) * | 2012-11-30 | 2015-09-30 | 三井金属鉱業株式会社 | 銀コート銅粉及びその製造方法 |
JP6011803B2 (ja) | 2013-03-21 | 2016-10-19 | 住友金属鉱山株式会社 | 銀粒子の製造方法 |
JP6389091B2 (ja) * | 2013-10-01 | 2018-09-12 | Dowaエレクトロニクス株式会社 | 銀被覆銅粉及びその製造方法、並びに導電性ペースト |
JP6442240B2 (ja) * | 2014-11-14 | 2018-12-19 | 三菱マテリアル電子化成株式会社 | 銀被覆粒子及びその製造方法 |
EP3758048B1 (en) * | 2015-10-02 | 2022-11-09 | Mitsui Mining & Smelting Co., Ltd. | A bonding junction structure |
-
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2005146408A (ja) * | 2003-10-22 | 2005-06-09 | Mitsui Mining & Smelting Co Ltd | 微粒銀粒子付着銀粉及びその微粒銀粒子付着銀粉の製造方法 |
CN101106048A (zh) * | 2006-06-28 | 2008-01-16 | 东丽株式会社 | 荧光体浆料及显示器的制造方法 |
TW201623638A (zh) * | 2014-12-19 | 2016-07-01 | 普蘭特太陽能光電公司 | 基於銀奈米粒子之複合太陽能金屬化漿料 |
Non-Patent Citations (2)
Title |
---|
杨洪霞;黄立达;朱敏蔚;蔡依群;: "银粉及银导电浆料制备技术的研究进展", 电子元件与材料, no. 10, 26 October 2018 (2018-10-26), pages 5 - 11 * |
鲁志强;甘卫平;黎应芬;周健;杨超;戈田田;: "化学还原法制备微纳米银粉", 粉末冶金材料科学与工程, no. 02, 15 April 2015 (2015-04-15), pages 50 - 56 * |
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