CN102604559A - 连接材料和半导体装置 - Google Patents
连接材料和半导体装置 Download PDFInfo
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- CN102604559A CN102604559A CN2012100164892A CN201210016489A CN102604559A CN 102604559 A CN102604559 A CN 102604559A CN 2012100164892 A CN2012100164892 A CN 2012100164892A CN 201210016489 A CN201210016489 A CN 201210016489A CN 102604559 A CN102604559 A CN 102604559A
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Images
Classifications
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- H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
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- C—CHEMISTRY; METALLURGY
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Abstract
本发明涉及连接材料和半导体装置,本发明提供的连接材料,其特征在于,其是含有粘合剂(A)、填料(B)以及添加剂(C)的连接材料,把所述填料(B)和所述添加剂(C)按照与所述连接材料中的重量比相同的重量比来进行混合、加热成型而得到的成型体的热导率为40W/mK以上。
Description
本发明是申请号为2009801151612(国际申请号为PCT/JP2009/058375)、申请日为2009年4月28日、发明名称为“连接材料和半导体装置”的发明申请的分案申请。
技术领域
本发明涉及一种导热性和粘接性优异的连接材料以及使用它的半导体装置。更详细地,涉及一种非常适合用于把IC、LSI、发光二极管(LED)等半导体元件粘接于引线框(lead frame)、陶瓷配线板、玻璃环氧树脂配线板、聚酰亚胺配线板等基板上的连接材料以及使用它的半导体装置。
背景技术
作为在制造半导体装置的时候、使半导体元件和引线框(支撑部件)连接的方法,有使银粉等填充剂分散于环氧系树脂、聚酰亚胺系树脂等树脂中形成糊状(例如,银糊)、将其作为粘接剂来使用的方法。
根据该方法,使用分散机、印刷机、压印机等,在把糊状粘接剂涂布于引线框的芯片焊垫(die pad)之后,把半导体元件芯片焊接(die bonding),通过加热固化来粘接而形成半导体装置。
该半导体装置进一步通过封固材料封固外部、进行半导体封装之后,在配线基板上进行钎焊来实施安装。最近的安装,因为要求高密度以及高效率,所以对于焊锡安装来说,把半导体装置的引线框直接钎焊在基板上的表面安装法是主流。
在该表面安装中,使用通过红外线等来加热整个基板的回流焊接,封装被加热到200℃以上的高温。此时,如果在封装的内部,特别是在粘接剂层中有水分存在时,该水分会气化而返回至芯片焊垫和封固材料之间,在封装中引起开裂(回流开裂)。
由于该回流开裂使半导体装置的可靠性显著降低,所以一直是深刻的问题和技术课题,对于在半导体元件和半导体支撑部件之间的粘接中经常使用的粘接剂,首先要求的是高温时的粘接强度的可靠性。
另外,近年来,伴随着半导体元件的高速化、高集成化的发展,除了以前所要求的粘接强度等的可靠性之外,为了确保半导体装置的动作稳定性,还要求高放热特性。即,为了解决上述技术课题,寻求一种用于接合放热部件(引线框)和半导体元件的粘接剂的连接材料,其兼备高粘接强度和高导热性。
另外,以前的导电性粘接剂中金属粒子彼此接触,作为实现放热性比该以前的导电性粘接剂高的手段之一,有人提出了使用烧结性优异的平均粒径为0.1μm以下的金属纳米粒子,使金属微粒在200℃以下的高温下烧结的那样的导电性粘接剂。上述现有技术记载于例如专利文献1~5。
以前,作为确保粘接剂的高导热性的方法,采取的方法是高填充热导率高的银粒子。另外也有的例子是:通过使用低熔点金属、用金属结合使得热导通路形成以及与粘附体金属化,确保高热传导化以及室温下的强度。进一步地,使用金属纳米粒子的导电性粘接剂的研究也正在进行。
先前技术文献
专利文献
专利文献1:日本特开2006-073811号公报
专利文献2:日本特开2006-302834号公报
专利文献3:日本特开2005-093996号公报
专利文献4:日本特开平11-066953号公报
专利文献5:日本特开2006-083377号公报
发明内容
发明所要解决的课题
但是,就以前的高填充热导率高的银粒子的方法而言,为了确保近年来的电源IC(power IC)、LED中所需要的20W/m·K以上的热导率,就需要非常大量的银粒子(银粒子的填充量为95重量份以上)。
在银粒子填充量变多的情况下,由于粘度上升,产生的问题是:分配时产生拉丝等、难以确保操作性;在为了确保操作性而大量添加溶剂的情况下,产生的问题是:产生空隙或者残留溶剂引起粘接强度的降低。
另外,关于使用低熔点金属、通过金属结合形成热导通路以及与粘附体金属化的方法而言,在把电源IC或者LED等PKG安装在基板上的情况下,在回流炉内暴露于260℃,存在的问题是:由于该热历程,使得接合部再熔融、不能够得到连接可靠性。
进一步地,关于使用金属纳米粒子的方法而言,虽然可以避免接合部的再熔融的问题,但是存在的问题是:为了制作纳米尺寸的金属粒子需要花费很多的成本;为了得到金属纳米粒子的分散稳定性需要大量的表面保护材料,为了烧结金属纳米粒子必须施加200℃以上的高温、载荷等。
因此,本发明的目的是提供一种即使在不施加载荷并且200℃以下的固化温度下进行接合的情况下,也具有高的热导率,而且即使在260℃对固化物进行加热的情况下,也具有充分的粘接强度的连接材料以及使用它的半导体装置。
解决问题的手段
鉴于上述情况,本发明提供一种连接材料,其含有金属粒子,所述金属粒子用X射线光电子能谱法测定的氧的状态比率为小于15%。根据该连接材料,即使在不施加载荷并且200℃以下的固化温度下进行接合的情况下,也具有高的热导率,而且即使在260℃对固化物进行加热的情况下,也具有充分的粘接强度。
优选地,上述金属粒子是:实施了除去其表面的氧化膜的处理以及实施了利用表面保护材料的表面处理的金属粒子。
优选地,上述金属粒子的平均粒径为0.1μm~50μm;另外,优选为在200℃以下烧结的金属粒子。
优选地,本发明的连接材料进一步含有挥发性成分和粘合剂成分。
另外,本发明提供一种连接材料,其是含有粘合剂(A)、填料(B)以及添加剂(C)的连接材料,把填料(B)和添加剂(C)按照与在连接材料中的重量比相同的重量比来进行混合、加热成型而得到的成型体的热导率为40W/m·K以上。根据该连接材料,能够具有操作性优异的粘度、维持粘接强度并且实现热导率的提高。
另外,上述“加热成型”是指,在成型为规定的大小之后在180℃下加热处理1小时;另外上述“热导率”是指,通过在实施例中记载的方法进行测定所得到的热导率。
优选地,上述添加剂(C)的含有量相对于100重量份的粘合剂(A)为1~100重量份。
另外,本发明还提供一种半导体装置,其具有的结构是:通过上述本发明的连接材料,半导体元件和半导体元件搭载用支撑部件被连接在一起。
发明效果
根据本发明,能够提供一种即使在不施加载荷并且200℃以下的固化温度下进行接合的情况下,也具有高的热导率,而且即使在260℃对固化物进行加热的情况下,也具有充分的粘接强度的连接材料以及使用它的半导体装置。这样的连接材料非常适合用作导电性连接材料、导热性粘接剂或者芯片焊接材料。
附图说明
图1是对表面的氧化膜少的金属粒子实施了利用表面保护材料的表面处理的金属粒子的示意图;
图2是表示图1所示的金属粒子的表面保护材料脱离、金属粒子彼此烧结后的状态的示意图;
图3是对表面的氧化膜多的金属粒子实施了利用表面保护材料的表面处理的金属粒子的示意图;
图4是表示:虽然图3所示的金属粒子的表面保护材料脱离、但是金属粒子彼此不能够烧结的状态的示意图;
图5是对氧化膜多的金属粒子实施了除去表面的氧化膜的处理以及实施了利用表面保护材料的表面处理的金属粒子的示意图;
图6是表示图5所示的金属粒子的表面保护材料脱离、金属粒子彼此烧结后的状态的示意图;
图7是表示本发明的半导体装置的一例的截面示意图;
图8是表示本发明的半导体装置的另一例的截面示意图。
具体实施方式
本发明的连接材料是含有用X射线光电子能谱法测定的氧的状态比率为小于15%的金属粒子的连接材料。
在上述金属粒子中,氧的状态比率优选为小于10%,更优选为小于5%。
作为X射线光电子能谱法的分析装置,可以使用例如Surface ScienceInstrument公司的S-Probe ESCA Model 2803,把AlKα射线用于照射X射线。所谓“状态比率”是测定样品中的特定元素的浓度,用根据元素的强度通过使用装置附属的相对灵敏度系数算出的值来表示。另外,用X射线光电子能谱法测定的金属粒子的氧的状态比率,作为金属粒子表面上的氧化膜的量的指标。
作为上述金属粒子,可以使用各种公知的金属粒子。可以举出例如:金、铂、银、铜、镍、钯、铁、铝等导电性的粉体等,另外,这些金属粒子可以单独使用或者组合使用两种以上。其中,从价格、导电性以及导热性等方面考虑,银和铜是特别优选的。
就上述金属粒子而言,平均粒径优选为0.1μm~50μm。如果是小于0.1μm的粒子,则制造上的成本有变大的倾向;对于超过50μm的粒子而言,具有的倾向是:粒子间的空隙大、热导率下降
对于上述金属粒子而言,优选为:实施了除去其表面的氧化膜的处理以及实施了利用表面保护材料的表面处理的金属粒子。
通过使用这样的金属粒子,能够得到上述本发明的效果,其理由还未必清楚,下面根据图1~6的示意图来说明本发明人们的研究。
首先,在对表面的氧化膜少的金属粒子实施了利用表面保护材料的表面处理的情况下,认为是图1中所示的那样的状态。即,认为状态是:在本体金属3上存在有少许残留的氧化膜2,并且除了氧化膜2之外,表面保护材料1覆盖着本体金属3。
在这种情况下,通过在200℃以下加热,如图2所示的那样,因为表面保护材料1脱离、活性的本体金属3的表面露出,所以该活性表面与其他金属粒子的活性表面接触,由此烧结得到促进,从而形成由金属粒子彼此之间的金属结合而成的通路。认为含有这样的金属粒子的连接材料,即使在200℃以下加热的情况下,也具有高的热导率。
另一方面,在如图3所示的那样的氧化膜2多的金属粒子的情况下,认为:在200℃以下加热时,虽然如图4所示,表面保护材料1脱离,但是由于金属粒子的表面被氧化膜2广泛地覆盖着,所以金属粒子之间难以发生烧结。
与此相对,即使在使用氧化膜2多的金属粒子的情况下,如果实施了除去表面的氧化膜2的处理以及实施了利用表面保护材料的表面处理,则如图5所示,得到的金属粒子的状态是:氧化膜2不存在,本体金属3的全部表面被表面保护材料4覆盖。
在这种情况下,与如图1所示的金属粒子一样,通过在200℃以下加热,表面保护材料4脱离,活性的本体金属3的表面露出,因此,该活性表面和其他金属粒子的活性表面相接触,由此烧结被促进,形成由金属粒子彼此之间的金属结合而成的通路。此时,与图1的金属粒子相比,因为活性的本体金属3的表面露出的面积更大,所以认为更加促进了烧结,认为得到了更高的热导率。
进一步地,本发明人等还确立了:降低或者完全除去金属粒子的氧化膜的量、防止金属粒子的再氧化以及凝集的金属粒子表面处理法。以下表示该方法。
首先,在溶解、分散有表面保护材料的酸性溶液中添加金属粒子、搅拌的同时除去氧化膜并施行表面保护。
其次,过滤该溶液,分离出金属粒子之后,用溶剂洗涤在金属粒子表面上物理吸附的表面保护材料和酸成分。其后,通过对金属粒子减压干燥而除去剩余的溶剂,得到干燥状态的进行过表面处理的金属粒子。
另外,在氧化膜除去的工艺中,在不含有表面保护材料的酸性溶液中进行氧化膜处理时,有可能金属粒子彼此凝集、得不到具有与氧化膜处理前的粒子同等的平均粒径的粉体状金属粒子。为了防止金属粒子的凝集,优选在酸性溶液中添加表面保护材料,同时进行氧化膜除去和表面处理。
酸性溶液没有限制,作为酸,可以使用硫酸、硝酸、盐酸、乙酸、磷酸等。酸的稀释溶剂也没有限制,优选与酸的相容性良好的、而且表面保护材料的溶解性、分散性优异的溶剂。
对于酸性溶液的酸的浓度而言,为了除去氧化膜,当把酸性溶液全体作为100重量份时,优选为1重量份以上,在含有氧化膜厚的金属粒子的情况下,更加优选为5重量份以上。
另外,如果酸的浓度过浓,则金属会大量地溶解在溶液中,因此,优选为50重量份以下,为了防止粒子彼此的凝集,更优选为40重量份以下。
表面保护材料优选具有对金属表面的吸附良好的末端官能团的化合物。例如,可举出具有羟基、羧基、氨基、硫醇基、二硫基的化合物,优选具有硫醇基的化合物。通过使用这些表面保护材料,可以防止再氧化和粒子的凝集。
另外,为了进一步高度防止金属粒子的再氧化和剩余有机物的吸附污染,优选化合物的主骨架具有能够使保护材料被紧密地填充的直链烷烃骨架。
对于烷烃骨架而言,进一步优选碳原子数为4个以上,以使得通过碳链彼此的分子间力来紧密地填充。
另外,为了在200℃以下的低温下使金属粒子烧结,更加优选表面保护材料从金属表面脱离的温度比200℃低的、碳原子数18个以下的烷烃骨架。
作为具有硫醇基、并且主骨架是直链烷烃骨架的化合物,可以举出例如:含有1~18个碳原子的乙硫醇、正丙硫醇、异丙硫醇、正丁硫醇、异丁硫醇、叔丁硫醇、戊硫醇、己硫醇、十二烷基硫醇、十八烷基硫醇这样的硫醇或者环烷基硫醇,所述环烷基硫醇可举出含有5~7个碳原子的环戊硫醇、环己硫醇、或者环庚硫醇那样的硫醇。
对于酸性溶液中的表面保护材料的浓度而言,当把酸性溶液全体作为100重量份时,为了防止金属粒子彼此的凝集,优选为0.0001重量份以上,为了防止表面保护材料对金属粒子的过度物理吸附,优选为0.1重量份以下。
对于上述金属粒子在连接材料中的比例而言,当把连接材料全体作为100重量份时,为了提高热导率,优选为80重量份以上;为了达到与高温焊锡同等或者更高的热导率,更加优选为87重量份以上。
另外,为了把连接材料做成糊状,当把连接材料的全体作为100重量份时,金属粒子的比例优选为99重量份以下,为了提高使用分散机、印刷机的操作性,更加优选为95重量份以下。
作为本发明中使用的挥发性成分,在对与金属粒子的混合物施加规定的热历程时,只要金属粒子能够烧结就没有特别的限制。
作为挥发性成分的一例,可以举出:乙二醇丁基醚、乙二醇苯基醚、二乙二醇甲基醚、二乙二醇乙基醚、二乙二醇丁基醚、二乙二醇异丁基醚、二乙二醇己基醚、三乙二醇甲基醚、二乙二醇二甲基醚、二乙二醇二乙基醚、二乙二醇二丁基醚、二乙二醇丁基甲基醚、二乙二醇异丙基甲基醚、三乙二醇二甲基醚、三乙二醇丁基甲基醚、乙二醇乙基醚乙酸酯、乙二醇丁基醚乙酸酯、二乙二醇乙基醚乙酸酯、二乙二醇丁基醚乙酸酯、丙二醇丙基醚、二丙二醇甲基醚、二丙二醇乙基醚、二丙二醇丙基醚、二丙二醇丁基醚、二丙二醇二甲基醚、三丙二醇甲基醚、三丙二醇二甲基醚、二丙二醇甲基醚乙酸酯、3-甲基-3-甲氧基丁醇、乳酸乙酯、乳酸丁酯、γ-丁内酯、α-萜品醇、异佛尔酮、对聚伞花素、1,3-二甲基-2-咪唑啉酮、茴香醚、二甲基亚砜、六甲基磷酰胺、间甲酚、邻氯代苯酚、乙二醇乙醚醋酸酯(cellosolve acetate)、N-甲基-2-吡咯烷酮、N,N-二甲基乙酰胺、N,N-二甲基甲酰胺、环丁砜、四氢呋喃、二噁烷、单乙二醇二甲基醚(monoglyme)、二乙二醇二甲基醚(diglyme)、苯、甲苯、二甲苯、甲基乙基酮、甲基溶纤剂、乙二醇乙醚醋酸酯(cellosolve acetate)、环己酮等。
上述的挥发性成分,可以使用1种或者根据需要混合使用2种以上的成分。为了提高导热性,当把连接材料的全体作为100重量份时,挥发性成分的含有量优选为20重量份以下。
在本发明中使用的粘合剂成分(粘合剂(A)),包含有机高分子化合物或者其前驱体,根据需要还可以含有以下物质中的一种以上:反应性稀释剂、固化剂、用于提高固化性的固化促进剂、用于缓和应力的增韧剂(可撓剤)、用于提高操作性的稀释剂、粘接力提高剂、润湿性提高剂、消泡剂以及用于低粘度化的反应性稀释剂。另外,本发明的连接材料也可以含有此处列举的以外的成分。
作为上述有机高分子化合物或者其前驱体,并没有特别的限制,优选例如热固性树脂或者其前驱体。作为这样的树脂,可以举出例如:环氧树脂、丙烯酸树脂、马来酰亚胺树脂、异氰酸酯树脂或者其前驱体等。
在它们当中,丙烯酸树脂、马来酰亚胺树脂等具有能够聚合的乙烯性碳-碳双键的化合物或者环氧树脂具有优异的耐热性、粘接性,而且能通过使用合适的溶剂而形成液态,所以操作性优异,从上述观点出发是优选的。上述树脂可以单独使用或者组合使用两种以上。
在使用环氧树脂作为上述热固性树脂的情况下,优选并用固化剂、固化促进剂。作为上述环氧树脂,优选在1分子中具有2个以上环氧基团的化合物,例如可举出由双酚A、双酚F、双酚AD等和表氯醇衍生的环氧树脂等。
作为这样的化合物,只要是在1分子中具有2个以上环氧基团的化合物就没有特别的限制,可以举出例如:双酚A型环氧树脂[AER-X8501(旭化成工业(株)、商品名)、R-301(油化壳牌环氧(株)、商品名)、YL-980(油化壳牌环氧(株)、商品名)]、双酚F型环氧树脂[YDF-170(东都化成(株)、商品名)]、双酚AD型环氧树脂[R-1710(三井石油化学工业(株)、商品名)]、苯酚酚醛清漆型环氧树脂[N-730S(大日本油墨化学工业(株)、商品名)、Quatrex-2010(陶氏化学公司、商品名)]、甲酚酚醛清漆型环氧树脂[YDCN-702S(东都化成(株)、商品名)、EOCN-100(日本化药(株)、商品名)]、多官能环氧树脂[EPPN-501(日本化药(株)、商品名)、TACTIX-742(陶氏化学公司、商品名)、VG-3010(三井石油化学工业(株)、商品名)、1032S(油化壳牌环氧(株)、商品名)]、具有萘骨架的环氧树脂[HP-4032(大日本油墨化学工业(株)、商品名)]、脂环式环氧树脂[EHPE-3150、CEL-3000(大赛璐化学工业(株)、商品名)、DME-100(新日本理化(株)、商品名)]、脂肪族环氧树脂[W-100(新日本理化(株)、商品名)]、胺型环氧树脂[ELM-100(住友化学工业(株)、商品名)、YH-434L(东都化成(株)、商品名)、TETRAD-X、TETRAC-C(三菱瓦斯化学(株)、商品名)]、间苯二酚型环氧树脂[DENACOLEX-201(长濑化成工业(株)、商品名)]、新戊二醇型环氧树脂[DENACOLEX-211(长濑化成工业(株)、商品名)]、己二醇二缩水甘油醚(ヘキサンデイネルグリコ一ル)型环氧树脂[DENACOL EX-212(长濑化成工业(株)、商品名)]、乙二醇丙二醇型环氧树脂[DENACOL EX-810、811、850、851、821、830、832、841、861(长濑化成工业(株)、商品名)]、下述通式(I)表示的环氧树脂[E-XL-24、E-XL-3L(三井东压化学(株)、商品名)]等。另外,这些环氧树脂可以适当地组合使用。
[化学式1]
(式中,a表示0~5的整数)
另外,作为环氧树脂,可以含有:在1分子中只含有1个环氧基的环氧化合物(反应性稀释剂)。对于这样的环氧化合物而言,可在不损害本发明的连接材料的特性的范围内使用,优选在相对于环氧树脂总量为0~30重量%的范围内使用。
作为这样的环氧化合物的市售品,可以举出PGE(日本化药(株)、商品名)、PP-101(东都化成(株)、商品名)、ED-502、509、509S(旭电化工业(株)、商品名)、YED-122(油化壳牌环氧(株)、商品名)、KBM-403(信越化学工业(株)、商品名)、TSL-8350、TSL-8355、TSL-9905(东芝有机硅(株)、商品名)等。
另外,作为环氧树脂固化剂,并没有特别的限制,可以举出例如:苯酚酚醛清漆树脂[H-1(明和化成(株)、商品名)、VR-9300(三井东压化学(株)、商品名)]、苯酚芳烷基树脂[XL-225(三井东压化学(株)、商品名)]、烯丙基化苯酚酚醛清漆树脂[AL-VR-9300(三井东压化学(株)、商品名)]、下述通式(II)所表示的特殊的酚醛树脂[PP-700-300(日本石油化学(株)、商品名)]、双酚F、双酚A、双酚AD、烯丙基化双酚F、烯丙基化双酚A、烯丙基化双酚AD、双氰胺、下述通式(III)所表示的二元酸二酰肼[ADH、PDH、SDH(任何一种均是日本肼工业(株)、商品名)]、包含有环氧树脂和胺化合物的反应物的微胶囊型固化剂[NOVACURE(旭化成工业(株)、商品名)]等。另外,这些固化剂可以适当地组合使用。
[化学式2]
(式中,R1表示甲基、乙基等碳原子数为1~6的烷基,R2表示氢或者甲基、乙基等碳原子数为1~6的烷基、b表示2~4的整数)
[化学式3]
(式中,R3表示间苯撑、对苯撑等2价的芳香族烃基、碳原子数为2~12的直链或者支链的亚烷基。)
环氧树脂固化的配合量相对于100重量份的环氧树脂优选为0.01~90重量份,更优选为0.1~50重量份。如果环氧树脂固化剂的配合量小于0.01重量份,则具有固化性降低的倾向;如果超过90重量份,则具有粘度上升、操作性降低的倾向。
在本发明的连接材料中可以根据需要添加固化促进剂。作为固化促进剂,可以举出有机硼盐化合物[EMZ·K、TPPK(北兴化学工业(株)、商品名)]、叔胺类或者他的盐[DBU、U-CAT102、106、830、840、5002(San-Apro公司、商品名)]、咪唑类[CUREZOL、2P4MHZ、C17Z、2PZ-OK(四国化成(株)、商品名)]等。
环氧树脂固化剂以及根据需要添加的固化促进剂可以分别单独使用,另外,也可以适当地组合使用多种的环氧树脂固化剂以及固化促进剂。固化促进剂的配合量相对于100重量份的环氧树脂优选为20重量份以下。
作为在本发明中使用的具有能够聚合的乙烯性碳-碳双键的化合物,可以举出丙烯酸酯化合物或者甲基丙烯酸酯化合物等,其是在1分子中具有1个以上的丙烯酰基或者甲基丙烯酰基的化合物,优选使用下述通式(IV)~(XIII)所表示的化合物。
通式(IV):
[化学式4]
(式中,R4表示氢或者甲基、R5表示碳原子数为1~100、优选碳原子数为1~36的2价的脂肪族或者具有环状结构的脂肪族烃基。)
作为通式(IV)所示的化合物,可以举出:丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸异丙酯、丙烯酸正丁酯、丙烯酸异丁酯、丙烯酸叔丁酯、丙烯酸戊酯、丙烯酸异戊酯、丙烯酸己酯、丙烯酸庚酯、丙烯酸辛酯、丙烯酸2-乙基己酯、丙烯酸壬酯、丙烯酸癸酯、丙烯酸异癸酯、丙烯酸月桂酯、丙烯酸十三烷酯、丙烯酸十六烷酯、丙烯酸十八烷酯、丙烯酸异十八烷酯、丙烯酸环己酯、丙烯酸异冰片酯、丙烯酸三环[5.2.1.02.6]癸酯等丙烯酸酯化合物,甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丙酯、甲基丙烯酸异丙酯、甲基丙烯酸正丁酯、甲基丙烯酸异丁酯、甲基丙烯酸叔丁酯、甲基丙烯酸戊酯、甲基丙烯酸异戊酯、甲基丙烯酸己酯、甲基丙烯酸庚酯、甲基丙烯酸辛酯、甲基丙烯酸2-乙基己酯、甲基丙烯酸壬酯、甲基丙烯酸癸酯、甲基丙烯酸异癸酯、甲基丙烯酸月桂酯、甲基丙烯酸十三烷酯、甲基丙烯酸十六烷酯、甲基丙烯酸十八烷酯、甲基丙烯酸异十八烷酯、甲基丙烯酸环己酯、甲基丙烯酸异冰片酯、甲基丙烯酸三环[5.2.1.02.6]癸酯等甲基丙烯酸酯化合物。
通式(V)所示的化合物:
[化学式5]
(式中,R4和R5表示的是与通式(IV)中的R4和R5相同的基团。)
作为通式(V)所示的化合物,包括:丙烯酸2-羟基乙酯、丙烯酸2-羟基丙酯、甲基丙烯酸2-羟基乙酯、甲基丙烯酸2-羟基丙酯等。
通式(VI)所示的化合物:
[化学式6]
(式中,R4表示的是与通式(IV)中的R4相同的基团,R6表示氢、甲基或者苯氧基甲基,R7表示氢、碳原子数为1~6的烷基、二环戊烯基、苯基或者苯甲酰基,b表示1~50的整数。)
作为通式(VI)所示的化合物,可以举出:二乙二醇丙烯酸酯、聚乙二醇丙烯酸酯、聚丙二醇丙烯酸酯、丙烯酸2-甲氧基乙酯、丙烯酸2-乙氧基乙酯、丙烯酸2-丁氧基乙酯、甲氧基二乙二醇丙烯酸酯、甲氧基聚乙二醇丙烯酸酯、二环戊烯基氧基乙基丙烯酸酯、丙烯酸2-苯氧基乙酯、苯氧基二乙二醇丙烯酸酯、苯氧基聚乙二醇丙烯酸酯、2-苯甲酰基氧基乙基丙烯酸酯、2-羟基-3-苯氧基丙基丙烯酸酯等丙烯酸酯化合物,二乙二醇甲基丙烯酸酯、聚乙二醇甲基丙烯酸酯、聚丙二醇甲基丙烯酸酯、甲基丙烯酸2-甲氧基乙酯、甲基丙烯酸2-乙氧基乙酯、甲基丙烯酸2-丁氧基乙酯、甲氧基二乙二醇甲基丙烯酸酯、甲氧基聚乙二醇甲基丙烯酸酯、甲基丙烯酸二环戊烯基氧基乙酯、甲基丙烯酸2-苯氧基乙酯、苯氧基二乙二醇甲基丙烯酸酯、苯氧基聚乙二醇甲基丙烯酸酯、甲基丙烯酸2-苯甲酰基氧基乙酯、甲基丙烯酸2-羟基-3-苯氧基丙酯等甲基丙烯酸酯化合物。
通式(VII)所示的化合物:
[化学式7]
[式中,R4表示的是与通式(IV)中的R4相同的基团,R8表示苯基、腈基、-Si(OR9)3(R9表示碳原子数为1~6的烷基)、
[化学式8]
(R10、R11以及R12分别独立地表示氢或者碳原子数为1~6的烷基、R13表示氢或者碳原子数为1~6的烷基或者苯基、c表示0、1、2或者3的数)]。
作为上述通式(VII)以及(VII’)所示的化合物,有丙烯酸苯甲酯、丙烯酸2-氰基乙酯、γ-丙烯酰氧基丙基三甲氧基硅烷、丙烯酸缩水甘油酯、丙烯酸四氢糠酯、丙烯酸四氢吡喃酯、丙烯酸二甲基氨基乙酯、丙烯酸二乙基氨基乙酯、丙烯酸1,2,2,6,6-五甲基哌啶酯、丙烯酸2,2,6,6-四甲基哌啶酯、丙烯酰氧基乙基磷酸酯、丙烯酰氧基乙基苯基酸式磷酸酯、β-丙烯酰氧基乙基氢化邻苯二甲酸酯、β-丙烯酰氧基乙基氢化琥珀酸酯等丙烯酸酯化合物,甲基丙烯酸苯甲酯、甲基丙烯酸2-氰基乙酯、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、甲基丙烯酸缩水甘油酯、甲基丙烯酸四氢糠酯、甲基丙烯酸四氢吡喃酯、甲基丙烯酸二甲基氨基乙酯、甲基丙烯酸二乙基氨基乙酯、甲基丙烯酸1,2,2,6,6-五甲基哌啶酯、甲基丙烯酸2,2,6,6-四甲基哌啶酯、甲基丙烯酰氧基乙基磷酸酯、甲基丙烯酰氧基乙基苯基酸式磷酸酯、β-甲基丙烯酰氧基乙基氢化邻苯二甲酸酯、β-甲基丙烯酰氧基乙基氢化琥珀酸酯等甲基丙烯酸酯化合物。
通式(VIII)所示的化合物:
[化学式9]
(式中,R4和R5表示的是与通式(IV)中的R4和R5相同的基团。)
作为通式(VIII)所示的化合物,有:乙二醇二丙烯酸酯、1,4-丁二醇二丙烯酸酯、1,6-己二醇二丙烯酸酯、1,9-壬二醇二丙烯酸酯、1,3-丁二醇二丙烯酸酯、新戊二醇二丙烯酸酯、二聚醇二丙烯酸酯等二丙烯酸酯化合物,乙二醇二甲基丙烯酸酯、1,4-丁二醇二甲基丙烯酸酯、1,6-己二醇二甲基丙烯酸酯、1,9-壬二醇二甲基丙烯酸酯、1,3-丁二醇二甲基丙烯酸酯、新戊二醇二甲基丙烯酸酯、二聚醇二甲基丙烯酸酯等二甲基丙烯酸酯化合物。
通式(IX)所示的化合物:
[化学式10]
(式中,R4表示的是与通式(IV)中的R4相同的基团,R6、b表示的是与通式(VI)中的R6、b相同的基团。)
作为通式(IX)所示的化合物,有:二乙二醇二丙烯酸酯、三乙二醇二丙烯酸酯、四乙二醇二丙烯酸酯、聚乙二醇二丙烯酸酯、三丙二醇二丙烯酸酯、聚丙二醇二丙烯酸酯等二丙烯酸酯化合物,二乙二醇二甲基丙烯酸酯、三乙二醇二甲基丙烯酸酯、四乙二醇二甲基丙烯酸酯、聚乙二醇二甲基丙烯酸酯、三丙二醇二甲基丙烯酸酯、聚丙二醇二甲基丙烯酸酯等二甲基丙烯酸酯化合物。
通式(X)所示的化合物:
[化学式11]
(式中,R4表示的是与通式(IV)中的R4相同的基团,R14和R16分别独立地表示氢或者甲基。)
作为通式(X)表示的化合物,有:1摩尔的双酚A、双酚F或双酚AD和2摩尔的丙烯酸缩水甘油酯的反应物、1摩尔的双酚A、双酚F或双酚AD和2摩尔的甲基丙烯酸缩水甘油酯的反应物等。)
通式(XI)所示的化合物:
[化学式12]
(式中,R4表示的是与通式(IV)中的R4相同的基团,R14和R15表示的是与通式(X)中的R14、R15相同的基团,R16和R17分别独立地表示氢或者甲基,d和e分别独立地表示1~20的整数。)
作为通式(XI)所示的化合物,有:双酚A、双酚F或者双酚AD的聚环氧乙烷加成物的二丙烯酸酯,双酚A、双酚F或者双酚AD的聚环氧丙烷加成物的二丙烯酸酯,双酚A、双酚F或者双酚AD的聚环氧乙烷加成物的二甲基丙烯酸酯,双酚A、双酚F或者双酚AD的聚环氧丙烷加成物的二丙烯酸酯等。
通式(XII)所示的化合物:
[化学式13]
(式中,R4表示的是与通式(IV)中的R4相同的基团,R18、R19、R20以及R21分别独立地表示氢或者甲基、f表示1~20的整数。)
作为通式(XII)所示的化合物,有:双(丙烯酰氧基丙基)聚二甲基硅氧烷、双(丙烯酰氧基丙基)甲基硅氧烷-二甲基硅氧烷共聚物、双(甲基丙烯酰氧基丙基)聚二甲基硅氧烷、双(甲基丙烯酰氧基丙基)甲基硅氧烷-二甲基硅氧烷共聚物等。
通式(XIII)所示的化合物:
[化学式14]
(式中,R4表示的是与通式(IV)中的R4相同的基团,g、h、i、j以及k分别独立地表示1以上、优选为1~10的整数。)
作为通式(XIII)所示的化合物,有:使加成有马来酸酐的聚丁二烯与分子内带有羟基的丙烯酸酯化合物或者甲基丙烯酸酯化合物进行反应而得到的反应物及其加氢产物;只要是在1分子中具有1个以上的丙烯酰基或者甲基丙烯酰基的化合物就没有特别的限制,例如MM-1000-80、MAC-1000-80(都是日本石油化学(株)商品名)等。
关于具有可聚合的乙烯性碳-碳双键的化合物而言,可以将上述化合物单独使用或者组合使用2种以上。
在使用具有乙烯性碳-碳双键的化合物作为上述热固性树脂的情况下,优选并用自由基引发剂作为固化剂催化剂。作为自由基引发剂并没有特别的限制,从空隙等方面考虑,优选为过氧化物,另外从连接材料的固化性以及粘度稳定性的观点出发,优选为过氧化物的分解温度为70~170℃的过氧化物。
作为自由基引发剂的具体例子,可以举出:1,1,3,3-四甲基过氧化2-乙基己酸酯、1,1-双(叔丁基过氧化)环己烷、1,1-双(叔丁基过氧化)环十二烷、二叔丁基过氧化异邻苯二甲酸酯、叔丁基过氧化苯甲酸酯、二异丙苯基过氧化物、叔丁基异丙苯基过氧化物、2,5-二甲基-2,5-二(叔丁基过氧化)己烷、2,5-二甲基-2,5-二(叔丁基过氧化)己炔、异丙基苯氢化过氧化物等。
自由基引发剂的配合量,相对于100重量份的具有能够聚合的乙烯性碳-碳双键的化合物的总量,优选为0.1~10重量份,特别优选为0.5~5重量份。
上述粘合剂成分,可以使用1种成分或者可以根据需要使用2种以上的成分。当把连接材料全体作为100重量份时,粘合剂成分的含有量优选为3~30重量份。
作为增韧剂的例子,可以举出:液态聚丁二烯(宇部兴产社制“CTBN-1300×31”、“CTBN-1300×9”)等丙烯腈丁二烯共聚物,优选为在分子内具有选自环氧基、羧基、氨基以及乙烯基中的至少1种以上的官能团的物质。
丙烯腈丁二烯共聚物可以先与上述的环氧树脂以环氧树脂∶丙烯腈丁二烯共聚物=10∶90~90∶10(重量份)的比例,在80℃~120℃反应20分钟~6小时左右的时间。在反应时根据需要可以使用:乙二醇单丁醚(butylcellosolve)、卡必醇、乙二醇单丁醚醋酸酯、卡必醇醋酸酯、乙二醇二乙醚、α-萜品醇等沸点比较高的有机溶剂。
作为丙烯腈丁二烯共聚物的数均分子量,优选为500~10000。如果分子量小于500,则具有芯片翘曲的降低效果劣化的倾向;如果分子量超过10000,则具有连接材料的粘度上升、操作性劣化的倾向。数均分子量是用蒸气压渗透法测定的值,或者是通过凝胶渗透色谱利用标准聚苯乙烯的标准曲线所测定(以下称作GPC法)的值。
另外,作为环氧化聚丁二烯,优选环氧当量为100~500(g/eq)的环氧化聚丁二烯。在环氧当量小于100的情况下,具有粘度增大、连接材料的操作性下降的倾向;如果超过500,则存在热时的粘接强度下降的倾向。另外,环氧当量通过高氯酸法求得。作为环氧化聚丁二烯,可以使用在分子内具有羟基的物质。
作为环氧化聚丁二烯的数均分子量,优选为500~10000。如果分子量小于500,则具有芯片翘曲的降低效果劣化的倾向;如果分子量超过10000,则具有连接材料的粘度上升、操作性劣化的倾向。数均分子量是通过GPC法所测定的值。
增韧剂具有的效果:对因粘接半导体元件和引线框而产生的应力进行缓和。通常,当把有机高分子化合物以及其前驱体的总量作为100重量份时,添加0~500重量份增韧剂。
在本发明的连接材料中,根据需要可以进一步适当添加:氧化钙、氧化镁等吸湿剂,硅烷偶联剂、钛酸酯偶联剂、铝偶联剂、铝酸锆偶联剂等粘接力提高剂,非离子系表面活性剂、氟系表面活性剂等润湿性提高剂,硅油等消泡剂,无机离子交换体等离子捕捉剂,阻聚剂等。
此处,作为硅烷偶联剂,例如,可举出乙烯基三(β-甲氧基乙氧基)硅烷、乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、β-(3,4-环氧环己基)乙基三甲氧基硅烷、γ-环氧丙氧基丙基三甲氧基硅烷、γ-环氧丙氧基丙基甲基二乙氧基硅烷、N-苯基-γ-氨基丙基三甲氧基硅烷、γ-巯基丙基三甲氧基硅烷、六甲基二硅氮烷、N,O-(双三甲基甲硅烷基)乙酰胺、N-甲基-3-氨基丙基三甲氧基硅烷、4,5-二氢化咪唑基丙基三乙氧基硅烷、γ-巯基丙基三乙氧基硅烷、γ-巯基丙基甲基二甲氧基硅烷、3-氰基丙基三甲氧基硅烷、甲基三(甲基丙烯酰氧基乙氧基)硅烷、甲基三(环氧丙氧基)硅烷、2-乙基己基-2-乙基己基磷酸酯、γ-环氧丙氧基丙基甲基二甲氧基硅烷、乙烯基三乙酰氧基硅烷、γ-苯胺基丙基三甲氧基硅烷、γ-巯基丙基甲基二甲氧基硅烷、γ-甲基丙烯酰氧基丙基甲基二甲氧基硅烷、N-三甲基甲硅烷基乙酰胺、二甲基三甲基甲硅烷基胺、二乙基三甲基甲硅烷基胺、三甲基甲硅烷基咪唑、三甲基甲硅烷基异氰酸酯、二甲基甲硅烷基二异氰酸酯、甲基甲硅烷基三异氰酸酯、乙烯基甲硅烷基三异氰酸酯、苯基甲硅烷基三异氰酸酯、四异氰酸酯硅烷、乙氧基硅烷三异氰酸酯等。
作为上述的钛酸酯偶联剂,例如,可以举出:异丙基三异十八酰基钛酸酯、异丙基三辛酰基钛酸酯、异丙基二甲基丙烯酰基异十八酰基钛酸酯、异丙基三(十二烷基)苯磺酰基钛酸酯、异丙基异十八酰基二丙烯酰基钛酸酯、异丙基三(二辛基磷酸酯)钛酸酯、异丙基三异丙苯基苯基钛酸酯、异丙基三(二辛基焦磷酸酯)钛酸酯、四异丙基双(二辛基亚磷酸酯)钛酸酯、四辛基双(二-十三烷基磷酸酯)钛酸酯、四(2,2-二烯丙基氧基甲基-1-丁基)双(二-十三烷基亚磷酸酯)钛酸酯、四(2,2-二苯基氧基甲基-1-丁基)双(二-十三烷基)亚磷酸酯钛酸酯、二异丙苯基苯基氧基乙酸酯钛酸酯、双(二辛基焦磷酸酯)氧基乙酸酯钛酸酯、二异十八酰基亚乙基钛酸酯、双(二辛基焦磷酸酯)亚乙基钛酸酯、二异丙氧基双(2,4-乙酰丙酮化物)钛(IV)、二异丙基双三乙醇氨基钛酸酯、乳酸钛酸酯(titanium lactate)、乙酰乙酸酯钛酸酯、二异丙氧基双(乙酰丙酮基)钛、二正丁氧基双(三乙醇胺根合)钛、二羟基双(乳酸酯)钛、钛异丙氧基亚辛基乙醇酸酯、钛十八酸酯(チタニウムステアレ一ト)、三正丁氧基钛单十八酸酯、钛乳酸乙酯、氨化三乙醇钛等。
作为阻聚剂,可以举出例如:醌类、氢醌、硝基-亚硝基化合物、胺类、多氧化合物、对叔丁基苯二酚、苦味酸、二硫代苄基二硫醚等含硫化合物,氯化铜、二苯基苦基苯肼、三对硝基苯基甲基(トリ-p-ニトロフエニルメチル)、三苯基绿腙肼、N-(3-N-氧基苯胺基-1,3-二甲基亚丁基)苯胺氧化物等,但是并不限于这些。
在本发明的连接材料中,根据需要可以进一步添加渗漏抑制剂。作为渗漏抑制剂,具有例如:全氟辛酸、辛酸酰胺、油酸等脂肪酸、全氟辛基乙基丙烯酸酯、有机硅等。
作为上述填料(B),可以使用各种公知的填料,例如,金、铂、银、铜、镍、钯、铁、铝等导电性的粉体。另外,这些填料可以单独使用或者组合使用二种以上。其中,从价格、导电性以及导热性等方面考虑,优选银和铜。
作为上述添加剂(C),可以使用上述的挥发性成分、表面保护剂。
在制造上述连接材料时,将金属粒子、挥发性成分、粘合剂以及根据需要添加的稀释剂等合在一起或者分开来,适当地组合搅拌器、研磨机、三辊、行星搅拌器等分散、溶解装置并根据需要进行加热,对上述材料进行混合、溶解、解粒混炼或者分散,从而形成均匀的糊状即可。
图7是表示使用本发明的连接材料所制造的半导体装置的一例的截面示意图。图7所示的半导体装置包括:3个引线框(放热体)12a、12b、12c;在引线框12a上经由本发明的连接材料来连接的芯片(发热体)11;将这些铸型的铸型树脂15。芯片11通过2根导线14分别连接在引线框12b、12c上。
图8是表示使用本发明的连接材料所制造的半导体装置的另外一例的截面示意图。图7所示的半导体装置,包括:基板16;以包裹基板的形式形成2个引线框17;在引线框17上隔着本发明的连接材料而连接的LED芯片18;对这些进行封固的透光性树脂19。LED芯片18通过导线14连接到引线框17。
本发明的半导体装置,通过使用本发明的连接材料把半导体元件连接在支撑部件上而得到。把半导体元件连接在支撑部件上之后,根据需要进行引线键合工序、封固工序。
作为支撑部件,可以举出例如:42合金引线框、铜引线框、钯PPF引线框等引线框,玻璃环氧树脂基板(玻璃纤维增强环氧树脂形成的基板)、BT基板(氰酸酯单体及其低聚物和双马来酰亚胺形成的BT树脂使用基板)等有机基板。
在使用本发明的连接材料把半导体元件粘接在引线框等支撑部件上时,可以如下施行:首先,通过分散法、网印法、压印法等在支撑部件上涂布连接材料后,压合半导体元件,其后,使用烘箱或者微量恒温仪等加热装置来加热固化。加热固化通常在100~200℃、加热5秒~10小时的时间来进行。进一步地,经过引线键合工序之后,通过使用通常的方法来进行封固,可以得到成品的半导体装置。
实施例
下面,通过实施例详细地说明本发明,但是本发明不受其限制。实施例以及参考例中使用的材料是按照如下方式制作的或者购得的。
(1)环氧树脂溶液:把7.5重量份的YDF-170(东都化成(株)、商品名、双酚F型环氧树脂、环氧当量=170)和7.5份重量份的YL-980(油化壳牌环氧(株)、商品名、双酚A型环氧树脂、环氧当量=185)加热到80℃,连续搅拌1小时,得到均匀的环氧树脂溶液。
(2)固化促进剂:1.1重量份的2PZCNS-PW(四国化成工业(株)、商品名、咪唑);
(3)挥发性成分:二丙二醇甲基醚乙酸酯(以下称作DMPA)(大赛璐化学(株))、甲苯(关东化学(株))、γ-丁内酯(三协化学(株))
(4)金属粒子:K-0082P(METALOR、商品名、银粉、平均粒径1.6μm,氧状态比率4%)、AgF10S(德力化学研究所(株)、商品名、银粉、平均粒径10μm、氧状态比率15%)
另外,按照下面的顺序,对AgF10S实施氧化膜除去以及表面处理,制作出表面处理Ag粉。
用80重量份的乙醇(关东化学(株))稀释28重量份的盐酸(关东化学(株)),制备成酸性溶液。在该酸性溶液中添加0.29重量份的作为表面保护材料的十八硫醇(东京化学工业(株)),制备表面处理液。
把AgF10S添加到该表面处理液中,在保持于40℃的状态下搅拌1小时,进行氧化膜除去以及表面处理。之后,通过过滤除去表面处理液,添加40℃的乙醇、洗涤表面处理Ag粉。
进一步,通过过滤去除乙醇洗涤液,该洗涤和过滤的工序重复10次左右,除去物理吸附在表面处理Ag粉表面上的十八硫醇以及盐酸。
最后,通过减压干燥洗涤后的表面处理Ag粉,除去乙醇,得到干燥状态的表面处理Ag粉。确认得到的表面处理Ag粉的氧的状态比率为0%,氧化膜完全被除去。
把材料(1)和(2)用研磨机混炼10分钟,得到粘合剂成分。
接下来,按照如表1所示的配合比例,加入材料(3)和(4),用研磨机混炼15分钟,得到连接材料。
用下述的方法来研究连接材料的特性。金属粒子、挥发性成分以及粘合剂成分的组成以及特性的测定结果如表1和表2所示。
(1)剪切强度:把0.2mg的连接材料涂布在镀银的铜引线框(连接盘(land)部:10×5mm)上,在其上粘接2mm×2mm的镀银的铜芯片(厚度为0.15mm)、进一步在加热板(HHP-401)上于180℃加热处理1小时。
使用万能型粘合强度试验机(DAGE公司制、4000系列),在测定速度为500μm/s、测定高度为100μm的条件下,在260℃加热30秒之后测定它的剪断强度(剪切强度)(MPa)。
(2)连接材料固化物的热导率:对上述连接材料在180℃加热处理1小时,得到10×10×1mm的试验片。用激光闪解法(NETZSCH公司制、LFA447、25℃)测定该试验片的热扩散率,进一步根据该热扩散率、通过差示扫描量热测定装置(PerkinElmer社制Pyris1)所得到的比热容和通过阿基米德(Archimedes)法得到的比重的积,算出25℃下连接材料的固化物热导率(W/m·K)。
表1
表2
*由于金属粒子没有烧结,所以10×10×1mm的热导率测定用的试验片不能够制作。
如表1和表2所示,可以明显地看出,实施例1~3的包含表面处理Ag粉和挥发性物质的连接材料表现出了70W/m·K以上这样高的热导率,以及在260℃下7MPa以上这样高的剪切强度。与此相对,由参考例1~3可以明显地看出,包含氧的状态比率为15%以上的Ag粉(AgF10S)和挥发性成分的连接材料,由于在180℃下金属粒子彼此间没有发生烧结,所以不能够制作热导率测定用试验片,也没有表现出剪切强度。
另外,由参考例4可以明显地看出,包含氧的状态比率为15%以上的Ag粉(AgF10S)和挥发性成分以及粘合剂成分的连接材料,具有3W/m·K以下这样低的热导率;而实施例4的包含表面处理Ag粉和挥发性成分以及粘合剂成分的连接材料不仅维持了剪切强度,而且表现出20W/m·K以上这样高的热导率。
另外,由参考例5可以明显地看出,包含氧的状态比率为15%以上的AgF10S和粘合剂成分的连接材料,具有2W/m·K以下这样低的热导率;而实施例5的包含表面处理AgF10S和粘合剂成分的连接材料不仅维持了剪切强度,而且表现出20W/m·K以上这样高的热导率。
另外,由实施例6和7可以明显地看出,包含氧的状态比率为10%的表面处理AgF5S和挥发性成分以及粘合剂成分的连接材料,与参考例6和7所示的包含氧的状态比率为20%以上的AgF5S和挥发性成分以及粘合剂成分的连接材料相比,表现出高的热导率和剪切强度。
(实施例8~14以及参考例8~11)
准备下述的粘合剂(A)、填料(B)以及添加剂(C)。
粘合剂(A):
粘合剂(A)通过用研磨机把下列物质混炼10分钟而制备:环氧树脂溶液(A1)37.6重量份、丙烯腈丁二烯共聚物(A2)9.2重量份、环氧化聚丁二烯(A3)18.4重量份、环氧树脂固化剂(A4)1.8重量份、固化促进剂(A5)0.8重量份、稀释剂(A6)18.2重量份、甲基丙烯酸酯化合物(A7)14.7重量份以及自由基引发剂(A8)0.5重量份。
环氧树脂溶液(A1):把YDF-170(东都化成株式会社、商品名、双酚F型环氧树脂、环氧当量=170)7.5重量份以及YL-980(日本环氧树脂株式会社、商品名、双酚A型环氧树脂、环氧当量=185)7.5重量份,加热至80℃,连续搅拌1小时,得到均匀的环氧树脂溶液。
丙烯腈丁二烯共聚物(A2):
CTBNX-1300×9(宇部兴产业株式会社、商品名、端羧基丙烯腈丁二烯共聚物)
环氧化聚丁二烯(A3):
E-1000-8.0(日本石油化学株式会社、商品名)
环氧树脂固化剂(A4):
双氰胺
固化促进剂(A5):
C17Z(四国化成株式会社、商品名、咪唑)
稀释剂(A6):
PP-101(东都化成株式会社、商品名、烷基苯基缩水甘油醚)
甲基丙烯酸酯化合物(A7):
乙二醇二甲基丙烯酸酯
自由基引发剂(A8):
二异丙苯基过氧化物
填料(B):
AgC-224(福田金属箔粉株式会社、商品名、银粉、平均粒径为10μm)
SPQ05J(三井金属矿业株式会社、商品名、银粉、平均粒径为0.85μm)
SA-1507(Metalor、商品名、银粉、平均粒径为15μm)
添加剂(C):
二丙二醇甲基醚
甲苯
丙二醇甲基醚乙酸酯
十二硫醇
把准备好的粘合剂(A)、填料(B)以及添加剂(C)按照表3所示的配合比例混合,用研磨机混炼15分钟之后,在5托耳(Torr)以下混炼,得到实施例8~14以及参考例8~11的连接材料。
实施例8~14以及参考例8~11的连接材料的特性、以及填料(B)和添加剂(C)的混合物成型体的特性,用下述的方法测定。其结果示于表3中。
(1)粘度:用EHD型旋转粘度计(东京计器社制),测定连接材料在25℃时的0.5rpm的粘度(Pa·s)。
(2)晶片剪切强度(剪断强度):把大约0.2mg的连接材料涂布在镀钯的引线框(PPF、连接盘(land)部:10×8mm)上,在其之上压接2mm×2mm的硅芯片(厚度为0.4mm)、进一步在洁净烘箱(ESPEC公司制)中在180℃下加热处理1小时。使用万能型粘合强度试验机(DAGE社制、4000系列),在测定速度为500μm/s、测定高度为120μm的条件下,在260℃加热30秒之后测定它的剪断强度(MPa)。
(3)填料(B)和添加剂(C)的混合物成型体的热导率:按照表3所示的配合比例、以总重量为20g的方式来配合填料(B)和添加剂(C),用研钵等混炼。把生成的粉体状或者糊状的混合物成型为10×10×1mm,在180℃加热处理1小时。用激光闪解法(NETZSCH公司制、LFA 447、25℃)测定该成型物的热扩散率,进一步根据该热扩散率、通过差示扫描量热测定装置(PerkinElmer公司制Pyris1)所得到的比热容和通过阿基米德法得到的比重的积,算出25℃下填料(B)和添加剂(C)的混合物成型体的固化物热导率(W/m·K)。
(4)连接材料的固化物的热导率:将上述连接材料在180℃加热处理1小时,得到10×10×1mm的试验片。用激光闪解法(NETZSCH公司制、LFA 447、25℃)测定该试验片的热扩散率,进一步根据该扩散率、通过差示扫描量热测定装置(PerkinElmer公司制Pyris1)所得到的比热容和通过阿基米德法得到的比重的积,算出25℃下连接材料的固化物热导率(W/m·K)。
表3
根据实施例8~14的连接材料,可以在具有操作性优异的粘度、维持粘接强度的同时,实现热导率的提高。关于不含有添加剂的参考例8的连接材料而言,填料(B)和添加剂(C)的混合物成型物的热导率低、连接材料的固化物的热导率也低。关于不含有添加剂的参考例9的连接材料而言,虽然连接材料的固化物的热导率比较高,但是由于填料(B)的含有比率高,所以连接材料的粘度高。参考例10的连接材料虽然含有添加剂,但是由于填料(B)和添加剂(C)的混合物成型体的热导率低,所以连接材料的固化物的热导率变低。参考例11的连接材料具有添加剂,连接材料的固化物的热导率高,但是填料(B)和添加剂(C)的混合物成型体的热导率低,连接材料的粘度高。
符号说明
1,4:表面保护材料、2:氧化膜、3:本体金属、11:芯片、12a,12b,12c:引线框、14:导线、15:铸型树脂、16:基板、17:引线框、18:芯片、19:透光性树脂。
Claims (7)
1.一种连接材料,其特征在于,其是含有粘合剂(A)、填料(B)以及添加剂(C)的连接材料,
把所述填料(B)和所述添加剂(C)按照与所述连接材料中的重量比相同的重量比来进行混合、加热成型而得到的成型体的热导率为40W/mK以上。
2.根据权利要求1所述的连接材料,其特征在于,所述添加剂(C)的含有量相对于100重量份的粘合剂(A)为1~100重量份。
3.根据权利要求1或2所述的连接材料,其特征在于,以所述连接材料全体作为100重量份时,所述粘合剂成分(A)为3~30重量份。
4.根据权利要求1~3中任一项所述的连接材料,其特征在于,所述粘合剂成分(A)为丙烯酸树脂、马来酰亚胺树脂等具有能够聚合的乙烯性碳-碳双键的化合物或者环氧树脂。
5.根据权利要求1~4中任一项所述的连接材料,其特征在于,所述填料(B)为银或铜。
6.根据权利要求1~5中任一项所述的连接材料,其特征在于,所述添加剂(C)为挥发性成分或表面保护材料。
7.一种半导体装置,其特征在于,具有如下结构:半导体元件和半导体元件搭载用支撑部件通过权利要求1~6中的任意一项所述的连接材料而被粘接。
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