CN104641423A - 用于粘合金属的具有助熔剂或还原剂的银烧结组合物 - Google Patents

用于粘合金属的具有助熔剂或还原剂的银烧结组合物 Download PDF

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CN104641423A
CN104641423A CN201380040569.4A CN201380040569A CN104641423A CN 104641423 A CN104641423 A CN 104641423A CN 201380040569 A CN201380040569 A CN 201380040569A CN 104641423 A CN104641423 A CN 104641423A
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H·R·库德
J·G·桑切斯
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Henkel AG and Co KGaA
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Abstract

可烧结的传导性组合物，其包含(i)微米或亚微米尺寸的银片或银粉，以及(ii)助熔剂、或含氧溶剂或过氧化物。所述组合物可用于在不施加压力和≤250℃的烧结温度下将具有银背衬的半导体裸片粘合到铜、银或金引线框。

Description

用于粘合金属的具有助熔剂或还原剂的银烧结组合物
背景技术
包含粘合剂树脂和传导性填料的传导性粘合剂组合物在半导体封装和微电子装置的制造和装配中用以机械地连接集成电路装置和其基材以及在集成电路装置和其基材之间产生导电性和导热性。最常用的传导性填料是银片。在传导性组合物中会使用粘合剂树脂，因为银片通常不能充分地将半导体或微电子装置粘合到其基材。然而，树脂的存在会限制银的高的导热性和导电性。
目前，仅包含银而不包含树脂的传导性组合物在热压粘结下或在无压力粘结下粘合到银或金基材。然而，在电子装置的制造中常用的基材是铜引线框，并且银不容易与铜形成金属间粘结。已经使用焊料，但在高功率和高温的应用中，当在高温或接近其熔融温度的温度下循环时，焊料会失效。此外，焊料需要存在助熔剂，其会在形成金属间粘结后留下助熔剂残余物，因而需要基材的清洁步骤。
有利的是具有不包含粘合剂树脂的银组合物，所述组合物可以烧结并粘合到铜，并且与目前可获得的强度相比，所述组合物可以增加的强度粘合到银和金基材。
发明内容
本发明是一种传导性组合物，其包含(i)微米或亚微米尺寸的银片，以及(ii)助熔剂(fluxing agent)、或含氧溶剂(oxygenated solvent)或过氧化物，其中所述组合物中不包含有机树脂。选择这样的助熔剂、过氧化物或含氧溶剂：在烧结温度下充分挥发，从而在烧结后在组合物中没有残余物剩余。所述组合物在250℃或更低的温度下烧结，并且可以在不施加压力的情况下与铜基材形成金属间粘结。在另一个实施方案中，本发明是一种组件，其包含：银或金的第一基材、烧结组合物以及选自铜、银或金的第二基材的，其中所述烧结组合物包含银片以及含氧溶剂、或过氧化物或助熔剂，并且所述烧结组合物被布置在所述第一基材与所述第二基材之间。
具体实施方式
微米或亚微米尺寸的银片是市售可得的，并且市售银片设有脂肪酸润滑剂和/或表面活性剂的涂层，以防止聚结。银片的制造商使用的典型润滑剂包括硬脂酸、异硬脂酸、月桂酸、癸酸、油酸、棕榈酸，或用胺例如咪唑中和的脂肪酸。润滑剂和/或表面活性剂的去除有助于在传导性组合物中的银片与所选择的金属基材之间形成金属间粘结，并且可以通过使用含氧溶剂或过氧化物实现。
合适的含氧溶剂的实例是酮、酯、二醇醚和醇。这些溶剂由于高溶解能力而被使用，并且用以去除银颗粒和基材表面上的有机物。含氧溶剂包括2-(2-乙氧基-乙氧基)-乙基乙酸酯、丙二醇单乙基醚、丁基乙氧基乙基乙酸酯、二甘醇单丁基醚乙酸酯、二甘醇、二丙二醇、单丁基醚乙酸酯和碳酸亚丙酯。其它合适的溶剂包括环状酮，例如环辛酮、环庚酮和环己酮。如果存在的话，含氧溶剂的量为组合物总量的不超过约15重量％(但不为0％)。
合适的过氧化物的实例包括过氧化-2-乙基己酸叔丁酯、过氧化新癸酸叔丁酯、二月桂酰基过氧化物、过氧辛酸叔丁酯(tertiary-butyl peroctoate)、过氧化-2-乙基己酸1,1,3,3-四甲基丁酯、二叔丁基过氧化物、2,5-双-(叔丁基过氧基)-2,5-二甲基己烷和二枯基过氧化物、二叔戊基过氧化物。如果存在的话，过氧化物的量为组合物总量的0-2.0重量％，优选0.0-1.0重量％。
助熔剂和还原剂(下文中称为助熔剂)被用作化学清洁剂，以从金属薄片或基材的金属表面去除氧化。助熔剂在升高的温度下可以变得具有强还原性，从而防止金属氧化物的形成。助熔剂和还原剂可以用在银粉、银片以及涂覆银的颗粒例如涂覆银的铜和涂覆银的玻璃上。合适的助熔剂的实例包括2,2,6,6-四甲基哌啶氧(2,2,6,6-tetramethylpiperidinoxy)、4,4’-二硫代二丁酸、琥珀酸、8-羟基喹啉、次氨基三甲基膦酸(nitrolotrimethylphosphonicacid)、三乙醇胺、戊二酸、苹果酸、酒石酸、乙酰丙酮、甘油、二硫苏糖醇、1,2,3-三羟基苯。如果存在的话，助熔剂的量为组合物总量的0.0-10.0重量％，优选0.5-5.0重量％。
在室温下制备包含银片以及上述含氧溶剂、过氧化物或助熔剂之一的传导性组合物，将所述组合物沉积在一种基材上，与第二基材接触，然后加热到银的烧结温度以将所述两个基材粘合在一起。
当用于制造半导体时，这些组合物在不使用任何有机树脂的情况下在烧结时具有足够的粘合性，从而将涂覆有金属的晶片(dies)粘合到涂覆有金属的基材。具体地，所述组合物可用于将涂覆有银或金的半导体晶片粘合到铜引线框。在一些实施方案中，本发明的组合物在低于250℃的温度下烧结。在其它实施方案中，本发明的组合物在低于200℃的温度下烧结。诱发烧结不需要压力。在烧结温度下，银片上的润滑剂和/或表面活性剂，以及组合物中所使用的溶剂、过氧化物或助熔剂被烧掉，从而只留下烧结的银。
可以设计各种烧结曲线方案，以适应从业人员的需要。大尺寸晶片可能需要较低的温度和较长时间的烧结曲线，以更缓和地逐渐去除溶剂，从而确保没有空的粘结线。这里给出典型的烧结曲线，但应理解，预期其它类似的烧结曲线同样有效。烧结曲线的实例包括：(i)经30分钟从室温斜坡上升到220℃，然后在220℃保持60分钟；(ii)经15分钟从室温斜坡上升到110℃，然后在110℃保持60分钟，然后在240℃保持60分钟；(iii)经30分钟从室温斜坡上升到250℃，然后在250℃保持60分钟；(iv)对于更高的烧结温度，经60分钟斜坡上升到300℃，然后在300℃保持2小时。在这些烧结曲线下，实现本发明组合物的烧结不需要压力。
在另一个实施方案中，本发明是一种组件，其包含：银或金的第一基材、烧结组合物以及选自铜、银或金的第二基材，其中所述烧结组合物包含银片以及含氧溶剂、或过氧化物或助熔剂，并且所述烧结组合物被置于所述第一基材与所述第二基材之间。
本发明的银粘合剂可用于需要高功率密度的电子工业的组件封装，例如在半导体、汽车、高电压和太阳能电池应用中所使用的那些。
实施例
实施例1.在该实施例中，制备以下样品并遵循测试方案。使用具有助熔剂的组合物以及不具有助熔剂的对照组合物来制备样品。将组合物在小的双离心混合机()中以1000rpm混合60秒，然后以1500rpm混合30秒。所有样品均进行以下烧结：经30分钟从环境温度斜坡上升到250℃并在250℃保持60分钟。未使用压力。
使用Dage 4000系列晶片剪切测试器测量晶片剪切，所述剪切测试器具有能够达到350℃并且实现至少50kg的力的加热器适配垫板。将组合物涂覆到3×3mm2的涂覆有银的晶片上，并使其与半导体工业中典型的裸铜引线框、涂覆有银的铜引线框和涂覆有金的铜引线框接触。按照上述的烧结曲线烧结样品。晶片剪切目标大于或等于1.0Kg/mm2。
体积电阻率使用Agilent 34401A数字万用表或QuadTech 1689 RLCDigibridge测量。测试媒介物是载玻片，其上涂覆有50微米×0.25毫米×25.4毫米的银粘合剂，按照上述的烧结曲线进行烧结。针对有效性和可重复性对至少三个样品测试多次，将结果汇总并取平均值。
导热率使用Holometrix Micro Flash-Laser热性能仪测量。测试样品是0.5mm×12.5mm的自立的(free-standing)银粘合剂圆片，按照上述的烧结曲线进行烧结。针对有效性和可重复性对最少两个样品测试多次，将结果汇总并取平均值。
粘度测量使用具有锥板CP51的Brookfield DV-III在25.0℃进行。在1.92sec-1和19.2sec-1的剪切速率下测量粘度。
DSC用TA仪器Q20以10℃/min从25℃斜坡上升到350℃进行测量。
本发明的样品和对照样品的按重量份(pbw)计的组成以及性能测试的结果列于下表中：
这些结果表明，用含有助熔剂、含氧溶剂和过氧化物的组合物时，在所有引线框上均实现更高的晶片剪切强度。
实施例2.在该实施例中，银烧结组合物不含助熔剂，并且一种组合物不含过氧化物。两个样品均含有含氧溶剂。TNA晶片是涂覆有钛-镍-银的硅晶片。Ag-LF是银引线框。Cu-LF是铜引线框，并且PPF-LF是闪光涂覆有镍-钯-金(金表面)的引线框。RT是室温。如实施例1中所述进行性能测试。数据表明，基本上由银片和含氧溶剂组成的组合物会烧结并且提供对于商业应用而言足够的晶片剪切强度。
实施例3.在该实施例中，如下表中所示制备配制物：一种配制物包含过氧化物和含氧溶剂；一种配制物仅包含含氧溶剂；并且一种配制物仅包含一种助熔剂。除非在表中指出，如实施例1中所述进行性能测试，并且性能测试表明，基本上由银片和助熔剂组成的配制物、或基本上由银片和含氧溶剂组成的配制物会烧结并且提供对于商业应用而言足够的晶片剪切强度。
这些数据表明，不存在过氧化物对具有助熔剂的烧结配制物的性能没有明显影响。
实施例4.在该实施例中，如下表中所示制备配制物：一种配制物包含含氧溶剂；一种配制物仅包含过氧化物；并且一种配制物仅包含一种助熔剂。除非在表中指出，如实施例1中所述进行性能测试，并且所述性能测试表明，基本上由银片和助熔剂组成的配制物、或基本上由银片和含氧溶剂组成的配制物会烧结并且提供对于商业应用而言足够的热性能和电性能以及一定的晶片剪切强度条件。

Claims (8)

1.传导性组合物，其包含(i)微米或亚微米尺寸的银片，以及(ii)助熔剂、或含氧溶剂或过氧化物，其中所述组合物中不包含有机树脂。
2.根据权利要求1所述的传导性组合物，其中存在所述助熔剂，并且所述助熔剂选自2,2,6,6-四甲基哌啶氧、4,4’-二硫代二丁酸、琥珀酸、8-羟基喹啉、次氨基三甲基膦酸、三乙醇胺、戊二酸、苹果酸、酒石酸、乙酰丙酮、甘油、二硫苏糖醇、1,2,3-三羟基苯。
3.根据权利要求2所述的传导性组合物，其中所述助熔剂在所述组合物中的存在量为所述组合物总量的0.1-10.0重量％。
4.根据权利要求1所述的传导性组合物，其中存在所述含氧溶剂，并且所述含氧溶剂选自2-(2-乙氧基-乙氧基)-乙基乙酸酯、丙二醇单乙基醚、二甘醇单丁基醚乙酸酯、二甘醇、二丙二醇、单丁基醚乙酸酯和碳酸亚丙酯。
5.根据权利要求4所述的传导性组合物，其中所述含氧溶剂的存在量为所述组合物总量的0.1-15.0重量％。
6.根据权利要求1所述的传导性组合物，其中存在所述过氧化物，并且所述过氧化物选自过氧化-2-乙基己酸叔丁酯、过氧化新癸酸叔丁酯、二月桂酰基过氧化物、过氧辛酸叔丁酯、过氧化-2-乙基己酸1,1,3,3-四甲基丁酯、二叔丁基过氧化物、2,5-双-(叔丁基过氧基)-2,5-二甲基己烷和二枯基过氧化物、二叔戊基过氧化物。
7.根据权利要求6所述的传导性组合物，其中所述过氧化物的存在量为所述组合物总量的0.0-1.0重量％。
8.组件，其包含：银第一基材、传导性组合物以及选自铜、银或金的第二基材，其中所述传导性组合物包含(i)微米或亚微米尺寸的银片，以及(ii)助熔剂、或含氧溶剂或过氧化物，其中所述组合物中不包含有机树脂，并且所述传导性组合物被置于所述第一基材与所述第二基材之间。
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