CN109467941B - 树脂组合物、树脂膜、半导体层叠体、半导体层叠体的制造方法及半导体装置的制造方法 - Google Patents
树脂组合物、树脂膜、半导体层叠体、半导体层叠体的制造方法及半导体装置的制造方法 Download PDFInfo
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- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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Abstract
Description
技术领域
本发明涉及树脂组合物、树脂膜、半导体层叠体、半导体层叠体的制造方法及半导体装置的制造方法。
背景技术
近年来,在半导体行业中,为了适应智能手机等移动设备的小型化及低成本化,正在研究向大型塑料基板的转换,该大型塑料基板以作为芯片基板的硅晶圆的薄型化、制造效率的提高为目的。然而,由于在薄型基板及柔软的塑料基板中翘曲的影响变得显著,因此为了不在密封材料上产生裂纹,密封材料的强度变得重要。至今为止,为了提高密封材料的强度,虽对使用双酚A、联苯等酚化合物或酚醛清漆树脂、甲酚酚醛清漆树脂等酚树脂等的固化剂进行了各种研究,但仍对更高强度的密封材料存在需求(专利文献1)。此外,由于基板变得柔软因此容易弯曲,弯曲时会在芯片端或芯片下部施加较大的应力,导致密封材料与芯片间、或密封材料与基板间容易发生剥离,因此产生了提高密封材料自身的粘合力的必要、及减少因固化收缩而导致的翘曲的必要。
此外,为了提高制造效率,塑料基板较多使用方形基板,然而在利用液状密封材料将其密封时,容易在基板内侧与外侧产生不均,因此谋求一种能够将其容易且均匀地密封的膜种类。
对此,谋求一种即使在弯曲时也难以产生裂纹的、高强度、翘曲小、且即使发生翘曲也不会发生剥离的高粘合树脂组合物,及使用有该组合物的具有良好的晶圆保护性能的晶圆成型材料的开发,及该组合物的膜化。
现有技术文献
专利文献
专利文献1:日本特开2012-158730号公报
发明内容
本发明要解决的技术问题
本发明是鉴于上述问题点而完成的,其目的在于,提供一种高强度、翘曲小、粘合力优异的树脂组合物、该组合物膜化而成的高强度树脂膜、具有该树脂膜的固化物的半导体层叠体及其制造方法、以及该半导体层叠体被切片而成的半导体装置及其制造方法。
解决技术问题的技术手段
为了达成上述目的,本发明提供一种树脂组合物,其特征在于,含有:
(A)成分:环氧树脂;
(B)成分:下述式(1)和/或式(2)中记载的环氧化合物;
(C)成分:下述式(3)所示的环氧化合物;
(D)成分:酚性固化剂;及
(E)成分:固化促进剂。
[化学式1]
[化学式2]
[化学式3]
式中,A为单键或选自下述式中的二价有机基团。
[化学式4]
若为这样的组合物,则其固化物强度高、翘曲小、粘合力优异。
此外,优选所述(A)成分为有机硅改性环氧树脂。
如此,作为(A)成分的一个例子,可列举出有机硅改性环氧树脂。
此时,优选所述有机硅改性环氧树脂由下述式(4)表示,且重均分子量为3,000~500,000。
[化学式5]
式中,R1~R6各自独立地为碳原子数为1~20的一价烃基或烷氧基,可相互相同或不同。此外,a、b、c、d及e表示各重复单元的组成比,为满足0<a<1、0≤b<1、0≤c<1、0<d<1、0≤e<1、0.67≤(b+d)/(a+c+e)≤1.67、且a+b+c+d+e=1的正数。g为0~300的整数。X为下述式(5)所示的二价有机基团。Y为下述式(6)所示的二价含硅氧烷骨架基团。Z为下述式(7)所示的二价有机基团。
[化学式6]
式中,E为单键或选自下述式中的二价有机基团。R7和R8为碳原子数为1~20的一价烃基或烷氧基,可相互相同或不同。t和u各自独立地为0~2的整数。
[化学式7]
[化学式8]
式中,v为0~300的整数。
[化学式9]
式中,G为单键或选自下述式中的二价有机基团。R9和R10为碳原子数为1~20的一价烃基或烷氧基,可相互相同或不同。w和x各自独立地为0~2的整数。
[化学式10]
若为这样的组合物,则可获得耐化学药品性、耐热性、耐压性更优异的固化物。
此外,所述树脂组合物的固化后的拉伸强度优选为6.0MPa以上。
若为这样的组合物,则显示良好的抗裂纹性。
此外,优选相对于所述(A)成分100质量份,含有0.5~100质量份的所述(B)成分。
若为这样的组合物,则可充分地得到强度提高效果及对粘合力提高的效果,且不易对耐化学药品性、弹性模量、线膨胀系数带来大的恶劣影响,故而优选。
优选进一步含有(F)无机填充剂。
若为这样的组合物,则晶圆保护性更优异,进一步,耐热性、耐湿性、强度等更优异。
此时,优选所述无机填充剂为二氧化硅,并以20~96质量%包含于所述树脂组合物中。
若为这样的组合物,则加工性变得良好、强度得以提高,故而优选。
本发明进一步提供一种树脂膜,其特征在于,由上述本发明的树脂组合物膜化而成。
由于这样的树脂膜的强度及粘合力高,因此可成为不易引起各种错误的晶圆成型材料。
此外,所述树脂膜的固化后的拉伸强度优选为6.0MPa以上。
若为这样的树脂膜,则显示良好的抗裂纹性。
本发明进一步提供一种半导体层叠体,其特征在于,在半导体晶圆上具有上述本发明的树脂膜的固化物。
若为这样的半导体层叠体,则由于树脂膜的强度及粘合力高,因此能够利用树脂膜充分保护半导体晶圆。
本发明进一步提供一种半导体装置,其特征在于,其为上述本发明的半导体层叠体被切片而成的半导体装置。
若为这样的半导体装置,则为高质量。
本发明进一步提供一种半导体层叠体的制造方法,其特征在于,具有:将上述本发明的树脂膜贴附于半导体晶圆,并对该半导体晶圆进行成型的工序;及将所述树脂膜加热固化的工序。
若为这样的半导体层叠体的制造方法,则能够制造利用树脂膜而充分地保护了半导体晶圆的半导体层叠体。
本发明进一步提供一种半导体装置的制造方法,其特征在于,具有:对利用上述本发明的半导体层叠体的制造方法而制造的半导体层叠体进行切片的工序。
若为这样的半导体装置的制造方法,则能够制造高质量的半导体装置。
发明效果
本发明的树脂组合物能够大幅度提高固化物的强度。且由于密合性、低翘曲性、粘合性、晶圆保护性优异,能够将晶圆一并成型,因此成为可适用于晶圆级封装的树脂膜。通过使用这些发明,能够成品率良好地提供高质量的半导体装置。
具体实施方式
以下,对本发明进行更加详细的说明。
如上述所述,谋求一种高强度、翘曲小、粘合力优异的树脂组合物、该组合物膜化而成的高强度树脂膜、具有该树脂膜的固化物的半导体层叠体及其制造方法、以及该半导体层叠体被切片而成的半导体装置及其制造方法。
为了达成上述目的,本申请的发明人进行了深入研究。其结果发现,通过组合(A)环氧树脂、(B)特定结构的环氧化合物、(C)另外的特定结构的环氧化合物、(D)酚性固化剂及(E)固化促进剂,能够得到固化物的拉伸强度大、粘合力也高、翘曲也小的树脂组合物。还发现通过使该所述树脂组合物膜化,能够得到更容易操作的晶圆成型材料,从而完成了本发明。
以下,对本发明的实施方式进行具体的说明,但本发明并不被其限定。
[树脂组合物]
本发明的树脂组合物含有(A)环氧树脂、(B)特定的含烯丙基的环氧化合物、(C)特定的不含烯丙基的环氧化合物及(D)酚性固化剂、(E)固化促进剂。
[(A)成分]
本发明的树脂组合物中,(A)成分为环氧树脂。作为所述环氧树脂,可列举出双酚A型环氧树脂、双酚F型环氧树脂、双酚AD型环氧树脂、苯酚酚醛清漆型环氧树脂、联苯型环氧树脂、萘型环氧树脂、脂环式环氧树脂、缩水甘油酯型环氧树脂、缩水甘油胺型环氧树脂、杂环式环氧树脂、二芳砜型环氧树脂、有机硅改性环氧树脂等,但并不被其限定。
作为所述有机硅改性环氧树脂,优选其由下述式(4)表示,且重均分子量为3,000~500,000。此时,含有该有机硅改性环氧树脂的组合物的固化物更加表现出耐化学药品性、耐热性、耐压性。
[化学式11]
式(4)中,R1~R6各自独立地为碳原子数为1~20的一价烃基或烷氧基,可相互相同或不同。作为所述一价烃基,无特别限定,可列举出直链状、支链状或环状的烷基、烯基、炔基等。作为R1~R6,优选碳原子数为1~12的一价烃基或烷氧基,更优选碳原子数为1~10的一价烃基或烷氧基,特别优选碳原子数为1~6的一价烃基或烷氧基。作为R1~R6,优选甲基、乙基、丙基、己基、环己基、苯基等,其中,从获取原料的难易度出发,优选甲基及苯基。
式(4)中,a、b、c、d及e表示各重复单元的组成比,为满足0<a<1、0≤b<1、0≤c<1、0<d<1、0≤e<1、0.67≤(b+d)/(a+c+e)≤1.67、且a+b+c+d+e=1的正数。式(4)中,g为0~300的整数。
式(4)中,X为下述式(5)所示的二价有机基团。
[化学式12]
式中,E为单键或选自下述式中的二价有机基团。
[化学式13]
式(4)中,Y为下述式(6)所示的二价的含硅氧烷骨架基团。
[化学式14]
式中,v为0~300的整数。
式(4)中,Z为下述式(7)所示的二价有机基团。
[化学式15]
式中,G为单键或选自下述式中的二价有机基团。
[化学式16]
式(5)、(7)中,R7、R8、R9和R10为碳原子数为1~20的一价烃基或烷氧基,可相互相同或不同。作为R7~R10,优选碳原子数为1~4的烷基或烷氧基,更优选碳原子数为1~2的烷基或烷氧基,具体而言,优选甲基、乙基、丙基、叔丁基、甲氧基、乙氧基等。
式(5)、(7)中,t、u、w及x各自独立地为0~2的整数,优选为0。
式(4)所示的有机硅改性环氧树脂的重均分子量(Mw)为3,000~500,000,优选为5,000~200,000。式(4)所示的有机硅改性环氧树脂可为无规共聚物,也可为嵌段共聚物。
环氧树脂可单独使用一种,也可组合使用两种以上。
式(4)所示的有机硅改性环氧树脂可通过使用选自下述式(8)所示的硅亚苯基化合物及下述式(9)~(12)所示的化合物中的化合物,并利用以下所示的方法而制备。
[化学式17]
式中,R1~R10、E、G、g、t、u、v、w及x与上述相同。
式(4)所示的有机硅改性环氧树脂能够通过使原料氢化硅烷化而合成。此时,可以以向反应容器中加入了全部原料的状态而使其反应,也可先使一部分原料反应后使剩余的原料反应,还可使原料一种一种地进行反应,反应顺序也可任意选择。关于各化合物的掺合比,以使上述式(8)及式(9)所示的化合物所具有的硅氢基的摩尔数的合计相对于上述式(10)、式(11)及式(12)所示的化合物所具有的烯基的摩尔数的合计为0.67~1.67的方式进行掺合即可,优选以0.83~1.25的方式进行掺合。
该聚合反应在催化剂的存在下进行。催化剂可使用用于进行氢化硅烷化的广为人知的催化剂。具体而言,可使用钯络合物,铑络合物,铂络合物等,但并不被其限定。优选相对于Si-H键,添加0.01~10.0摩尔%左右的催化剂。若为0.01摩尔%以上,则反应的进行不会变慢,反应充分进行,若为10.0摩尔%以下,则不易进行脱氢反应,不会阻碍加成反应的进行。
作为聚合反应中使用的溶剂,可广泛使用不阻碍氢化硅烷化的有机溶剂。具体而言,可列举出辛烷、甲苯、四氢呋喃、二噁烷等,但并不被其限定。优选以使溶质成为10~70质量%的方式使用溶剂。若为10质量%以上,则反应体系不会变稀薄,反应的进行不会变慢。此外,若为70质量%以下,则粘度不会变高,不会在反应途中变得无法充分搅拌体系。
反应通常以40~150℃、优选以60~120℃、特别优选以70~100℃的温度而进行。若反应温度为150℃以下,则不易引起分解等的副反应,若为40℃以上,则反应的进行不会变慢。此外,反应时间通常为0.5~60小时,优选为3~24小时,特别优选为5~12小时。
[(B)成分]
(B)成分为下述式(1)和/或(2)所示的环氧化合物。
[化学式18]
[化学式19]
式中,A为单键或选自下述式中的二价有机基团。
[化学式20]
具体而言,以以下的结构表示。
[化学式21]
[化学式22]
在二价有机基团中,特别优选上述A为以下的二价有机基团。
[化学式23]
通过使用这些二价有机基团,组合物的固化物的物性变得更良好。
进一步,由于这些化合物所具有的烯丙基通过π-π相互作用而使强度得以提高,且同时以填埋交联间的间隙的方式而发挥作用,因此固化物的均匀性得以提高,韧性得以提高。由此,作为密封材料而进行使用时,由于在能够抑制由基板的翘曲导致的裂纹的产生的同时,还可抑制剥离,因此能够适用于晶圆级封装。
关于(B)环氧化合物的含量,相对于(A)成分含量100质量份,(B)成分优选为0.5~100质量份,更优选为3~50质量份。若(B)成分的含量为0.5质量份以上,则可充分地得到强度提高效果及对粘合力提高的效果,若为100质量份以下,则不易对耐化学药品性、弹性模量、线膨胀系数带来大的恶劣影响,故而优选。
[(C)成分]
(C)成分为下述式(3)所示的环氧化合物。
[化学式24]
式中,A为单键或选自下述式中的二价有机基团。
[化学式25]
具体而言,以以下的结构表示。
[化学式26]
在二价有机基团中,特别优选上述A为以下的二价有机基团。
[化学式27]
由于这些化合物(C)与(B)成分为不相容体系,因此通过添加而在一部分形成海岛结构。在将组合物固化时产生应力的情况下,由于应力在海岛结构中逃散,因此结构体不易发生翘曲。即,作为密封材料而进行使用时,由于能够将基板的翘曲抑制得较小,因此可适用于晶圆级封装。
相对于(B)成分的掺合量,(C)环氧化合物的含量优选为80质量%~120质量%。若(C)成分的含量在上述范围内,则能够形成适合的海岛结构。
[(D)成分]
作为(D)成分的酚性固化剂,可广泛使用公知的酚性固化剂。作为固化剂的结构,可例示出以下所示的结构,但并不被其限定。
[化学式28]
关于(D)成分的含量,优选以相对于组合物中的环氧基当量、(D)成分中的酚性羟基当量为70mol%~140mol%的方式进行掺合,更优选为90mol%~110mol%。若为所述范围,则固化反应良好地进行。若为所述范围,则环氧基及酚性羟基不会过度剩余,可靠性不易变差。
[(E)成分]
作为(E)成分的固化促进剂,只要是用于环氧基的开环的固化促进剂,则可广泛使用。作为所述固化促进剂,可列举出咪唑、2-甲基咪唑、2-乙基咪唑、2-十一烷基咪唑、2-十七烷基咪唑、1,2-二甲基咪唑、2-乙基-4-甲基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、1-苄基-2-甲基咪唑、1-氰基乙基-2-甲基咪唑、1-氰基乙基-2-十一烷基咪唑、1-氰基乙基-2-乙基-4-甲基咪唑、1-氰基乙基-2-苯基咪唑、2-苯基-4,5-二羟基甲基咪唑、2-苯基-4-甲基-5-羟基甲基咪唑等咪唑类;2-(二甲基氨基甲基)苯酚、三亚乙基二胺、三乙醇胺、1,8-二氮杂双环[5.4.0]十一烯-7,三(二甲基氨基甲基)苯酚等叔胺类;二苯基膦、三苯基膦、三丁基膦等有机膦类;辛酸锡等金属化合物;四苯基鏻-四苯硼酸盐、四苯基鏻-乙基三苯硼酸盐等四取代鏻-四取代硼酸盐等。
相对于(A)成分100质量份,(E)成分的含量优选为0.05~20.0质量份,更优选为0.5~3.0质量份。若为所述范围,则以没有过量或不足的方式进行固化反应。若为0.05质量份以上,则不易反应不彻底,若为20.0质量份以下,则固化物不易变脆。
[(F)成分]
为了赋予晶圆保护性,且进一步提高耐热性、耐湿性、强度等,并提高固化物的可靠性,本发明的树脂组合物也可含有无机填充剂作为(F)成分。作为无机填充剂,例如可列举出滑石、烧成粘土、未烧成粘土、云母、玻璃等硅酸盐;氧化钛、氧化铝、熔融二氧化硅(熔融球状二氧化硅,熔融破碎二氧化硅)、结晶二氧化硅粉末等氧化物;碳酸钙、碳酸镁、水滑石等碳酸盐;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。这些无机填充剂可以单独使用一种,也可组合使用两种以上。其中,优选熔融二氧化硅、结晶二氧化硅等二氧化硅粉末。作为所述二氧化硅粉末,例如可列举出气相二氧化硅、沉淀性二氧化硅等补强性二氧化硅;石英等结晶性二氧化硅。具体而言,可列举出NIPPON AEROSIL CO.,LTD.制造的Aerosil(注册商标)R972,R974,R976;Admatechs.制造的SE-2050,SC-2050,SE-1050,SO-E1,SO-C1,SO-E2,SO-C2,SO-E3,SO-C3,SO-E5,SO-C5;Shin-Etsu Chemical Co.,Ltd.制造的Musil 120A,Musil 130A等。
无机填充剂的平均粒径无特别限定,优选为0.01~20μm,更优选为0.01~10μm。若无机填充剂的平均粒径为0.01μm以上,则无机填充剂变得不易凝集,强度变高,故而优选。此外,若为20μm以下,则树脂向芯片间的流动性变高,填充性变得良好,故而优选。另外,平均粒径能够通过基于激光衍射法的粒度分布测定装置而求得,可作为质量平均值D50(即,累积质量为50%时的粒径或中值粒径)而测定。
树脂组合物的固体成分中,(F)成分的含量优选为20~96质量%,更优选为50~96质量%,特别优选为75~94质量%。若无机填充剂的含量为96质量%以下,则加工性变得良好且强度得以提高,故而优选。此外,若为20质量%以上,则充分发挥效果。另外,固体成分是指除有机溶剂以外的成分。
[(G)有机溶剂]
本发明的树脂组合物也可含有(G)成分作为有机溶剂。作为有机溶剂,例如可列举出N,N-二甲基乙酰胺、甲基乙基酮、N,N-二甲基甲酰胺、环己酮、环戊酮、N-甲基-2-吡咯烷酮、甲醇、乙醇、异丙醇、丙酮、丙二醇单甲醚、丙二醇单甲醚乙酸酯、甲苯、二甲苯等,特别优选甲基乙基酮、环戊酮、丙二醇单甲醚、丙二醇单甲醚乙酸酯,但并不被其限定。这些有机溶剂可单独使用一种,也可混合使用两种以上。优选有机溶剂的使用量为使树脂组合物中的固体成分浓度成为60~90质量%的量。
[其他成分]
以阻燃性的提高为目的,本发明的树脂组合物还可含有阻燃剂。作为阻燃剂,可列举出磷类阻燃剂,其为不含卤原子而赋予阻燃性的物质,作为其例,可列举出磷腈化合物,磷酸酯化合物,磷酸酯酰胺化合物等。磷腈化合物及磷酸酯酰胺化合物由于分子内含有磷原子和氮原子,因此能够得到特别高的阻燃性。相对于(A)成分100质量份,阻燃剂的含量优选为5~30质量份。
本发明的树脂组合物还可含有硅烷偶联剂。通过含有硅烷偶联剂,能够进一步提高树脂组合物对被粘物的密合性。作为硅烷偶联剂,可列举出环氧硅烷偶联剂、含芳香族氨基硅烷偶联剂等。这些硅烷偶联剂可单独使用一种,也可组合使用两种以上。硅烷偶联剂的含量无特别限定,在本发明的树脂组合物中优选为0.01~5质量%。
此外,本发明的树脂组合物也可进一步含有除上述成分以外的成分。例如为了提高(A)成分与(B)成分的相容性,或为了提高树脂组合物的储存稳定性或操作性等各种特性,还可适当添加各种添加剂。例如可添加脂肪酸酯、甘油酸酯、硬脂酸锌、硬脂酸钙等内部脱模剂;酚类、磷类或硫类抗氧化剂等。此外,也可使用碳等颜料,对组合物进行着色。
其他成分可以以无溶剂的方式添加于本发明的树脂组合物中,也可溶解或分散于有机溶剂中,制备为溶液或分散液后再进行添加。
此外,上述树脂组合物的固化后的拉伸强度优选为6.0MPa以上,特别优选为8.0~20.0MPa的范围。若拉伸强度为6.0MPa以上,则能够防止由于因基板或芯片的热而导致的膨胀收缩、搭载半导体封装时的力等而产生裂纹,即,显示良好的抗裂纹性。
若为上述本发明的组合物,则能够将晶圆一并成型(晶圆成型),特别是对大口径、薄膜晶圆具备良好的成型性,且同时为高强度、并具有不易发生与基板的剥离的高粘合性及低翘曲性,能够良好地进行成型工序,能够适用于晶圆级封装。
进一步,以往的树脂组合物进行固化后的应力通常为10.0~20.0Mpa,而使用本发明的树脂组合物时,能够使该应力成为7.0~15.0MPa。对于以88重量%添加填料时的固化物,以往的树脂组合物的通常为5.0~13.0MPa的应力有时会降低至3.0~9.0MPa左右。由于通过使应力降低而使得封装体不易发生翘曲,且拉伸强度及伸长率几乎不发生变化,因此能够适用于封装材料。
[树脂膜]
本发明的树脂膜为上述本发明的树脂组合物膜化而成的树脂膜。即,本发明的树脂膜为使用所述树脂组合物并加工为膜状而得到的物质。通过形成为膜状,相对于大口径、薄膜晶圆具有良好的成型性能,在将晶圆一并成型时,不需流入树脂,因此不会发生对晶圆表面的填充不良等问题。此外,若为使用所述树脂组合物而形成的树脂膜,则强度及粘合力高,因此成为不易引起各种错误的晶圆成型材料。
本发明的树脂膜的固化后的拉伸强度优选为6.0MPa以上,更优选为8.0~20.0MPa。若拉伸强度为6.0MPa以上,则能够防止由于因基板或芯片的热而导致的膨胀收缩、搭载半导体封装时的力等而产生裂纹,即,显示良好的抗裂纹性。
希望本发明的树脂膜为无填料的膜时,固化后弹性模量为150~1,500MPa;本发明的树脂膜为加入了填料的膜时,固化后弹性模量为1,000~20,000MPa左右。通过提高弹性模量,封装变得不易变形,保护性能有时会得以提升。
本发明的树脂膜可在由所述树脂组合物得到的树脂膜上层叠有保护膜。对此时的本发明的树脂膜的制造方法的一个例子进行说明。
将所述(A)~(E)成分、以及根据所需的(F)(G)成分、及其他成分混合,从而制备树脂组合物溶液,使用逆转辊涂布机、逗号涂布机(comma coater)等将该树脂组合物溶液以成为所需厚度的方式涂布在保护膜上。将涂布有所述树脂组合物溶液的保护膜通入在线干燥机(in-line dryer),以80~160℃历时2~20分钟将有机溶剂去除,从而使其干燥,接着使用辊式层压机与另外的保护膜压接,进行层叠,由此能够得到形成有树脂膜的层叠体膜。将该层叠体膜用作晶圆成型材料时,提供良好的成型性。
将本发明的树脂组合物形成为膜状时,厚度虽无限制,但优选为2mm以下,更优选为50μm以上、1,200μm以下,进一步优选为80~850μm。若为这样的厚度,则作为半导体密封材料的保护性优异,故而优选。
所述保护膜只要能够以不损伤由本发明的树脂组合物形成的树脂膜的形态的方式进行剥离,则无特别限定,其作为晶圆用保护膜及剥离膜而发挥作用,通常可列举出聚乙烯(PE)膜、聚丙烯(PP)膜、聚甲基戊烯(TPX)膜、实施了脱模处理的聚酯膜等塑料膜等。此外,剥离力优选为50~300mN/min。保护膜的厚度优选为25~150μm,更优选为38~125μm。
[半导体层叠体及其制造方法]
本发明的半导体层叠体在半导体晶圆上具有上述本发明的树脂膜的固化物。本发明的半导体层叠体的制造方法为具有以下工序的方法:将所述树脂膜贴附于半导体晶圆,并对该半导体晶圆进行成型的工序;及将所述树脂膜加热固化的工序。
作为所述半导体晶圆,可以为表面上装载有半导体元件(芯片)的晶圆,也可以为表面上制作有半导体元件的半导体晶圆。本发明的树脂膜在成型前对这样的晶圆表面具有良好的填充性,此外,成型后具有高强度及高粘合性,对这样的晶圆的保护性优异。此外,本发明的树脂膜能够适用于直径8英寸以上、例如直径8英寸(200mm)、12英寸(300mm)或其以上的大口径的晶圆及薄膜晶圆的成型。作为所述薄型晶圆,优选薄型加工至厚度为5~400μm的晶圆。
关于使用了本发明的树脂膜的晶圆的成型方法,无特别限定,例如可以以下述方式进行:将粘贴在树脂膜上的一个保护层剥下,使用Takatori Corporation.制造的真空层压机(产品名称:TEAM-300),将真空室内的真空度设定为50~1,000Pa、优选设定为50~500Pa、例如设定为100Pa,并以80~200℃、优选以80~130℃、例如以100℃将粘贴有另一个保护层的树脂膜与所述晶圆一并进行密合,恢复至常压后,将所述晶圆冷却至室温并从所述真空层压机中取出,将另一个保护层剥离。
此外,对于层叠有半导体芯片的晶圆而言,可以适当使用压模装置、或具备真空隔膜层压机(vacuum diaphragm laminator)和用于平坦化的金属板压机(金属板プレス)的装置等。例如,作为压模装置,可使用APIC YAMADA CORPORATION.制造的装置(产品名称:MZ-824-01),将层叠有半导体芯片的300mm硅晶圆成型时,可以以100~180℃、成型压力100~300kN、模压时间(clamp time)30~90秒、成型时间5~20分钟的条件进行成型。
此外,作为具备真空隔膜层压机和用于平坦化的金属板压机的装置,可使用Nichigo-Morton Co.,Ltd.制造的装置(产品名称:CVP-300),可以以层压温度100~180℃、真空度50~500Pa、压力0.1~0.9MPa、层压时间30~300秒的条件进行层压后,以上下热板温度100~180℃、压力0.1~3.0MPa、加压时间30~300秒的条件使树脂成型面平坦化。
成型后,通过以120~220℃、15~360分钟的条件对树脂膜进行加热,能够将树脂膜固化。由此得到半导体层叠体。
[半导体装置及其制造方法]
本发明的半导体装置为上述本发明的半导体层叠体被切片而成的半导体装置。本发明的半导体装置的制造方法为具有下述工序的方法:对利用上述本发明的半导体层叠体的制造方法而制造的半导体层叠体进行切片的工序。如此,通过将利用树脂膜成型的半导体晶圆切片,得到具有加热固化覆膜的半导体装置。以使成型树脂面或晶圆面与切割胶带等半导体加工用保护胶带相接的方式粘贴成型的晶圆,并设置于切割机的吸附台上,使用具有切割刀片的划片机(例如DISCO公司制造的DFD6361)将该成型的晶圆切断。切割时的主轴转速及切断速度适当选择即可,通常,主轴转速为25,000~45,000rpm,切断速度为10~50mm/sec。此外,切片的尺寸根据半导体封装的设计而不同,大致为2mm×2mm~30mm×30mm左右。
如此,由于所述利用树脂膜成型的半导体晶圆的树脂膜的强度和粘合力高,因此能够充分保护半导体晶圆,因而能够成品率良好地对其进行切片而得到高质量的半导体装置。
实施例
以下,示出合成例、实施例及比较例对本发明进行更具体的说明,但本发明并不被下述的实施例所限定。
使用的化合物S-1~S-8如下所示。
[化学式29]
[化学式30]
[化学式31]
[化学式32]
[化学式33]
[化学式34]
[化学式35]
[化学式36]
[环氧化合物(1)合成例]
向具备搅拌机、温度计、氮置换装置及回流冷却器的5L烧瓶内,加入617g(2.0摩尔)的化合物S-1、256g(8.0摩尔)的甲醇、852g(8.0摩尔)的环氧氯丙烷,历时2小时添加768g(19.2摩尔)的氢氧化钠,之后,升温至60℃使其反应3小时。反应后,加入500mL的甲苯,利用纯水进行清洗直至水层成为中性后,在减压下将有机层中的溶剂去除,得到了757g(1.8摩尔)的环氧化合物(1)。
[化学式37]
[环氧化合物(2)合成例]
向具备搅拌机、温度计、氮置换装置及回流冷却器的5L烧瓶内,加入617g(2.0摩尔)的化合物S-1、256g(8.0摩尔)的甲醇,724g(8.0摩尔)的氯丙烯,历时2小时直接添加768g(19.2摩尔)的颗粒状的氢氧化钠,添加结束后,加温至60℃并进行3小时的老化。之后,向反应溶液中加入500mL的甲苯,利用纯水进行清洗操作直至水层成为中性后,在减压下去除有机层中的有机溶剂,得到了740g的粗生成物。将其再次移至具备搅拌机、温度计、氮置换装置及回流冷却器的5L烧瓶内,通过以180℃搅拌4小时引发克莱森重排(ClaisenRearrangement)。之后,将体系中的温度降至45℃,再次加入245g(7.6摩尔)的甲醇、810g(7.6摩尔)的环氧氯丙烷,历时1小时添加365g(9.1摩尔)的氢氧化钠,之后,升温至60℃使其反应3小时。反应后,加入500mL的甲苯,利用纯水进行清洗直至水层成为中性后,在减压下馏去有机层中的有机溶剂,得到了851g(1.7摩尔)的环氧化合物(2)。
[化学式38]
[1]树脂的合成
合成例中,重均分子量(Mw)为使用GPC色谱柱TSKgel Super HZM-H(TOSOHCORPORATION制造),并以流量0.6mL/分钟、洗脱溶剂四氢呋喃、色谱柱温度40℃的分析条件,通过以单分散聚苯乙烯为标准的凝胶渗透层析法(GPC)而测定的值。
[树脂合成例1]
向具备搅拌机、温度计、氮置换装置及回流冷却器的3L烧瓶内,加入195.9g(0.333摩尔)的化合物S-2后,加入1,400g的甲苯,加温至70℃。之后,投入1.0g的氯铂酸甲苯溶液(铂浓度0.5质量%),并分别历时1小时滴加414.9g(0.267摩尔)的化合物S-3、及13.0g(0.067摩尔)的化合物S-4(硅氢基的合计摩尔数/烯基的合计摩尔数=0.5/0.5=1/1)。滴加结束后,加温至100℃,进行6小时的老化后,从反应溶液中减压馏去甲苯,得到了570g的下述式所表示的树脂1。树脂1的Mw为37,400。另外,树脂1中所含的硅氧烷量为67质量%。
[化学式39]
[树脂合成例2]
向具备搅拌机、温度计、氮置换装置及回流冷却器的3L烧瓶内,加入133.5g(0.227摩尔)的化合物S-2后,加入甲苯1,500g,加温至70℃。之后,投入1.0g的氯铂酸甲苯溶液(铂浓度0.5质量%),并分别历时1小时滴加525.6g(0.182摩尔)的化合物S-5、8.8g(0.045摩尔)的化合物S-4(硅氢基的合计摩尔数/烯基的合计摩尔数=0.500/0.500=1)。滴加结束后,加温至100℃,进行6小时的老化后,从反应溶液中减压馏去甲苯,得到了605g的下述式所表示的树脂2。树脂2的Mw为51,100。另外,树脂2中所含的硅氧烷量为79质量%。
[化学式40]
[树脂合成例3]
向具备搅拌机、温度计、氮置换装置及回流冷却器的3L烧瓶内,加入104.9g(0.179摩尔)的化合物S-2、及61.5g(0.143摩尔)的化合物S-6、及6.6g(0.036摩尔)的化合物S-7后,加入甲苯1,600g,加温至70℃。之后,投入1.0g的氯铂酸甲苯溶液(铂浓度0.5质量%),并分别历时1小时滴加516.3g(0.179摩尔)的化合物S-5、及34.7g(0.179摩尔)的化合物S-4(硅氢基的合计摩尔数/烯基的合计摩尔数=0.500/0.500=1.00)。滴加结束后,加温至100℃进行6小时的老化后,从反应溶液中减压馏去甲苯,得到了680g的树脂3。树脂3的Mw为46,800。另外,树脂3中所含的硅氧烷量为72质量%。
[化学式41]
[树脂合成例4]
向具备搅拌机、温度计、氮置换装置及回流冷却器的3L烧瓶内,加入140.2g(0.333摩尔)的化合物S-8后,加入甲苯1,500g,加温至70℃。之后,投入1.0g的氯铂酸甲苯溶液(铂浓度0.5质量%),并历时1小时滴加518.7g(0.333摩尔)的S-3(硅氢基的合计摩尔数/烯基的合计摩尔数=0.500/0.500=1.00)。滴加结束后,加温至100℃,进行6小时的老化后,从反应溶液中减压馏去甲苯,得到了610g的树脂4。树脂4的Mw为49,500。另外,树脂4中所含的硅氧烷量为79质量%。
[化学式42]
[树脂合成例5]
向具备搅拌机、温度计、氮置换装置及回流冷却器的3L烧瓶内,加入420.5g(1.000摩尔)的化合物S-8后,加入甲苯1,400g,加温至70℃。之后,投入1.0g的氯铂酸甲苯溶液(铂浓度0.5质量%),并历时1小时滴加194.4g(1.000摩尔)的S-4(硅氢基的合计摩尔数/烯基的合计摩尔数=1.000/1.000=1.00)。滴加结束后,加温至100℃进行6小时的老化后,从反应溶液中减压馏去甲苯,得到了570g的树脂5。树脂5的Mw为53,200。另外,树脂5中不含硅氧烷。
[化学式43]
[2]树脂膜的制作
[实施例1~20及比较例1~16]
以下述表1~4中记载的组成,将(A)合成例5中合成的环氧树脂(树脂5)或合成例1~4中合成的有机硅改性环氧树脂(树脂1~4)、(B)环氧化合物(1)~(2)、(C)环氧化合物(3)、(D)酚性固化剂、(E)固化促进剂、及(F)无机填充剂掺合。进一步,以使固形成分浓度成为65质量%的量添加环戊酮,使用搅拌器或均相混合机进行搅拌,从而进行混合及分散,制备了树脂组合物的分散液。以使苯酚当量同(A)成分中所含的环氧基与(B)(C)成分中所含的环氧基的当量相同的方式加入(D)酚性固化剂。
使用模涂机作为涂膜机,使用E7304(商品名称,TOYOBO CO.,LTD.制造的聚酯,厚度75μm,剥离力200mN/50mm)作为保护膜,并将各树脂组合物涂布于保护膜上。接着,通过将其放入设定为100℃的烘箱内30分钟,从而使溶剂完全蒸发,在所述保护膜上形成膜厚100μm的树脂膜。
上述以外的使用于树脂组合物的制备的各成分如下所示。
[环氧化合物]
环氧化合物(3)
[化学式44]
[酚性固化剂]
[化学式45]
[化学式46]
[化学式47]
[固化促进剂]
·Curezol 2P4MHZ(SHIKOKU CHEMICALS CORPORATION.制造,2-苯基-4-甲基-5-羟基甲基咪唑)
[无机填充剂]
·二氧化硅(Admatechs.制造,平均粒径5.0μm)
[3]树脂膜的评价
对于所得到的树脂膜,利用以下的方法进行评价。将结果示于表1~4。
<拉伸强度的测定方法>
使用拉伸强度测定装置(Shimadzu Corrporation.制造的Autograph AGS-5kNG),测定制作的已固化的膜的拉伸弹性模量、强度及伸长率。树脂膜的固化条件为180℃×4小时。
<粘合试验方法>
将制作的膜贴附于20mm见方的硅晶圆上,从其上方按压切为2mm见方的硅芯片,并将它们加热固化(180℃×4小时),之后,使用粘合力测定装置(Nordson AdvancedTechnology(Japan)K.K.制造的万能型Bond Tester系列4000(DS-100)),测定从芯片侧面弹开时的粘合力(推晶试验(die shear test))。
<翘曲应力测定试验方法>
利用膜层压机(TAKATORI TEAM-100)将制作的膜层压于硅晶圆上,并进行加热固化(180℃×4小时),利用Toho Technology Corporation制造的薄膜应力测定装置(FLX-2320-S),测定它们的翘曲应力。
[表1]
[表2]
[表3]
[表4]
以上的结果显示,由本发明的树脂组合物得到的树脂膜与由不含(C)成分的组合物得到的比较例的树脂膜相比,虽然强度和粘合力不存在较大差异,但比较不含二氧化硅的表1、3或含二氧化硅的表2、4时,翘曲应力大幅度降低。由该特征可以说明,将本发明的树脂组合物使用于半导体密封用膜时,不易引起裂纹及剥离、且翘曲也小。
本发明的树脂组合物,通过适当组合具有烯丙基的特定结构的环氧化合物和不具有烯丙基的环氧化合物,可较大地改善固化物的强度和粘合力、翘曲应力。由此,例如将本发明的树脂组合物使用于膜状成型用途时,能够对芯片搭载晶圆显示良好的抗裂纹性、低翘曲性、难剥离性。
另外,本发明并不被上述实施方式所限定。上述实施方式仅为例示,具有与本发明的专利权利要求书中所记载的技术构思实质相同的构成、实现相同技术效果的发明均包含于本发明的技术范围内。
Claims (16)
2.根据权利要求1所述的树脂组合物,其特征在于,所述(A)成分为有机硅改性环氧树脂。
3.根据权利要求2所述的树脂组合物,其特征在于,所述有机硅改性环氧树脂由下述式(4)表示,且重均分子量为3,000~500,000,
[化学式5]
式中,R1~R6各自独立地为碳原子数为1~20的一价烃基或烷氧基,可相互相同或不同;此外,a、b、c、d及e表示各重复单元的组成比,为满足0<a<1、0≤b<1、0≤c<1、0<d<1、0≤e<1、0.67≤(b+d)/(a+c+e)≤1.67、且a+b+c+d+e=1的正数;g为0~300的整数;X为下述式(5)所示的二价有机基团;Y为下述式(6)所示的二价的含硅氧烷骨架基团;Z为下述式(7)所示的二价有机基团,
[化学式6]
式中,E为单键或选自下述式中的二价有机基团;R7和R8为碳原子数为1~20的一价烃基或烷氧基,可相互相同或不同;t和u各自独立地为0~2的整数,
[化学式7]
[化学式8]
式中,v为0~300的整数,
[化学式9]
式中,G为单键或选自下述式中的二价有机基团;R9和R10为碳原子数为1~20的一价烃基或烷氧基,可相互相同或不同;w和x各自独立地为0~2的整数,
[化学式10]
4.根据权利要求1所述的树脂组合物,其特征在于,所述树脂组合物的固化后的拉伸强度为6.0MPa以上。
5.根据权利要求2所述的树脂组合物,其特征在于,所述树脂组合物的固化后的拉伸强度为6.0MPa以上。
6.根据权利要求3所述的树脂组合物,其特征在于,所述树脂组合物的固化后的拉伸强度为6.0MPa以上。
7.根据权利要求1~6中任一项所述的树脂组合物,其特征在于,相对于所述(A)成分100质量份,含有0.5~100质量份的所述(B)成分。
8.根据权利要求1~6中任一项所述的树脂组合物,其特征在于,进一步含有(F)无机填充剂。
9.根据权利要求8所述的树脂组合物,其特征在于,所述无机填充剂为二氧化硅,并以20~96质量%包含于所述树脂组合物中。
10.一种树脂膜,其特征在于,由权利要求1~6中任一项所述的树脂组合物固化而成。
11.一种树脂膜,其特征在于,由权利要求7所述的树脂组合物固化而成。
12.根据权利要求10所述的树脂膜,其特征在于,所述树脂膜的固化后的拉伸强度为6.0MPa以上。
13.一种半导体层叠体,其特征在于,在半导体晶圆上具有权利要求10所述的树脂膜的固化物。
14.一种半导体装置,其特征在于,其为权利要求13所述的半导体层叠体被切片而成的半导体装置。
15.一种半导体层叠体的制造方法,其特征在于,具有:将权利要求10所述的树脂膜贴附于半导体晶圆,并对该半导体晶圆进行成型的工序;及将所述树脂膜加热固化的工序。
16.一种半导体装置的制造方法,其特征在于,具有:对利用权利要求15所述的半导体层叠体的制造方法而制造的半导体层叠体进行切片的工序。
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