CN114730715B - 临时固定用组合物及接合结构体的制造方法 - Google Patents

临时固定用组合物及接合结构体的制造方法 Download PDF

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CN114730715B
CN114730715B CN202180006483.4A CN202180006483A CN114730715B CN 114730715 B CN114730715 B CN 114730715B CN 202180006483 A CN202180006483 A CN 202180006483A CN 114730715 B CN114730715 B CN 114730715B
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bonded
temporary fixing
organic component
fixing composition
boiling point
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CN114730715A (zh
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穴井圭
赵亭来
田代健悟
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Mitsui Mining and Smelting Co Ltd
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Mitsui Mining and Smelting Co Ltd
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  • Engineering & Computer Science (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Powder Metallurgy (AREA)
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Abstract

为用于在将第1被接合材与第2被接合材接合之前将两者临时固定的临时固定用组合物。该临时固定用组合物包含25℃下的粘度小于70mPa·s并且沸点为200℃以下的第1有机成分、和25℃下的粘度为70mPa·s以上并且沸点为210℃以上的第2有机成分。优选在升温速度10℃/分钟、氮气气氛、试样质量30mg的条件下进行热重差热分析时的95％失重温度低于300℃。

Description

临时固定用组合物及接合结构体的制造方法
技术领域
本发明涉及为了在将两种被接合材接合之前将两者临时固定而使用的组合物。另外，本发明涉及使用了该组合物的接合结构体的制造方法。
背景技术
半导体元件、与电路基板、陶瓷基板等基板或引线框等布线体的连接中，迄今为止使用焊料。焊料本来为含有铅的合金，铅为环境负荷物质，因此随着近年的环境意识升高，提出了各种不含有铅的无铅焊料。
但是，近年作为逆变器等电力变换·控制装置，盛行使用被称为功率器件的半导体装置。功率器件与存储器、微处理器等集成电路不同，用于控制高电流，因此工作时的发热量非常大。因此，对于功率器件的安装中使用的焊料要求耐热性。但是，上述无铅焊料与通常的含有铅的焊料相比，存在耐热性低这种缺点。
因此，提出了下述各种技术：替代使用焊料，而使用含有金属微粒的糊剂，将其通过各种涂布装置涂布于对象物，并进行焙烧。例如专利文献1中记载了，在半导体芯片与芯片装载部之间配置含有银颗粒的糊剂，通过银颗粒的烧结体将半导体芯片和芯片装载部接合的方法。该方法中，以具有与芯片装载部接触的部分的方式供给具有粘性的临时固定剂，并且以半导体芯片的背面的一部分与临时固定剂接触的方式将半导体芯片装载于糊剂上。
现有技术文献
专利文献
专利文献1：US2018/247884A1
发明内容
利用专利文献1中记载的技术时，配置于芯片装载部的临时固定剂与含有银颗粒的糊剂有可能接触。此时，根据临时固定剂中含有的成分的种类，含有银颗粒的糊剂的特性有可能变化。这是在半导体芯片与芯片装载部的接合产生不良问题的原因之一。因此，本发明的目的在于，提供不会对于接合材料的特性造成影响，为了利用该接合材料将被接合材彼此顺利地接合而使用的临时固定用组合物、以及使用了该组合物的接合结构体的制造方法。
本发明提供一种临时固定用组合物，其包含25℃下的粘度小于70mPa·s并且沸点为200℃以下的第1有机成分、和
25℃下的粘度为70mPa·s以上并且沸点为210℃以上的第2有机成分，
所述临时固定用组合物用于在将第1被接合材与第2被接合材接合之前将两者临时固定。
附图说明
图1的(a)～(d)为依次表示使用本发明的临时固定用组合物将两种被接合材接合的工序的示意图。
具体实施方式
本发明涉及临时固定用组合物。临时固定用组合物用于在将第1被接合材与第2被接合材接合(即正式固定)之前将两者临时固定。被临时固定的第1被接合材和第2被接合材通过以下工序、例如烧结工序接合而形成接合结构体。
“临时固定”指的是，第1被接合材和第2被接合材被固定的状态并且虽然施加大的外力时固定状态变化但是不会由于小的外力(例如将第1被接合材和第2被接合材的临时固定物以两被接合材的接合面朝向铅直方向的方式载置时，第1或第2的被接合材中任意一者由于自重而落下的程度的力)而固定状态变化的固定方式。
对于第1被接合材和第2被接合材的种类没有特别限制。通常优选第1被接合材和第2被接合材都在它们的接合对象面含有金属。例如作为第1被接合材和第2被接合材中的至少一者，可以使用具有由金属形成的表面的构件。另外，作为第1被接合材和第2被接合材中的至少一者，也可以使用含有金属微粒和有机溶剂的糊剂的干燥体。具体而言，可以作为第1被接合材，使用具有由金属形成的表面的构件，作为第2被接合材，使用含有金属微粒和有机溶剂的糊剂的干燥体。需要说明的是，使用糊剂的干燥体的情况下，优选通过在由铜等金属形成的支承基材涂布糊剂并进行干燥而形成干燥体。
需要说明的是，上述“含有金属微粒和有机溶剂的糊剂的干燥体”例如在以下工序中被加热的情况下，该干燥体中含有的该金属微粒彼此烧结，因此该干燥体可以看作烧结前体。因此本说明书中，在此以后将“含有金属微粒和有机溶剂的糊剂的干燥体”也称为“烧结前体”。
第1被接合材由具有表面的构件形成、所述表面由金属形成，第2被接合材由烧结前体形成的情况下，第1被接合材中的金属与第2被接合材中的金属微粒的金属可以为相同种类或不同种类。在此所称的“金属”指的是与其它元素不形成化合物的金属其本身、或两种以上的金属的合金。对于金属的种类没有特别限制，但是若考虑到本发明的临时固定用组合物与替代焊料的接合构件组合使用，则使用具有高于焊料的熔点的熔点的金属是有利的。作为这种金属，可列举出例如铜、银、金、铝、钛、镍或由它们中的两种以上的组合形成的合金。
第1被接合材和第2被接合材中的至少一者为具有由金属形成的表面的构件的情况下，由该金属形成的表面可以由一种金属构成、或由两种以上的金属构成。由两种以上的金属构成的情况下，该表面可以为合金。由金属形成的表面通常优选为平面，但是根据需要也可以为曲面。
第1被接合材和第2被接合材中的至少一者为烧结前体的情况下，该烧结前体由干燥体形成，该干燥体是从含有金属微粒和有机溶剂的糊剂的涂膜将该有机溶剂挥发、去除而得到的。
糊剂中含有的金属微粒可以由一种金属构成、或由两种以上的金属的合金构成。另外，金属微粒也可以由不同的两种以上的金属微粒的混合物构成。
金属微粒的体积累积粒径DSEM50为0.01μm以上且30μm以下从良好地保持第1被接合材与第2被接合材的接合的观点考虑优选。从同样的观点考虑，金属微粒的体积累积粒径DSEM50进一步优选为0.03μm以上且20μm以下、进一步优选0.05μm以上且15μm以下。
体积累积粒径DSEM50例如利用以下的方法测定。使用MOUNTECH Co.Ltd.,制Mac-View，读入金属微粒的SEM图像后，随机选择SEM图像上的金属微粒50个以上，测定该颗粒的粒径(海伍德直径)。接着由所得到的海伍德直径，算出假定颗粒为真球时的体积，作为该体积的累积体积50容量％时的体积累积粒径DSEM50。
对于金属微粒的形状没有特别限制，可列举出例如球状、多面体状、扁平状、不定形、或它们的组合等。另外，金属微粒可以在其粒度分布中具有两个以上的峰。
金属微粒可以在其表面附着表面处理剂。通过在金属微粒的表面附着表面处理剂，可以抑制金属微粒彼此的过度聚集。
对于表面处理剂没有特别限定，可以使用脂肪酸、脂肪族胺、硅烷偶联剂、钛酸酯(盐)系偶联剂、铝酸酯(盐)系偶联剂等。通过使用它们，与颗粒的表面相互作用，可以改善与糊剂中含有的有机溶剂的相容性，改善糊剂的流动性，防止颗粒表面的氧化。
前述糊剂及作为其干燥体的烧结前体中可以适当含有用于调节糊剂、烧结前体的各种特性的调节剂。作为调节剂，可列举出例如固体还原剂、粘度调节剂、表面张力调节剂。
作为固体还原剂，优选在25℃下示出固体的性质、并且示出还原作用，可列举出例如双(2-羟基乙基)亚氨基三(羟基甲基)甲烷、三羟甲基丙烷、核糖醇、葡萄糖、抗坏血酸、对苯二酚等。
作为粘度调节剂，若可以调节前述糊剂的粘度的高低即可，可列举出例如酮类、酯类、醇类、二元醇类、烃、聚合物等。
作为表面张力调节剂，若可以调节前述糊剂的表面张力即可，可列举出例如丙烯酸类表面活性剂、硅氧烷系表面活性剂、烷基聚氧亚乙基醚、脂肪酸甘油酯等聚合物、醇系、烃系、酯系、二元醇等单体。
上述烧结前体由干燥体形成，该干燥体是从含有金属微粒和有机溶剂以及根据需要的调节剂的糊剂的涂膜将该有机溶剂挥发、去除而得到的。特别是有机溶剂无需去除其总量，只要以糊剂的涂膜失去流动性的程度去除有机溶剂即可。因此，烧结前体中可以残留有机溶剂。烧结前体中含有的有机溶剂的比率例如可以为15质量％以下、特别是可以为10质量％以下。
对于前述有机溶剂的种类没有特别限制，若可以分散金属微粒而形成糊剂状即可。作为有机溶剂的例子，可列举出一元醇、多元醇、多元醇烷基醚、多元醇烯丙基醚、酯类、含氮杂环化合物、酰胺类、胺类、饱和烃等。这些有机溶剂可以单独使用一种或组合两种以上来使用。
作为一元醇，例如可以使用1-丙醇、1-丁醇、1-戊醇、1-己醇、环己醇、1-庚醇、1-辛醇、1-壬醇、1-癸醇、缩水甘油、苯甲醇、甲基环己醇、2-甲基1-丁醇、3-甲基-2-丁醇、4-甲基-2-戊醇、2-丙醇、2-乙基丁醇、2-乙基己醇、2-辛醇、2-甲氧基乙醇、2-乙氧基乙醇、2-正丁氧基乙醇、2-苯氧基乙醇、松油醇等。
作为多元醇，可以使用乙二醇、丙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇、二甘醇、一缩二丙二醇、三甘醇、四乙二醇、己二醇、聚乙二醇等。
作为多元醇烷基醚，可以使用乙二醇单甲基醚、乙二醇单乙基醚、乙二醇单丁基醚、二甘醇单甲基醚、二甘醇单乙基醚、二甘醇单丁基醚、三甘醇单甲基醚、三甘醇单乙基醚、丙二醇单丁基醚等。
作为多元醇烯丙基醚，可以使用乙二醇单苯基醚等。作为酯类，可以使用乙基溶纤剂乙酸酯、丁基溶纤剂乙酸酯、γ-丁内酯等。作为含氮杂环化合物，可以使用N-甲基吡咯烷酮、1,3-二甲基-2-咪唑啉酮等。作为酰胺类，可以使用甲酰胺、N-甲基甲酰胺、N,N-二甲基甲酰胺等。作为胺类，可以使用单乙醇胺、二乙醇胺、三乙醇胺、三丙胺、三丁胺等。作为饱和烃，例如可以使用庚烷、辛烷、壬烷、癸烷、十一烷、十二烷、十三烷、十四烷、十五烷、十六烷等。
本发明中，在第1被接合材与第2被接合材之间借助临时固定用组合物将两者临时固定、将被临时固定的两者接合，由此制造接合结构体。临时固定用组合物的成分优选通过为了形成烧结前体而使用的糊剂中含有的有机溶剂的种类、与附着于该糊剂中含有的金属微粒的表面的表面处理剂的种类的关系来选择。
临时固定用组合物优选含有25℃下的粘度小于70mPa·s并且沸点为200℃以下的有机化合物(以下将该有机成分称为“第1有机成分”)、和25℃下的粘度为70mPa·s以上并且沸点为210℃以上的有机化合物(以下将该有机成分称为“第2有机成分”)。
本发明中，前述临时固定用组合物中含有的第1有机成分优选为25℃下前述糊剂的干燥体、即前述烧结前体的形态不会变化的成分、更优选所有有机成分为25℃下前述干燥体的形态不会变化的成分。通过这种有机成分含有于临时固定用组合物中，从而在第1被接合材与第2被接合材之间借助临时固定用组合物将两者临时固定时，烧结前体不易变质，可以将两被接合材可靠地临时固定。
本发明中所称的“干燥体的形态不会变化”指的是在干燥体上滴加1μl的有机成分，在110℃以下的条件下干燥的情况下用显微镜以倍率140倍观察时，在滴加前后干燥体没有发现变化。“没有发现变化”指的是，除了在滴加前后干燥体完全没有观察到变化之外，还包含即使在接合后的超声波探伤图像中也没有发现滴加的痕迹。
另外，优选构成临时固定用组合物的第1有机成分是对于前述糊剂中含有的前述有机溶剂和/或前述糊剂中含有的前述金属微粒的表面处理剂为难溶性的液态成分。液态成分指的是25℃下为液体的成分。若定量地表示液态成分的难溶性的程度则该液态成分优选的是，在25℃下将第1有机成分9g、与前述有机溶剂1g、前述调节剂1g或前述表面处理剂1g混合时，在两者之间观察到液-液界面、或在混合液中观察到析出物。通过这种液态成分含有于临时固定用组合物中，借助临时固定用组合物使第1被接合材和第2被接合材接触而进行临时固定的情况下，第1被接合材和/或第2被接合材的特性不易被临时固定用组合物影响。特别是第1被接合材和/或第2被接合材为烧结前体的情况下，该烧结前体的特性不易被临时固定用组合物影响。其结果，能够可靠地进行第1被接合材和第2被接合材的临时固定，并且将被接合材彼此可靠地接合。
构成临时固定用组合物的第1有机成分优选为观察到上述液-液界面、或观察到析出物的成分，更优选所有有机成分为观察到上述液-液界面、或观察到析出物的成分。
本发明中所称的“在两者之间观察到液-液界面”指的是在25℃下将前述液态成分9g、与前述有机溶剂1g、调节剂1g或前述表面处理剂1g加入到试管，利用试管混合机混合10分钟后，在25℃下静置5分钟时，两者分离而观察到两者的界面。
另外，本发明中所称的“在混合液中观察到析出物”指的是同样地在25℃下将前述液态成分9g、与前述有机溶剂1g、调节剂1g或前述表面处理剂1g加入到试管，利用试管混合机混合10分钟后，在25℃下静置5分钟时，两者中的一者的析出物在另一者的液相中被观察到。
临时固定用组合物中含有的第1有机成分为在将第1被接合材和第2被接合材临时固定的情况下，这些被接合材不易变质并且在两被接合材为临时固定状态期间能够容易地挥发的物质。
第1有机成分进一步优选25℃下的粘度为50mPa·s以下、进一步优选40mPa·s以下。另外，第1有机成分进一步优选其沸点为195℃以下、进一步优选190℃以下。
粘度为根据利用流变仪设想的粘度而适当变更所适用的传感器(平行板等)并测定得到的100/s的值(以下称为“粘度”时指的是利用该方法测定得到的值)。
从能够可靠地维持第1被接合材和第2被接合材的临时固定状态的观点、以及在临时固定状态下第1被接合材和第2被接合材不易变质的观点考虑，优选第1有机成分在临时固定用组合物中含有1质量％以上且70质量％以下。从这种观点考虑，第1有机成分在临时固定用组合物中更优选含有1质量％以上且70质量％以下、进一步优选含有1质量％以上且50质量％以下、更进一步优选含有1质量％以上且30质量％以下。
作为第1有机成分，如上所述只要前述烧结前体的形态不会变化即可，可列举出一元醇、多元醇、多元醇烷基醚、多元醇烯丙基醚、酯类、含氮杂环化合物、酰胺类、胺类、饱和烃、萜醇类、酮类、羧酸类等与作为上述有机溶剂列举出的例子相同的例子。这些有机成分可以单独使用一种或组合两种以上来使用。
临时固定用组合物中，优选除了第1有机成分之外，还含有种类与第1有机成分不同的第2有机成分。第2有机成分优选为粘合性高的化合物。具体而言，第2有机成分优选为如下的成分：在第1被接合材和第2被接合材被临时固定的状态下，即使从临时固定用组合物中将第1有机成分挥发而去除后，也会残留于第1被接合材与第2被接合材之间，且通过粘合性而能够维持两被接合材的临时固定状态。从这种优点进一步显著的观点考虑，第2有机成分进一步优选25℃下的粘度为70mPa·s以上、粘度也可以无限大。也就是说，第2有机成分在25℃下可以为固体。另外，第2有机成分优选其沸点为210℃以上、进一步优选220℃以上。
第2有机成分优选为如下的成分：在通过加热将第1被接合材和第2被接合材接合时能够通过热来去除。“能够通过热来去除”包含通过热而挥发来去除的情况、通过热而分解来去除的情况。从这种观点考虑，第2有机成分优选为分子量比较低的单体。具体而言，优选分子量为1000以下、更优选800以下、进一步优选600以下。
从能够可靠地维持第1被接合材和第2被接合材的临时固定状态的观点考虑，优选第2有机成分在临时固定用组合物中含有30质量％以上且99质量％以下。从同样的观点考虑，第2有机成分更优选在临时固定用组合物中含有50质量％以上且99质量％以下。
第1有机成分与第2有机成分的质量比率优选为1:99～70:30、更优选3:97～60:40、进一步优选5:95～50:50。
作为第2有机成分，可以使用与作为第1有机成分列举出的例子相同的例子。它们之中，特别是优选使用甘油(沸点290℃)、1,2,4-丁三醇(沸点312℃)、4-(1’-乙酰氧基-1’-甲基乙基)-环己醇乙酸酯(沸点223℃)、异冰片基环己醇(沸点313℃)等。另外，作为25℃下为固体的例子，例如优选使用龙脑(沸点213℃)、2,4,6-三异丙基-1,3,5-三聚甲醛(沸点244℃)、三羟甲基丙烷(沸点295℃)、肉豆蔻醇(沸点超过260℃)、2,4-二乙基-1,5-戊二醇(沸点264℃)等。这些化合物可以单独使用一种或组合两种以上来使用。
临时固定用组合物是为了直至将第1被接合材和第2被接合材通过烧结而完全固定为止期间的临时固定而使用的，因此烧结后尽可能不会残留于两被接合材之间，从不会对于接合结构体造成意外的不良影响的观点考虑优选。从这种观点考虑，临时固定用组合物优选的是，在氮气流通下由25℃以升温速度2℃/分钟升温至40℃并保持20分钟后，在升温速度10℃/分钟、氮气气氛下(例如氮气流通下)、试样质量30mg的条件下进行热重差热分析时的95％失重温度低于300℃、更优选290℃以下、进一步优选270℃以下。
临时固定用组合物除了上述第1有机成分和第2有机成分之外，在不会阻碍本发明效果的范围内可以含有其它成分。临时固定用组合物中的这些其它成分的比率优选它们的总量相对于临时固定用组合物为5质量％以下、进一步优选3质量％以下。
临时固定用组合物优选实质上不含有有机高分子化合物。有机高分子化合物通常为不挥发性或不易挥发的物质，因此若有机高分子化合物含有于临时固定用组合物中，则在将第1被接合材和第2被接合材通过烧结而完全固定后，有可能在两被接合材之间残留有机高分子化合物或源自其的化合物。这种化合物有可能对于接合结构体造成意外的不良影响。从这种观点考虑，临时固定用组合物优选不含有有机高分子化合物。从同样的观点考虑，临时固定用组合物也优选实质上不含有无机化合物。“实质上不含有有机高分子化合物”指的是临时固定用组合物没有有意地含有有机高分子化合物，但是容许在临时固定用组合物中不可避免地混入有机高分子化合物。“实质上不含有无机化合物”也是同样的意思。
作为前述有机高分子化合物，可列举出例如聚乙烯、聚丙烯和乙烯-α-烯烃共聚物等聚烯烃；聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯等聚酯；聚氯乙烯和聚苯乙烯等乙烯基聚合物；聚(甲基)丙烯酸和聚(甲基)丙烯酸烷基酯等(甲基)丙烯酸类聚合物；聚乙二醇、萜烯聚合物、萜烯苯酚聚合物等萜烯聚合物；聚碳酸酯、聚醚砜等。
接着对于本发明的临时固定用组合物的使用方法进行说明。
图1的(a)～(d)示意性地示出使用临时固定用组合物将第1被接合材和第2被接合材接合的工序。首先如图1的(a)所示，在基板10上涂布含有金属微粒和有机溶剂的糊剂而形成涂膜，从该涂膜去除有机溶剂，形成作为该糊剂的干燥体的烧结前体、即第2被接合材11。图1的(a)中示出在一张基板10的表面上形成作为第2被接合材11的一个烧结前体的状态。作为基板10，可列举出例如铜、银、镍、金、铝等金属、或氧化铝、碳化硅、氮化硅、氮化铝等陶瓷。另外，在该金属、陶瓷上，可以在单面或两面形成铜、银、镍、金、铝等金属镀层、金属图案。
接着如图1的(b)所示，对于第2被接合材11的表面赋予临时固定用组合物12。对于临时固定用组合物12的赋予而言，如该图所示可以仅对于第2被接合材11的一部分(例如烧结前体11的角部)进行、或对于第2被接合材11的整个区域进行。临时固定用组合物12的赋予可以采用公知的方法，例如分配、针转印、喷墨、丝网印刷等。
接着如图1的(c)所示，在第2被接合材11上重叠第1被接合材13。第1被接合材13与第2被接合材11的对置面由金属构成。通过这种重叠，在两被接合材11、13之间夹设临时固定用组合物12。临时固定用组合物12中优选不含有使作为第2被接合材11的烧结前体的形态变化的成分，因此第2被接合材11稳定地保持其形状。另外，临时固定用组合物12中优选含有粘合性高的成分，因此两被接合材11、13的临时固定状态被稳定地保持。
接着，对被临时固定的两被接合材11、13进行加热。通过加热，第2被接合材11、即烧结前体中含有的金属微粒烧结，从而两被接合材11、13接合。该工序如图1的(d)所示。加热通常利用加热炉(未图示)进行，因此图1的(c)所示的被临时固定的两被接合材11、13，通过搬送装置(未图示)，由该图所示的步骤被搬送到加热步骤。两被接合材11、13被临时固定用组合物12可靠地临时固定，因此，可以有效地防止搬送中在两被接合材11、13之间产生位置偏移。其结果，在加热炉中，两被接合材11、13在当初的接合预定位置处被可靠地接合。
将两被接合材11、13加热时，有时使用加压构件14进行加压，特别是第1被接合材13为半导体功率器件的情况下，需要提高第1被接合材13和第2被接合材11的接合可靠性，因此为了形成致密的烧结结构，有时使用加压构件14。若使用加压构件14则在被临时固定的状态的两被接合材11、13之间容易产生位置偏移，但是若使用本发明的临时固定用组合物12将两被接合材11、13临时固定，则即使通过加压构件14对两被接合材11、13进行加压的情况下，也不易在两被接合材11、13之间产生位置偏移。
从可靠地进行两被接合材11、13的接合观点考虑，加热时的利用加压构件14进行的加压优选为1MPa以上且40MPa以下。加热温度优选为200℃以上且300℃以下。通过在该温度下加热，可以使作为第2被接合材11的烧结前体中的金属微粒可靠地烧结，另外，通过热可以将临时固定用组合物12去除。焙烧气氛也可以使用大气等含氧气氛、氮气等非活性气氛、和含氢气氛中的任意一种。
如以上所述，根据本发明，也提供：一种组合物在将第1被接合材与第2被接合材接合之前将两者临时固定中的应用，所述组合物包含25℃下的粘度小于70mPa·s并且沸点为200℃以下的第1有机成分、和25℃下的粘度为70mPa·s以上并且沸点为210℃以上的第2有机成分。
实施例
以下通过实施例对于本发明进行更详细说明。但是本发明的范围不被上述实施例限制。只要没有特别说明则“％”指的是“质量％”。
[实施例1]
(1)临时固定用组合物的制造
作为第1有机成分，使用癸烷(25℃下的粘度0.7mPa·s、沸点174℃)。作为第2有机成分，使用2,4,6-三异丙基-1,3,5-三聚甲醛(25℃下固体、沸点244℃)。将两者混合而制造临时固定用组合物。临时固定用组合物中的第1有机成分的浓度为70％、第2有机成分的浓度为30％。该临时固定用组合物中不含有有机高分子化合物和无机化合物。
＜临时固定用组合物的失重温度的确认＞
对于临时固定用组合物，在氮气流通下以升温速度2℃/分钟升温至40℃并保持20分钟后，在升温速度10℃/分钟、氮气流通下、试样质量30mg的条件下，利用Bruker AXS公司制的差热·热重同时测定装置TG-DTA2000SA进行热重差热分析时的95％失重温度为152℃。
(2)接合用糊剂的制造
将利用湿式法合成的两种铜颗粒(球状、DSEM50＝0.14μm；薄片状DSEM50＝4.7μm)、作为有机溶剂的己二醇及PEG300、和固体还原剂等其它调节剂混合而制造接合用糊剂。作为固体还原剂，使用双(2-羟基乙基)亚氨基三(羟基甲基)甲烷(以下也称为“BIS-TRIS”)。
接合用糊剂中的铜颗粒的比率为74％、己二醇的比率为23.4％、PEG300的比率为0.74％。另外，球状颗粒在铜颗粒中所占的比率为30％、薄片状颗粒的比率为70％。另外，作为固体还原剂使用的BIS-TRIS的比率为1.85％。
＜干燥体的形态变化确认＞
在由无氧铜形成的基板上通过丝网印刷而涂布接合用糊剂，形成具有1cm×1cm的尺寸的矩形的涂膜。将该涂膜在110℃下干燥20分钟而去除有机溶剂，由此形成干燥体。然后，在干燥体滴加作为实施例1的第1有机成分的癸烷1μl，直接利用显微镜以倍率140倍确认状态，结果在癸烷滴加前后没有发现干燥体的形态变化。
在25℃下将作为临时固定用组合物中的第1有机成分的癸烷9g与作为接合用糊剂中含有的有机溶剂的PEG300 1g混合并静置，结果两者发生相分离，从而观察到两者的液-液界面。
在25℃下将作为临时固定用组合物中的第1有机成分的癸烷9g与作为接合用糊剂中含有的固体还原剂的BIS-TRIS 1g混合并静置，结果两者发生相分离，从而观察到两者的固-液界面。
(3)由烧结前体形成的第2被接合材的形成
在由铜板(20mm×20mm、厚度0.5mm)形成的基板上通过丝网印刷而涂布接合用糊剂，形成具有0.6cm×0.6cm的尺寸的矩形的涂膜。将该涂膜在110℃下干燥20分钟去除有机溶剂，由此形成由作为干燥体的烧结前体形成的第2被接合材。
(4)第1被接合材的重叠
作为半导体功率器件的模型构件，准备镀Ag的氧化铝芯片(0.5cm×0.5cm、厚度0.5mm)。使用该氧化铝芯片作为第1被接合材。在(3)中形成的烧结前体的整面滴加数滴的临时固定用组合物，接着在烧结前体上重叠氧化铝芯片，施加0.8MPa、2秒的载荷。
＜粘性的评价＞
重叠氧化铝芯片后，以前述铜板和氧化铝芯片的接合面朝向铅直方向的方式竖立接合体，然后恢复水平作为1次操作，每隔10分钟实施总计6次这种操作。在6次操作中的任意一次中，氧化铝芯片都不会由铜板脱落，粘性得到确保。
[实施例2]
替代作为实施例1的(1)临时固定用组合物的制造中使用的第2有机成分的2,4,6-三异丙基-1,3,5-三聚甲醛，使用4-(1’-乙酰氧基-1’-甲基乙基)-环己醇乙酸酯(25℃下液体、25℃下的粘度77mPa·s、沸点223℃)，与作为第1有机成分的癸烷的质量比设为1:99来制作临时固定用组合物。除此之外直至实施例1的(4)第1被接合材的重叠为止与实施例1同样地制作。
对于实施例2中制作的基板，进行上述粘性的评价，结果即使60分钟后氧化铝芯片也没有脱落，因此可知粘性得到确保。进而进行接合评价，结果芯片的位置没有产生偏移。
对于临时固定用组合物，在与实施例1同样的条件下进行热重差热分析时的95％失重温度为233℃。
[比较例1]
不使用作为实施例1的(1)临时固定用组合物的制造中使用的第2有机成分的2,4,6-三异丙基-1,3,5-三聚甲醛，来制作临时固定用组合物。除此之外直至实施例1的(4)第1被接合材的重叠为止与实施例1同样地制作。对于所制作的基板，进行上述粘性的评价，结果20分钟后氧化铝芯片脱落，因此可知粘性没有得到确保。
[比较例2]
替代作为实施例1的(1)临时固定用组合物的制造中使用的第2有机成分的2,4,6-三异丙基-1,3,5-三聚甲醛，使用樟脑(25℃下固体、沸点204℃)来制作临时固定用组合物。除此之外直至实施例1的(4)第1被接合材的重叠为止与实施例1同样地制作。对于所制作的基板，进行上述粘性的评价，结果20分钟后氧化铝芯片脱落，因此可知粘性没有得到确保。
产业上的可利用性
根据本发明，通过接合材料将被接合材彼此接合时，可以使该接合材料的特性尽可能不会变化地将被接合材彼此临时固定。

Claims (9)

1.一种临时固定用组合物，其包含25℃下的粘度小于70mPa·s并且沸点为200℃以下的第1有机成分、和
25℃下的粘度为70mPa·s以上并且沸点为210℃以上的第2有机成分，
所述临时固定用组合物用于在将第1被接合材与第2被接合材接合之前将两者临时固定。
2.根据权利要求1所述的临时固定用组合物，其中，所述第1有机成分在25℃下不改变第2被接合材的形态。
3.根据权利要求1或2所述的临时固定用组合物，其中，第1被接合材和第2被接合材中的至少一者为含有金属微粒、有机溶剂和调节剂的糊剂的干燥体，
在25℃下将所述临时固定用组合物中的第1有机成分9g、与所述有机溶剂1g、附着于所述金属微粒的表面处理剂1g或所述调节剂1g混合时，在两者之间观察到液-液界面或在混合液中观察到析出物。
4.根据权利要求1或2所述的临时固定用组合物，其中，第1有机成分与第2有机成分的质量比率为1:99～70:30。
5.根据权利要求1或2所述的临时固定用组合物，其中，在升温速度10℃/分钟、氮气气氛、试样质量30mg的条件下进行热重差热分析时的95％失重温度低于300℃。
6.根据权利要求1或2所述的临时固定用组合物，其实质上不含有有机高分子化合物。
7.一种接合结构体的制造方法，其包括如下工序：
在第1被接合材与第2被接合材之间借助临时固定用组合物将两者临时固定，
对被临时固定的两者进行焙烧，将两者接合，
作为所述临时固定用组合物，使用包含25℃下的粘度小于70mPa·s并且沸点为200℃以下的第1有机成分、和25℃下的粘度为70mPa·s以上并且沸点为210℃以上的第2有机成分的临时固定用组合物。
8.根据权利要求7所述的制造方法，其中，第1被接合材和第2被接合材中的至少一者由作为含有金属微粒和有机溶剂的糊剂的干燥体的烧结前体形成。
9.一种组合物在将第1被接合材与第2被接合材接合之前将两者临时固定中的应用，所述组合物包含25℃下的粘度小于70mPa·s并且沸点为200℃以下的第1有机成分、和25℃下的粘度为70mPa·s以上并且沸点为210℃以上的第2有机成分。
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