CN107001895B - 粘合剂组合物、包含其固化物的半导体器件及使用其的半导体器件的制造方法 - Google Patents

粘合剂组合物、包含其固化物的半导体器件及使用其的半导体器件的制造方法 Download PDF

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CN107001895B
CN107001895B CN201580064713.7A CN201580064713A CN107001895B CN 107001895 B CN107001895 B CN 107001895B CN 201580064713 A CN201580064713 A CN 201580064713A CN 107001895 B CN107001895 B CN 107001895B
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adhesive composition
semiconductor devices
grain diameter
film
average grain
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CN107001895A (zh
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松村和行
藤丸浩一
金森大典
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Toray Industries Inc
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Toray Industries Inc
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Abstract

本发明的目的在于提供能够进行对准标记的识别、充分地确保接合部的焊料润湿性、且在抑制空隙产生方面效果优异的粘合剂组合物，本发明为粘合剂组合物，其特征在于，含有：(A)高分子化合物；(B)重均分子量为100以上且3,000以下的环氧化合物；(C)助焊剂；及(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子，其中，(C)助焊剂含有酸改性松香。

Description

粘合剂组合物、包含其固化物的半导体器件及使用其的半导 体器件的制造方法
技术领域
本发明涉及在将半导体芯片与电路基板电接合或粘合时、将半导体芯片彼此接合或层合时使用的粘合剂组合物、包含其固化物的半导体器件及使用其的半导体器件的制造方法。
背景技术
近年来，随着半导体器件的小型化和高密度化，作为将半导体芯片封装于电路基板的方法，倒装芯片封装备受瞩目，并且迅速得到推广。倒装芯片封装中，半导体芯片的粘合采用了下述通常的方法：使环氧树脂系粘合剂介于形成在半导体芯片上的凸块电极(bump electrode)与电路基板的焊盘电极(pad electrode)之间。
在凸块电极上具有焊料的倒装芯片封装中，为了除去存在于焊料表面、电极表面的氧化膜，提出了具有助焊剂(flux)功能的粘合剂(例如，参见专利文献1及2)。
另外，在倒装芯片封装中，要求隔着粘合剂组合物对形成于基板、芯片上的对准(alignment)标记进行识别。即，对于粘合剂组合物而言，透明性是必须的。然而，欲使用上述那样的粘合剂组合物来制作半导体器件时，存在下述情况：透明性不足而无法识别对准标记；或由于助焊性不足而导致封装后的接合部的焊料润湿性不良；或封装后在半导体器件内残留有空隙。
现有技术文献
专利文献
专利文献1：日本特开2013-173834号公报
专利文献2：国际公开第2014/103637号
发明内容
发明所要解决的课题
鉴于上述情况，本发明的目的在于，提供能够进行对准标记的识别、充分地确保接合部的焊料润湿性、且在抑制空隙产生方面效果优异的粘合剂组合物。
用于解决课题的手段
即，本发明为粘合剂组合物，其特征在于，含有：(A)高分子化合物；(B)重均分子量为100以上且3,000以下的环氧化合物；(C)助焊剂；及(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子，其中，(C)助焊剂含有酸改性松香。
发明的效果
根据本发明，可得到能够进行对准标记的识别、充分地确保接合部的焊料润湿性、且在抑制空隙产生方面效果优异的粘合剂组合物。
附图说明
图1是表示使用本发明的粘合剂组合物制作的半导体器件的接合部的焊料润湿性的示意图。
具体实施方式
本发明的粘合剂组合物的特征在于，其含有：(A)高分子化合物；(B)重均分子量为100以上且3,000以下的环氧化合物；(C)助焊剂；及(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子，其中，(C)助焊剂含有酸改性松香。
对于本发明的粘合剂组合物而言，通过含有(A)高分子化合物，从而在制成膜状时的制膜性优异。所谓高分子化合物，是指以重均分子量计为5,000以上且500,000以下的化合物。
作为(A)高分子化合物，可举出丙烯酸树脂、苯氧基树脂、聚酯树脂、聚氨酯树脂、聚酰亚胺树脂、硅氧烷改性聚酰亚胺树脂、聚苯并噁唑树脂、聚酰胺树脂、聚碳酸酯树脂、聚丁二烯等，但不限于此。可将这些中的2种以上组合。这些之中，从(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子的分散性良好、并且制成膜时膜的透明性高、对准标记的识别变得容易的方面考虑，优选苯氧基树脂。另外，从抑制封装后的空隙的观点考虑，优选聚酰亚胺树脂。
作为(A)高分子化合物的重均分子量的下限，优选为10,000以上，更优选为30,000以上。另外，重均分子量的上限优选为100,000以下，更优选为80,000以下。含有2种以上(A)高分子化合物的情况下，其中的至少1种的重均分子量为上述范围即可。若重均分子量为10,000以上，则固化膜的机械强度提高，热循环试验中的裂纹产生等被抑制，能够得到可靠性高的半导体器件。另一方面，若重均分子量为100,000以下，则粘合剂组合物的流动性升高，封装后的接合部的焊料润湿性提高。需要说明的是，本发明中的(A)高分子化合物的重均分子量是利用凝胶渗透色谱法(GPC法)进行测定、并以聚苯乙烯换算而算出的。
本发明的粘合剂组合物含有(B)重均分子量为100以上且3,000以下的环氧化合物。环氧化合物一般通过不伴有收缩的开环反应而进行固化，因此，能够减少粘合剂组合物在固化时的收缩。另外，通过使重均分子量为100以上且3,000以下，环氧化合物的反应性高，结果固化速度加快，能够抑制封装后的空隙。作为(B)重均分子量为100以上且3,000以下的环氧化合物，优选为具有2个以上环氧基的环氧化合物、环氧当量为100～500的环氧化合物。通过使环氧当量为100以上，能够提高固化后的粘合剂组合物的韧性。通过使环氧当量为500以下，固化后的粘合剂组合物的交联密度升高，能够提高耐热性。需要说明的是，与(A)高分子化合物的重均分子量同样地，本发明中的(B)重均分子量为100以上且3,000以下的环氧化合物的重均分子量是利用凝胶渗透色谱法(GPC法)进行测定、并以聚苯乙烯换算而算出的。
另外，(B)重均分子量为100以上且3,000以下的环氧化合物优选含有液态环氧化合物和固态环氧化合物这两者。通过含有液态环氧化合物，能够在将粘合剂组合物制成膜状时抑制膜的裂纹。通过含有固态环氧化合物，能够抑制封装后的空隙的产生。
此处，液态环氧化合物是指在25℃、1.013×105N/m2下呈现150Pa·s以下的粘度的环氧化合物，固态环氧化合物是指于25℃呈现大于150Pa·s的粘度的环氧化合物。作为液态环氧化合物，可举出例如jER(注册商标)YL980、jER(注册商标)YL983U、jER(注册商标)152、jER(注册商标)630、jER(注册商标)YX8000(以上为商品名，三菱化学(株)制)、EPICLON(注册商标)HP-4032(以上为商品名，DIC(株)制)等，但不限于此。可将这些中的2种以上组合。另外，作为固态环氧化合物，可举出jER(注册商标)1002、jER(注册商标)1001、jER(注册商标)YX4000H、jER(注册商标)4004P、jER(注册商标)5050、jER(注册商标)154、jER(注册商标)157S70、jER(注册商标)180S70、jER(注册商标)1032H60(以上为商品名，三菱化学(株)制)、TEPIC(注册商标)S(以上为商品名，日产化学工业(株)制)、EPOTOTE(注册商标)YH-434L(商品名，新日铁化学(株)制)、EPPN502H、NC3000(以上为商品名，日本化药(株)制)、EPICLON(注册商标)N695、EPICLON(注册商标)N865、EPICLON(注册商标)HP-7200、EPICLON(注册商标)HP-4700(以上为商品名，DIC(株)制)等，但不限于此。可将这些中的2种以上组合。
另外，作为(B)重均分子量为100以上且3,000以下的环氧化合物的含量，从充分地呈现粘合力、提高封装后的半导体器件的连接可靠性的方面考虑，相对于100质量份的(A)高分子化合物而言，优选为50质量份以上，更优选为100质量份以上。另一方面，从接合部的焊料润湿性提高的方面考虑，优选为500质量份以下，更优选为300质量份以下。
本发明的粘合剂组合物的特征在于含有(C)助焊剂，其中，(C)助焊剂含有酸改性松香。(C)助焊剂是除去金属表面的氧化物、提高焊料的润湿性的化合物。酸改性松香是使脂松香、木松香、浮油松香(tall rosin)等原料松香类与(甲基)丙烯酸、马来酸(酐)、富马酸、柠康酸(酐)、衣康酸(酐)等不饱和羧酸进行迪尔斯-阿尔德反应(Diels-Alderreaction)(加成反应)而得到的。对于原料松香而言，优选使用为了除去金属等杂质及改善树脂色调而利用蒸馏、重结晶、萃取等进行了纯化的松香。另外，对于酸改性松香而言，可以通过氢化而制成透明色调的酸改性松香。作为这样的酸改性松香，可举出PINECRYSTAL(注册商标)KE-604、PINECRYSTAL(注册商标)KR-120、MALKYD(注册商标)No.33(以上为商品名，荒川化学工业(株)制)。这些酸改性松香含有2个以上的羧基。因此，酸改性松香与环氧化合物反应，形成高密度的网状结构，从而能够提高耐热性。需要说明的是，酸改性松香具有该化合物自身的大体积结构和经酸改性而生成的大体积环结构，这会给环氧基对羧基的反应造成立体阻碍，粘合剂组合物于室温下的保存性提高。另一方面，在焊料熔点附近即200℃至250℃的温度下，酸改性松香的分子运动性提高，可除去焊料表面、接合金属表面的氧化被膜，接合部的焊料润湿性提高。
从提高粘合剂组合物于室温下的保存稳定性的观点、抑制封装后的空隙的观点考虑，(C)助焊剂中的酸改性松香的含量优选为50质量％以上，进一步优选为90质量％以上，更优选为95质量％以上。另外，作为上限，为100质量％(助焊剂全部为酸改性松香)。
从焊料的润湿性提高的方面考虑，相对于100质量份的(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子而言，粘合剂组合物中的(C)助焊剂中的酸改性松香的含量优选为5质量份以上，更优选为10质量份以上，进一步优选为15质量份以上。另一方面，从抑制封装后的空隙的方面考虑，相对于100质量份的(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子而言，(C)助焊剂的含量优选为35质量份以下，更优选为30质量份以下，进一步优选为25质量份以下。
本发明的粘合剂组合物含有(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子。如上述那样地在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm时，无机粒子向粘合剂树脂组合物中的分散性优异，结果可确保粘合剂组合物的透明性，能够进行对准标记的识别。此外，由于该无机粒子的分散性优异，因此能够将无机粒子高浓度地填充至粘合剂组合物中，在制成粘合剂组合物时能够抑制封装后空隙的产生，进而能够降低制成固化物时的线性膨胀系数，提高半导体器件的连接可靠性。另外，作为(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子的平均粒径的下限，优选为50nm以上，更优选为75nm以上。另外，作为(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子的平均粒径的上限，优选为175nm以下，更优选为150nm以下。
作为在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子，可举出利用苯基硅烷偶联剂进行表面处理而得到的无机粒子、例如Sciqas 0.15μm苯基硅烷处理、Sciqas 0.1μm苯基硅烷处理、Sciqas 0.05μm苯基硅烷处理(以上为商品名，堺化学工业(株)制)、YA050C(商品名，(株)Admatechs制)。
需要说明的是，所谓无机粒子的平均粒径，表示无机粒子单独存在时的粒径，是指观察到的粒径的平均值。形状为球状的情况下，表示其直径，为椭圆状及扁平状的情况下，表示形状的最大长度。此外，为棒状或纤维状的情况下，表示长度方向的最大长度。作为测定粘合剂组合物中的无机粒子的平均粒径的方法，可利用下述方法来测定：利用SEM(扫描电子显微镜)直接观察粒子，并计算100个粒子的平均粒径。
作为用于(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子中的无机粒子，例如，可举出滑石、烧结粘土、未烧结粘土、云母、玻璃等硅酸盐；氧化钛、氧化铝、二氧化硅等氧化物；碳酸钙、碳酸镁等碳酸盐；氢氧化铝、氢氧化镁、氢氧化钙等氢氧化物；硫酸钡、硫酸钙、亚硫酸钙等硫酸盐或亚硫酸盐；硼酸锌、偏硼酸钡、硼酸铝、硼酸钙、硼酸钠等硼酸盐；氮化铝、氮化硼、氮化硅等氮化物等。这些无机粒子可含有多种，但从可靠性及成本的方面考虑，优选二氧化硅或氧化钛。
相对于除溶剂外的粘合剂组合物的有机物总量而言，(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子的含量优选为45质量份以上，更优选为50质量份以上。为45质量份以上时，在制成粘合剂组合物时能够抑制封装后的空隙的产生，进而能够降低制成固化物时的线性膨胀系数，提高半导体器件的连接可靠性。另外，从无机粒子彼此的凝集被抑制、粘合剂组合物的流动性良好、封装后的接合部的焊料润湿性提高的方面考虑，优选为70质量％以下，更优选为65质量份以下。
(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子的形状可以为球状、椭圆状、扁平状、棒状、纤维状等非球状中的任一种，球状的无机粒子由于容易在碱溶性粘合剂膜中均匀分散，因此可优选使用。
本发明的粘合剂组合物优选含有(E)固化促进剂。固化促进剂不溶解地存在于粘合剂组合物中时，环氧化合物的固化反应变慢，于室温下的保存性提高，从上述观点考虑，(E)固化促进剂优选为固化促进剂粒子。另外，若使用咪唑系固化促进剂粒子作为固化促进剂粒子，则环氧树脂的固化速度快，能够抑制封装后的空隙，故而优选。作为这样的固化促进剂粒子，优选使用Curezol(注册商标)2PZCNS、Curezol(注册商标)2PZCNS-PW、Curezol(注册商标)C11Z-CNS、Curezol(注册商标)2MZ-A、Curezol(注册商标)C11-A、Curezol(注册商标)2E4MZ-A、Curezol(注册商标)2MZA-PW、Curezol(注册商标)2MAOK-PW、Curezol(注册商标)2PHZ-PW(以上为商品名，四国化成工业(株)制)等。
作为固化促进剂粒子的平均粒径的下限，优选为0.1μm以上，更优选为0.15μm以上。另外，作为平均粒径的上限，优选为2μm以下，更优选为1μm以下。此处，所谓平均粒径，表示固化促进剂粒子单独存在时的平均粒径。固化促进剂粒子的形状为球状的情况下，表示其直径，为椭圆状及扁平状的情况下，表示形状的最大长度。此外，在形状为棒状或纤维状的情况下，表示长度方向的最大长度。作为测定平均粒径的方法，可利用下述方法来测定：利用SEM(扫描电子显微镜)直接观察粒子，并计算100个粒子的平均粒径。若平均粒径为0.1μm以上，则粘合剂膜的分散性良好，制成膜时膜的透明性高，对准标记的识别变得容易。若平均粒径为2μm以下，则固化促进剂的比表面积变大，环氧化合物的固化反应容易进行，粘合剂组合物中含有的固化促进剂的量减少，从而能够抑制封装后的空隙的产生。
另外，作为(E)固化促进剂的含量，从使环氧化合物的固化反应进行、呈现充分的粘合力、提高封装后的半导体器件的连接可靠性的观点考虑，相对于100质量份的(B)重均分子量为100以上且3,000以下的环氧化合物而言，优选为1质量份以上，更优选为3质量份以上。另一方面，从固化反应被抑制、于室温下的保存稳定性提高、结果接合部的焊料润湿性提高的观点考虑，相对于100质量份的(B)重均分子量为100以上且3,000以下的环氧化合物而言，(E)固化促进剂的含量优选为15质量份以下，更优选为10质量份以下。
本发明的粘合剂组合物还可含有离子捕获剂、表面活性剂、硅烷偶联剂、有机染料、无机颜料等。
对于本发明的粘合剂组合物而言，可将各构成材料在溶剂中制成清漆来使用，也可将该清漆涂布在剥离性基材上并进行脱溶剂、制成膜来使用。
作为溶剂，可将作为酮系溶剂的丙酮、甲基乙基酮、甲基异丁基酮、环戊酮、环己酮；作为醚系溶剂的1，4-二氧杂环己烷、四氢呋喃、二乙二醇二甲醚；作为二醇醚系溶剂的乙二醇单甲醚、乙二醇单乙醚、丙二醇单甲醚、丙二醇单乙醚、丙二醇单丁醚、二乙二醇甲乙醚；以及苯甲醇、N-甲基吡咯烷酮、γ-丁内酯、乙酸乙酯、N，N-二甲基甲酰胺等单独使用或混合2种以上而使用，但不限于此。
作为剥离性基材，可举出聚丙烯膜、聚对苯二甲酸乙二醇酯膜、聚萘二甲酸乙二醇酯膜、聚酯膜、聚氯乙烯膜、聚碳酸酯膜、聚酰亚胺膜、聚四氟乙烯膜等氟树脂膜、聚苯硫醚膜、聚丙烯膜、聚乙烯膜等，但不限于此。另外，可利用有机硅系脱模剂、长链烷基系脱模剂、氟系脱模剂、脂肪族酰胺系脱模剂等对剥离性基材实施脱模处理。剥离性基材的厚度没有特别限定，通常优选为5～75μm。另外，优选在粘合剂的与具有脱模性基材的面呈相反侧的面上进一步层压其他的剥离性基材，从而制成上下被剥离性基材夹持的粘合剂膜。作为其他的剥离性基材的材质及厚度，可使用与前文说明相同的材质及厚度。两片剥离性基材也可以相同。
另外，对于在溶剂中混合各构成材料而以清漆状得到的粘合剂组合物而言，也可以将其涂布在半导体晶片、电路基板等上并进行脱溶剂而使用。
本发明的粘合剂组合物可优选用作半导体用粘合剂组合物，所述半导体用粘合剂组合物用于半导体器件中使用的半导体元件、电路基板、金属布线材料等电路构件彼此的粘合或固定、用于半导体元件的密封。
本发明的半导体器件包含上述粘合剂组合物的固化物或上述粘合剂组合物膜的固化物。本发明中所谓的半导体器件，是指能够通过利用半导体元件的特性而发挥功能的所有装置。将半导体元件与基板连接而形成的器件、将半导体元件彼此或基板彼此连接而形成的器件、电光学装置、半导体电路基板及电子设备全部包含在半导体器件中。
本发明的半导体器件的制造方法的特征在于，使上述粘合剂组合物或上述粘合剂组合物膜介于第一电路构件与第二电路构件之间，利用加热加压将所述第一电路构件与所述第二电路构件电连接。
使用了本发明的粘合剂组合物的半导体器件的制造方法的一例如下。首先，准备具有第一连接端子的第一电路构件、和具有第二连接端子的第二电路构件。此处，所谓电路构件，可举出半导体芯片、电阻器芯片、电容器芯片等芯片部件、具有TSV(硅通孔，throughsilicon via)电极的半导体芯片、硅中介层(silicon interposer)、玻璃环氧树脂电路基板、膜电路基板等基板等。另外，作为连接端子，可举出电镀凸块(plated bump)、钉头凸块(stud bump)等凸块电极、焊盘电极等。另外，也可在第一电路构件及/或第二电路构件上形成贯通电极，在构件的一面及/或两面上形成连接端子。
将第一电路构件和第二电路构件以第一连接端子与第二连接端子相对的方式进行配置。接着，使本发明的粘合剂组合物介于上述相对配置的第一连接端子与第二连接端子之间。然后，对第一电路构件和第二电路构件进行加热加压，使上述相对配置的第一连接端子与第二连接端子电连接。通过该工序，第一电路构件与第二电路构件被牢固地电连接，并且，粘合剂发生固化，第一电路构件与第二电路构件被物理性地固定。
此处，可以先仅在任一个电路构件的连接端子侧的面上赋予粘合剂组合物，也可以在第一及第二电路构件的连接端子侧的两个面上赋予粘合剂组合物。
作为更详细的实施方式的例子，对制作半导体器件的方法进行说明，所述方法中，使用具有凸块的半导体芯片作为第一电路构件，使用具有布线图案的电路基板或半导体芯片作为第二电路构件，介由本发明的粘合剂组合物膜将二者连接，用粘合剂将第一电路构件与第二电路构件之间的空隙密封。
首先，将粘合剂组合物膜粘贴于作为第二电路构件的、形成有布线图案的电路基板或半导体芯片上。此时，粘合剂组合物膜可在切成规定的大小后，粘贴于形成有布线图案的电路基板的布线图案面或半导体芯片的凸块形成面上。另外，也可在半导体晶片的凸块形成面上粘贴粘合剂膜后，对半导体晶片进行切割(dicing)从而将其单片化，由此制作粘贴有粘合剂膜的半导体芯片。
接着，配置作为第一电路构件的半导体芯片，使第一电路构件的凸块与第二电路构件的布线图案相对，使用接合装置(bonding apparatus)对二者进行加热加压。加热加压条件只要在能够良好地获得电连接的范围内即可，没有特别限定，但为了进行粘合剂的固化，需要进行温度为100℃以上、压力为1mN/凸块以上、时间为0.1秒以上的加热加压。在下述接合(bonding)条件下进行：温度优选为120℃以上且300℃以下，更优选为150℃以上且250℃以下；压力优选为5mN/凸块以上且50000mN/凸块以下，更优选为10mN/凸块以上且10000mN/凸块以下；时间优选为1秒以上且60秒以下，更优选为2秒以上且30秒以下。另外，在接合时，作为临时压接，也可通过温度为50℃以上、压力为1mN/凸块以上、时间为0.1秒以上的加热加压，使半导体芯片上的凸块与电路基板上的布线图案接触后，在上述条件下进行接合。根据需要，也可在接合后将附有半导体芯片的电路基板在50℃以上且200℃以下的温度下加热10秒以上且24小时以下。
除此以外，本发明的粘合剂还可用作粘合性树脂材料，所述粘合性树脂材料用于制作芯片粘结膜(die attach film)、切割芯片粘结膜(dicing die attach film)、引线框固定胶带、散热板、增强板、屏蔽材料的粘合剂、阻焊剂等。
实施例
以下，基于实施例对本发明进行具体说明，但本发明不限于这些实施例。
＜高分子化合物、环氧化合物的重均分子量＞
将化合物溶解于N-甲基-2-吡咯烷酮(以下记为NMP)中配制浓度为0.1重量％的溶液，作为测定试样。使用如下所示构成的GPC装置Waters2690(Waters(株)制)，算出以聚苯乙烯换算的重均分子量。GPC测定条件如下：流动相为分别以0.05mol/L的浓度溶解有LiCl和磷酸的NMP，流量为0.4mL/分钟。另外，使用恒温柱箱(column oven)将色谱柱加热至40℃。
检测器：Waters996
系统控制器：Waters2690
色谱柱：TOSOH TSK-GELα-4000
色谱柱：TOSOH TSK-GELα-2500。
＜无机粒子的平均粒径＞
利用SEM(扫描电子显微镜，日本电子公司制JSM-6510A)观察100个粒子的粒径，将其平均值作为平均粒径。观察中，粒子以圆形被观察到的情况下，将其直径作为粒径；以椭圆等形状被观察到的情况下，将粒子的轮廓中距离最长的区间的长度作为粒径。
＜对准标记的识别＞
粘合剂组合物的对准标记的识别的评价如以下这样进行。从各实施例及比较例中制作的粘合剂膜剥离保护膜后，使用层压装置((株)名机制作所制，MVLP600)将该粘合剂组合物膜贴合于附有铜柱凸块的TEG芯片((株)WALTS制，WALTS-TEGCC80-0101JY)的铜柱凸块形成面上。接下来，将基材膜剥离，制作附有粘合剂组合物的评价芯片。制作10个该评价芯片。然后，利用倒装芯片接合装置(Toray Engineering(株)制，FC-3000WS)的相机，对芯片上的图案识别性进行评价。记录所制得的10个评价芯片中的能够进行自动识别的数量。
＜空隙的评价＞
如上述那样进行对准标记的识别评价后，对作为被粘物的基板((株)WALTS制，WALTS-KIT CC80-0102JY[MAP]-ModelI(Cu+OSP规格))实施倒装芯片接合。倒装芯片接合的条件如下：将基板置于被加热至140℃的接合台上，在温度为140℃、压力为150N/芯片、时间为1秒的条件下进行临时压接后，在温度为250℃、压力为150N的条件下进行正式压接(时间为5秒)。使用超声波影像装置(Hitachi Power Solutions Co.，Ltd.制，FS300III)对得到的半导体器件的空隙进行观察。在空隙的评价中，记录芯片面积中空隙占据的比例。需要说明的是，结果的下限设为1％以下，结果的上限设为10％以上。
＜接合部的焊料润湿性评价＞
如上述那样进行空隙的评价后，研磨半导体器件的截面而使接合部位露出。然后，用光学显微镜观察接合形状。如图1所示，将铜柱凸块100的焊料101润湿了基板的铜布线102的两个侧面的情况评价为A，将仅润湿单侧的情况评价为B，将任一个侧面均未润湿、但布线上润湿的情况评价为C，将任一个侧面均未润湿、且在布线上还存在粘合剂组合物103的啮入的情况评价为D(图1)。
各实施例及比较例中使用的(A)成分的聚酰亚胺是如以下这样合成的。
合成例1聚酰亚胺的合成
在干燥氮气流下，将4.82g(0.0165摩尔)1，3-双(3-氨基苯氧基)苯、3.08g(0.011摩尔)3，3’-二氨基-4，4’-二羟基二苯砜、4.97g(0.02摩尔)1，3-双(3-氨基丙基)四甲基二硅氧烷、及0.47g(0.005摩尔)作为封端剂的苯胺溶解于130g的NMP中。向其中与20g的NMP一同加入26.02g(0.05摩尔)2，2-双{4-(3，4-二羧基苯氧基)苯基)丙烷二酐，于25℃使其反应1小时，接着于50℃搅拌4小时。之后，于180℃搅拌5小时。搅拌结束后，将溶液投入3L水中，过滤并回收沉淀，用水清洗3次后，使用真空干燥机于80℃干燥20小时。测定得到的聚合物固体的红外吸收光谱，结果，在1780em-1附近、1377cm-1附近检测到来自聚酰亚胺的酰亚胺结构的吸收峰。另外，得到的聚酰亚胺的重均分子量为18000。
除此以外，各实施例及比较例中使用的(A)～(F)成分如下。
(A)成分
1256(商品名，苯氧基树脂，重均分子量为50000，三菱化学(株)制)
4250(商品名，苯氧基树脂，重均分子量为60000，三菱化学(株)制)
(B)成分
YL-980(商品名，液态环氧化合物，重均分子量为370，三菱化学(株)制)
N-865(商品名，固态环氧化合物，重均分子量为850，DIC(株)制)
1032H60(商品名，固态环氧化合物，重均分子量为525，三菱化学(株)制)
(C)成分
KR-120(商品名，酸改性松香100％，荒川化学工业(株)制)
(D)成分
Sciqas 0.15μm苯基硅烷处理(商品名，二氧化硅，平均粒径为150nm，苯基硅烷偶联表面处理、即在表面具有含苯基的烷氧基硅烷，堺化学工业(株)制)
YA050C(商品名，二氧化硅，平均粒径为50nm，苯基硅烷偶联表面处理、即在表面具有含苯基的烷氧基硅烷，(株)Admatechs制)
(E)成分
2MAOK-PW(商品名，咪唑系固化促进剂粒子，四国化成工业(株)制)
(F)其他
己二酸(助焊剂)
Sciqas 0.15μm(商品名，二氧化硅，平均粒径为150nm，未进行表面处理，堺化学工业(株)制)
实施例1～9及比较例1～3
(1)粘合剂组合物膜的制作方法
将表1所示的(A)～(F)成分按照表1中记载的组成比进行混合，制作粘合剂组合物清漆。作为有机溶剂，使用环己酮，将溶剂以外的添加物作为固态成分，制成固态成分浓度为53％的粘合剂组合物清漆。使用狭缝模式涂布机(涂布机)，将制作的粘合剂组合物清漆涂布在剥离性基材即厚度为38μm的聚对苯二甲酸乙二醇酯膜的表面处理面上，于100℃进行干燥10分钟。在由此得到的干燥后的厚度为30μm的粘合剂膜上贴合切割胶带(dicingtape)(T1902-90，聚烯烃基材，古河电气工业(株)制)的粘着面，得到由基材膜与保护膜夹持的结构的粘合剂组合物膜。此时，切割胶带作为基材膜而发挥功能，聚对苯二甲酸乙二醇酯膜作为保护膜而发挥功能。使用得到的粘合剂组合物膜，如上述那样实施对准标记的识别、空隙的评价、接合部的焊料润湿性评价。将结果示于表1。
产业上的可利用性
本发明的粘合剂组合物可用作用于个人电脑、移动终端中使用的电子部件或散热板与印刷基板或柔性基板的粘合、及基板彼此的粘合的粘合剂。此外，可优选用作在将IC、LSI等半导体芯片与柔性基板、玻璃环氧树脂基板、玻璃基板、陶瓷基板等电路基板粘合或直接电接合时使用的半导体用粘合剂。
附图标记说明
100：铜柱凸块
101：焊料
102：铜布线
103：粘合剂组合物

Claims (7)

1.粘合剂组合物，其特征在于，含有：
(A)高分子化合物、
(B)重均分子量为100以上且3,000以下的环氧化合物、
(C)助焊剂、及
(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子，
其中，所述(A)高分子化合物是重均分子量为10,000以上且100,000以下的苯氧基树脂，(C)助焊剂含有酸改性松香。
2.如权利要求1所述的粘合剂组合物，其中，所述(C)助焊剂中的酸改性松香的含量为50质量％以上且100质量％以下。
3.如权利要求1或2所述的粘合剂组合物，其中，相对于100质量份的所述(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子而言，所述(C)助焊剂中的酸改性松香的含量为5～35质量份。
4.如权利要求1或2所述的粘合剂组合物，所述粘合剂组合物还含有(E)固化促进剂。
5.如权利要求1或2所述的粘合剂组合物，其中，相对于粘合剂组合物的总量而言，所述(D)在表面具有含苯基的烷氧基硅烷、且平均粒径为30～200nm的无机粒子的含量为45～70质量％。
6.半导体器件，其包含权利要求1～5中任一项所述的粘合剂组合物的固化物。
7.半导体器件的制造方法，其中，使权利要求1～5中任一项所述的粘合剂组合物介于第一电路构件与第二电路构件之间，将所述第一电路构件与所述第二电路构件电连接。
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