CN104603181A - 可固化有机硅组合物、制备半导体器件的方法和半导体器件 - Google Patents
可固化有机硅组合物、制备半导体器件的方法和半导体器件 Download PDFInfo
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- CN104603181A CN104603181A CN201380044524.4A CN201380044524A CN104603181A CN 104603181 A CN104603181 A CN 104603181A CN 201380044524 A CN201380044524 A CN 201380044524A CN 104603181 A CN104603181 A CN 104603181A
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
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- Microelectronics & Electronic Packaging (AREA)
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- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
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Abstract
本发明涉及一种可固化有机硅组合物,其包含:(A)有机聚硅氧烷,其由以下部分构成:(A-1)在分子中具有至少两个硅键合的烯基基团的直链有机聚硅氧烷,以及(A-2)包含1.5重量%至5.0重量%的烯基基团的类树脂有机聚硅氧烷;(B)在分子中具有至少两个硅键合的氢原子的有机聚硅氧烷;(C)在25℃具有2至10mm2/s的粘度并且具有在两个分子链末端封端的烯基基团的直链二烷基聚硅氧烷;以及(D)硅氢加成反应催化剂。所述可固化有机硅组合物形成具有低表面粘着性和低摩擦系数的固化产品。
Description
技术领域
本发明涉及可固化有机硅组合物,利用该组合物制备半导体器件的方法,以及通过该方法获得的半导体器件。
本发明要求提交于2012年9月10日的日本专利申请No.2012-198803的优先权,该专利申请的内容以引用方式并入本文中。
背景技术
由二甲基聚硅氧烷作为主要组分构成的可固化有机硅组合物由于形成具有优异的类橡胶性质(即硬度、伸长率等)以及具有诸如耐候性、耐热性等特性的固化产品而被用于多种类型的应用。可固化有机硅组合物由于形成具有低折光率的透明固化产品而尤其被用作半导体器件的密封剂。然而,该固化产品一直存在一定的问题:由于其表面的粘着性高,因此粉尘易于附着到以可固化有机硅组合物密封的半导体器件上,并且在以该固化产品密封的半导体器件的刀片切割步骤中,通过切割获得单个半导体器件时,切屑易于附着到所述半导体器件上。此外,还存在由于切割的半导体器件彼此粘附所致的处理和可加工性变差的问题。
日本未经审查的专利申请公布NO.2009-052038和2010-174234提出了一种用于形成具有高折光率并且无表面粘性的高度透明的固化产品的可固化有机硅组合物,其包含:(A)由以下组分构成的有机聚硅氧烷:(A-1)具有硅键合的烯基基团的二烷基聚硅氧烷,和(A-2)具有硅键合的烯基基团的类树脂有机聚硅氧烷;(B)具有硅键合的氢原子,并且除硅键合的氢原子之外,具有硅键合的含1至10个碳原子烯基基团的有机聚硅氧烷;以及(C)硅氢加成反应催化剂。
然而,当使用分别在所述专利文献中提及的可固化有机硅组合物密封半导体器件时,据发现,存在的问题在于粉尘易于附着到获得的半导体器件上,并且半导体器件彼此粘附以致后续处理和可加工性较差。
本发明的一个目标是提供一种形成具有低表面粘着性和低摩擦系数的固化产品的可固化有机硅组合物。本发明的另一个目标是提供一种制备半导体器件的方法,所述半导体器件能够避免粉尘粘附并且防止半导体器件彼此粘附;以及提供这样的半导体器件。
发明内容
本发明的可固化有机硅组合物包含:
(A)100质量份的有机聚硅氧烷,其由以下部分构成:
(A-1)30质量%至70质量%的在25℃具有10至100,000mPa·s粘度的直链有机聚硅氧烷,其在分子中具有至少两个硅键合的烯基基团,并且除烯基基团之外的各硅键合的基团独立地选自含1至10个碳原子的烷基基团,以及
(A-2)70质量%至30质量%的类树脂有机聚硅氧烷,其具有1.5质量%至5.0质量%的烯基基团,并且包含SiO4/2单元、R1 2R2SiO1/2单元和R1 3SiO1/2单元,其中各R1独立地为选自含1至10个碳原子的烷基基团的基团,并且R2为烯基基团;
(B)在分子中具有至少两个硅键合的氢原子的有机聚硅氧烷,并且除氢原子之外的各硅键合的基团独立地选自含1至10个碳原子的烷基基团,其量使得组分(B)中所含的硅键合的氢原子的含量相对1摩尔组分(A)中所含的总烯基基团在0.5至5摩尔的范围内;
(C)0.5至12质量份的直链二烷基聚硅氧烷,其在25℃具有2至10mm2/s的粘度并且具有在两个分子链末端封端的烯基基团;以及
(D)催化量的硅氢加成反应催化剂。
制备本发明的半导体器件的方法包括通过上述可固化有机硅组合物密封半导体元件的步骤。
另外,本发明的半导体器件通过上述方法获得。
本发明的效果
本发明的可固化有机硅组合物的特征是形成具有低表面粘着性和低摩擦系数的固化产品。此外,制备本发明的半导体器件的方法的特征在于:该方法能够以良好的效率制造抗粉尘粘附且抗彼此粘附的半导体器件。另外,本发明的半导体器件的特征在于所述半导体器件抗粉尘粘附且抗彼此粘附。
附图说明
图1是在以可固化有机硅组合物密封之前的半导体器件的局部截面图。
图2是显示使用可固化有机硅组合物填充模具之前的状态的局部截面图。
图3是显示使用可固化有机硅组合物填充模具之后的状态的局部截面图。
图4是显示可固化有机硅组合物的压缩模制的局部截面图。
图5是与固化产品整合的半导体器件的局部截面图。
图6是与固化产品整合的其他半导体器件的局部截面图。
图7是与固化产品整合的另外的半导体器件的局部截面图。
具体实施方式
首先,将详细阐释本发明的可固化有机硅组合物。
组分(A)的有机聚硅氧烷为本发明组合物的主要组分,并由以下部分构成:(A-1)30质量%至70质量%的在25℃具有10至100,000mPa·s粘度的直链有机聚硅氧烷,其在分子中具有至少两个硅键合的烯基基团,并且除烯基基团之外的各硅键合的基团独立地选自含1至10个碳原子的烷基基团;以及(A-2)70质量%至30质量%的类树脂有机聚硅氧烷,其具有1.5质量%至5.0质量%的烯基基团并且包含SiO4/2单元、R1 2R2SiO1/2单元和R1 3SiO1/2单元,在这些式中,各R1独立地为选自含1至10个碳原子的烷基基团的基团,并且R2为烯基基团。
组分(A-1)为赋予本发明组合物的固化产品塑性的组分。组分(A-1)中的烯基基团的示例为乙烯基基团、烯丙基基团、异丙烯基基团、丁烯基基团、己烯基基团和环己烯基基团。组分(A-1)中的烯基基团优选地为具有2至10个碳原子的烯基基团,尤其优选地为乙烯基基团。对直链聚有机硅氧烷中该烯基基团的键合位置无特别限制。该烯基基团可以与分子链末端的硅原子或分子链中的硅原子的任一者键合,或这些烯基基团可以与分子链末端的硅原子和分子链中的硅原子两者键合。组分(A-1)中的烷基基团的示例为甲基基团、乙基基团、丙基基团、环戊基基团、环己基基团或具有1至10个碳原子的类似烷基基团。组分(A-1)中的烷基基团优选地为甲基基团。虽然组分(A-1)的分子结构优选地为基本上直链的,但分子链的一部分可以一定程度地支化。
组分(A-1)在25℃的粘度在10至100,000mPa·s的范围内,优选地在20至10,000mPa·s的范围内,尤其优选地在40至3,000mPa·s的范围内。当组分(A-1)在25℃的粘度大于或等于上述范围的下限时,获得具有所需柔韧性的固化产品。另一方面,当组分(A-1)在25℃的粘度小于上述范围的上限时,获得具有良好处理和可加工性的组合物。
这种类型的组分(A-1)的示例为具有在两个分子链末端封端的二甲基乙烯基甲硅烷氧基基团的聚二甲基硅氧烷、具有在两个分子链末端封端的二甲基乙烯基甲硅烷氧基基团的二甲基硅氧烷-甲基乙烯基硅氧烷共聚物、具有在两个分子链末端封端的三甲基甲硅烷氧基基团的甲基乙烯基聚硅氧烷、具有在两个分子链末端封端的三甲基甲硅烷氧基基团的二甲基硅氧烷-甲基乙烯基硅氧烷共聚物,以及两种或更多种此类化合物的混合物。
组分(A-2)为赋予基底粘附性以及赋予本发明组合物的固化产品强度的组分,并为由SiO4/2单元、R1 2R2SiO1/2单元和R1 3SiO1/2单元构成的类树脂有机聚硅氧烷。在这些式中,各R1独立地为选自具有1至10个碳原子的烷基基团的基团,示例为甲基基团、乙基基团、丙基基团、环戊基基团、环己基基团等。在这些式中,各R2独立地为诸如乙烯基基团、烯丙基基团、异丙烯基基团、丁烯基基团、己烯基基团、环己烯基等烯基基团。R2还优选地为选自具有2至10个碳原子的烯基基团的基团,尤其优选地为乙烯基基团。组分(A-2)包含1.5质量%至5.0质量%的烯基基团,优选地包含2.0质量%至4.0质量%的烯基基团。当在组分(A-2)中烯基基团的含量大于或等于上述范围的下限时,获得的固化产品可以具有所需的高硬度。另一方面,当该烯基基团含量小于或等于上述范围的上限时,获得的固化产品具有所需的柔韧性。表述“质量%的烯基基团”是指烯基基团在转化成乙烯基基团(CH2=CH-)后所计算的占总组分的质量%。
此外,虽然对组分(A-2)中相对于1摩尔SiO4/2单元的R1 2R2SiO1/2单元和R1 3SiO1/2单元的总摩尔数无特别限制,但此数值优选地在0.5至1.4的范围内,还优选地在0.6至1.3的范围内,尤其优选地在0.7至1.2的范围内。当相对于1摩尔SiO4/2的R1 2R2SiO1/2单元和R1 3SiO1/2单元的总摩尔数大于或等于上述范围的下限时,获得具有优选处理和加工能力的组合物。另一方面,当相对于1摩尔SiO4/2单元的R1 2R2SiO1/2单元和R1 3SiO1/2单元的总摩尔数小于或等于上述范围的上限时,获得具有优选柔韧性的固化产品。
虽然对组分(A-2)的分子量无特别限制,但转化成标准聚苯乙烯并通过凝胶渗透色谱法测得的质量平均分子量优选地在3,000至7,000的范围内,还优选地在4,000至6,000的范围内。此外,组分(A-2)可以是两种或更多种类型的有机聚硅氧烷的混合物。当组分(A-2)为两种或更多种类型的有机聚硅氧烷的混合物时,转化成标准聚苯乙烯通过凝胶渗透色谱法测得的质量平均分子量的平均值优选地在上述范围内。
组分(A)由30质量%至70质量%的组分(A-1)和70质量%至30质量%的组分(A2)构成,并且优选地由35质量%至65质量%的组分(A-1)和35质量%至65质量%的组分(A-2)构成。当组分(A-1)的含量大于或等于上述范围的下限时,获得具有良好处理和加工能力的组合物。另一方面,当组合物小于或等于上述范围的上限时,获得具有良好柔韧性的固化产品。
组分(B)的有机聚硅氧烷为本发明组合物的交联剂。虽然对组分(B)的分子结构没有限制,但组分(B)的分子结构的示例为直链、部分支化的直链、支链状、环状和树突结构。组分(B)的分子结构优选地为直链、部分支化的直链或树突结构。对组分(B)中硅键合的氢原子的键合位置无特别限制。例如,组分(B)中的硅键合的氢原子可以与分子链中的硅原子键合,或可以与分子链的末端硅原子键合,或可以与这两种位置的硅原子键合。组分(B)中除氢原子之外的各硅键合的基团独立地为选自烷基基团(诸如甲基基团、乙基基团、丙基基团、环戊基基团、环己基基团等)的基团,并且选地为甲基基团。
虽然对组分(B)的粘度没有限制,但组分(B)在25℃的粘度优选地在1至10,000mm2/s的范围内,尤其优选地在1至1,000mm2/s的范围内。
组分(B)优选地具有至少0.7质量%的硅键合的氢原子。组分(B)尤其优选地为具有至少0.7质量%的硅键合的氢原子并且由SiO4/2单元和HR3 2SiO1/2单元(在该式中,各R3独立地为选自具有1至10个碳原子的烷基基团(诸如甲基基团、乙基基团、丙基基团、环戊基基团、环己基基团等)的基团,并优选地为甲基基团)构成的有机聚硅氧烷,或组分(B)尤其优选地为具有至少0.7质量%的硅键合的氢原子的直链有机聚硅氧烷,其中除氢原子之外的各硅键合的基团独立地为选自具有1至10个碳原子的烷基基团的基团。
这种类型的组分(B)的示例为两个分子链末端被二甲基氢甲硅烷氧基基团封端的二甲基硅氧烷-甲基氢硅氧烷共聚物,两个分子链末端被三甲基甲硅烷氧基基团封端的甲基氢聚硅氧烷,两个分子链末端被三甲基甲硅烷氧基基团封端的二甲基硅氧烷-甲基氢硅氧烷共聚物,由SiO4/2单元和H(CH3)2SiO1/2单元构成的有机聚硅氧烷,由SiO4/2单元、H(CH3)2SiO1/2单元和(CH3)3SiO1/2单元构成的有机聚硅氧烷,以及两种或更多种此类化合物的混合物。
本发明组合物中的组分(B)的含量(以组分(A)中每1摩尔总烯基基团计)在一定的范围内,以使得组分(B)中的硅键合的氢原子在0.5至5摩尔的范围内,并且优选地在0.7至2.5摩尔的范围内。当组分(B)的含量大于或等于上述范围的下限时,获得具有优选固化性的组合物。另一方面,当组分(B)的含量小于或等于上述范围的上限时,获得具有优选耐热性的固化产品。
组分(C)用于降低表面粘着性以及降低得自本发明组合物的固化产品的摩擦系数,并且为在两个分子链末端具有烯基基团的直链二烷基聚硅氧烷。组分(C)具有由重复的二有机硅氧烷单元(D单元)(通常约2至20个单元,优选地约4至18个单元,还优选地约6至11个单元)构成的直链结构。组分(C)在25℃的粘度在2至10mm2/s的范围内,优选地在3至8mm2/s的范围内。上述烯基基团优选地为具有2至10个碳原子的烯基基团,尤其优选地为乙烯基基团。
在本发明组合物中,组分(C)相对于100质量份组分(A)的含量在0.5至12质量份的范围内,优选地在0.5至10质量份的范围内。当组分(C)的含量大于或等于上述范围的下限时,获得具有低表面粘着性的固化产品。另一方面,若组分(C)的含量小于或等于上述范围的上限,则可以抵抗组分(C)从固化产品中溢出。
组分(D)的硅氢加成反应催化剂为用于加速本发明组合物的固化的催化剂,并且例子包括铂基催化剂、铑基催化剂和钯基催化剂。在这些之中,铂基催化剂为优选的。该铂基催化剂为铂基化合物,示例为铂细粉、铂黑、铂负载二氧化硅细粉、铂负载活性炭、氯铂酸、氯铂酸醇溶液、铂的烯烃复合物、铂的烯基硅氧烷复合物等。
在本发明组合物中组分(D)的量为催化量。对组分(D)的量无特别限制,只要该量能够固化本发明组合物即可。具体地讲,在本发明组合物中组分(D)的含量基于该催化剂中的金属原子优选地在0.01至1,000ppm(以质量计)的范围内。当组分(D)的含量大于或等于前述范围的下限时,获得具有足够可固化性的组合物。另一方面,当该含量小于或等于上述范围的上限时,基本不必顾虑获得的固化产品的着色。
除组分(A)至(D)之外,还可以适当地将其他所需的组分添加到本发明组合物中。反应阻滞剂可以作为此类所需组分而添加,以便调节本发明组合物的固化速度。反应阻滞剂的示例为炔醇,诸如2-甲基-3-丁炔-2-醇、3,5-二甲基-1-己炔-3-醇、1-乙炔基环己-1-醇、2-苯基-3-丁炔-2-醇等;烯炔化合物,诸如3-甲基-3-戊烯-1-炔、3,5-二甲基-3-己烯-1-炔等;1,3,5,7-四甲基-1,3,5,7-四乙烯基环四硅氧院、1,3,5,7-四甲基-1,3,5,7-四己烯基环四硅氧烷、苯并三唑等。对本发明组合物中该反应阻滞剂的含量没有限制,并且该反应阻滞剂可以适当地根据模制方法和固化条件加以选择。一般而言,本发明组合物中该反应阻滞剂的含量优选地在10至5,000ppm(以质量计)的范围内。
只要不妨碍本发明的目标,则可以在本发明组合物中共混其他组分,示例为粘附促进剂、阻燃剂、无机填料、抗静电剂等。
虽然对本发明组合物在25℃的粘度无特别限制,但从处理和可加工性(即,可模制性、浇注能力、脱气容易性等)立场来看,粘度优选地在100至10,000mPa·s的范围内,尤其优选地在1,000至7,000mPa·s的范围内。
此外,可以通过将本发明组合物加热至100至250℃的温度而形成固化产品。虽然对该固化产品的硬度没有限制,但在根据JIS K 6253进行测量的情况下,如JIS K 6253中所规定的A型硬度计硬度优选地大于或等于60并且小于或等于95,还优选地大于或等于65并且小于或等于95。
接下来将详细阐释制备半导体器件的方法和本发明的半导体器件。
制备本发明的半导体器件的方法的特征是包括以上述可固化有机硅组合物密封半导体元件的步骤。具体地讲,半导体器件的密封优选地通过上述可固化有机硅组合物使用压缩模制进行。用于密封半导体器件的这种类型的方法的示例为以下步骤:
(i)将发光元件或光接收元件安装在支撑主体上;
(ii)将经成形为与模具中的腔体相同形状的离型膜附接到模具,该模具具有与上述元件相对定位的腔体;
(iii)将可固化有机硅组合物浇注到上述离型膜上;以及
(iv)之后,在将支撑主体抵靠着上述模具压缩的状态下模制上述组合物,以获得以固化产品密封的半导体器件。
根据本发明的方法,使用可固化有机硅组合物密封安装在支撑主体上的发光元件或光接收元件,并且使用能够赋予固化产品所需形状的模制机。然而,就这种类型的模制机而言,可以使用任何常用的模制机。该模制机优选地具有吸气机构以便将离型膜附接到模制机的模具的腔体。该吸气机构用于在可固化有机硅组合物的固化和模制期间使上述离型膜附接到模具的腔体。在组合物的固化和模制之后,吸气机构通过馈入空气而运行以促进离型膜从模具脱离并使得模制产品易于从模具取出。
将使用附图来阐释本发明的方法。图1是显示在使用有机硅组合物的固化产品进行密封之前的半导体器件的局部截面图(图1右端往右部分已省略,与下文所述附图类似)。在图1中,LED芯片2通过晶粒粘结粘合剂等安装在支撑主体上。在该支撑主体1的表面上形成的外部引线或电路(均未示出)通过接合线3电连接到上述LED芯片2。
图2是显示在使用可固化有机硅组合物进行填充之前的状态的局部截面图。承载LED芯片2的支撑主体1与模具4的腔体的位置相对设置。之后,在支撑主体1与模具4之间馈入离型膜5,并且离型膜通过布置在模具4中的吸气机构(未示出)附接到模具的腔体。图3是将可固化有机硅组合物6馈入被离型膜5覆盖的模具4后不久的状态的局部截面图。
图4是显示在可固化有机硅组合物的模制和固化期间的状态的局部截面图。通过抵靠着模具4压缩支撑主体1,离型膜5被夹在支撑主体1与模具4之间,以有机硅组合物密封的区域的周边部分牢靠地密封,并且可能抑制上述组合物的渗漏。
这种类型的离型膜5可以通过吸气等轻易地附接到模具,并且离型膜具有针对可固化有机硅组合物的固化温度的耐热性。这种类型的离型膜的示例为氟树脂膜,诸如聚四氟三乙烯树脂(PTFE)膜、乙烯-四氟乙烯共聚物树脂(ETFE)膜、四氟三乙烯-全氟丙烯共聚物树脂(FEP)膜、聚偏二氟乙烯树脂(PVDF)膜等;聚酯树脂膜,诸如聚对苯二甲酸乙二醇酯树脂(PET)膜等;以及非含氟聚烯烃树脂膜,诸如聚丙烯树脂(PP)膜、环烯烃共聚物树脂(COC)膜等。虽然对这种类型的离型膜的厚度无特别限制,但离型膜的厚度优选地为约0.01mm至0.2mm。
可以使用能够使该组合物固化的任何固化条件作为该可固化有机硅组合物的固化条件。不存在特别限制,此类固化条件的示例优选地为50至200℃、尤其优选地为100至150℃的温度,优选地持续约0.5至60分钟、尤其优选地持续约1至30分钟的时间段。在需要时,可在150至200℃的温度下进行约0.5至4小时的二次固化(后固化)。
图6是显示与有机硅制成的凸透镜整合的本发明的光学器件的局部截面图。在图6中,多个LED芯片安装在单一支撑主体板上。然而,单个半导体器件可以通过使用刀片切割、激光切割等切割该支撑主体而制备。
实例
将使用实践例和比较例更详细地阐释本发明的可固化有机硅组合物、制备半导体器件的方法和半导体器件。注意,实践例中的粘度是在25℃下的值。就本说明书中的术语“粘度”而言,运动粘度(mm2/s单位)是基于JIS Z 8803使用毛细管粘度计测得。另一方面,粘度(mPa·s单位)是使用旋转粘度计测得的值。此外,固化产品的性质测量如下。
[固化产品的硬度]
在150℃下加热可固化有机硅组合物1小时以制备固化产品。使用JISK 6253中规定的A型硬度计测量固化产品的硬度。
[固化产品的动摩擦系数]
通过在150℃下加热可固化有机硅组合物1小时制得1mm厚的片状固化产品。将该片状固化产品设置在TRIBOGEAR型14DR表面测量仪(由新东科学株式会社(Shinto Scientific Co.,Ltd.)制造)中。在使用球形压头施加200g负荷的同时,使球形压头沿水平方向以2,000mm/分钟的速度滑动,并且测量动摩擦系数(μk)。
[固化产品的粉尘附着量]
在150℃下加热可固化有机硅组合物1小时以制备块状5mm方形固化产品。使Dyneon(注册商标)TF超细粉TF9205(8μm平均粒径,由住友3M株式会社(Sumitomo 3M Ltd.)制造)附着到该块状固化产品。使用鼓吹空气从附着有粉末的样品吹掉多余的粉末,并且测量附着粉末的残留量以确定粉末附着量。
此外,按以下方式制备半导体器件。
[制备半导体器件的方法(1)]
通过压缩模制方法,使用可固化有机硅组合物密封半导体元件。即是说,准备压缩模制设备,并且将附接的上部模具和下部模具加热到130℃。将切出穹顶形状的模具用作下部模具。将上面安装有LED芯片的基底设置在上部模具中以使得LED芯片朝下。将乙烯-四氟乙烯共聚物树脂(ETFE)离型膜(AFLEX 50LM)设置在下部模具上,并且使用吸气将离型膜附接到下部模具。在将可固化有机硅组合物浇注到离型膜上之后,将上部模具和下部模具放置在一起,并且通过在130℃下施加3MPa的负荷而压缩模制有机硅组合物3分钟。之后,从模具取出被有机硅树脂密封的基底,然后在150℃下加热该组合件1小时以使可固化有机硅组合物固化。将Dyneon(注册商标)TF超细粉TF9205(8μm平均粒径,由住友3M株式会社制造)喷洒到获得的固化产品上。之后,使用鼓吹空气从前述固化产品吹掉多余的粉末,并且目测观察残余粉末的粘合状态。观察到附着粉末以“×”表示,未观察到附着粉末以“○”表示。
[制备半导体器件的方法(2)]
借助压缩模制方法,使用可固化有机硅组合物密封半导体元件。即是说,准备压缩模制设备,并且将附接的上部模具和下部模具加热到130℃。对于下部模具而言,使用呈10行和10列形式排列100个穹顶状模制品的模具。将承载的LED呈10列和10行形式布置以使得各穹顶能够密封LED芯片的基底抵靠着上部模具设置,以使得LED芯片面朝下。将乙烯-四氟乙烯共聚物树脂(ETFE)离型膜(AFLEX 50LM)设置在下部模具上方,并且使用吸气将离型膜吸引和附接到下部模具。在将可固化有机硅组合物浇注到离型膜上之后,将上部模具和下部模具配合在一起,其中基底处于被夹住的状态,然后在130℃下使用3MPa的负荷压缩模制有机硅组合物3分钟。之后,从模具取出被有机硅树脂密封的基底,并且在烘箱中在150℃下将基底加热处理1小时。获得以实践例1和比较例1的可固化有机硅组合物密封的半导体器件,其具有平坦部分及其上的穹顶形状。将Dyneon(注册商标)TF超细粉TF9205(8μm平均粒径,由住友3M株式会社制造)喷洒到获得的固化产品上。之后,通过鼓风吹掉附着在有机硅固化产品上的多余粉末,并且通过光学显微镜观察残留粉末的粘附状态。观察到附着粉末以“×”表示,而如果未观察到附着粉末,则以“○”表示。
[制备半导体器件的方法(3)]
通过使用由DISCO株式会社(Disco Corp.)制造的DAD 651切割装置以及由DISCO株式会社制造的刀片(B1A862SS)以3mm/秒的馈入速度切割使用上述制备半导体器件的方法(2)密封的LED器件树脂的平坦部分,从而制备单独的半导体器件。之后,使用旋转洗涤设备洗涤这些器件并进行干燥。通过光学显微镜测量密封获得的LED器件的固化有机硅树脂的表面。观察到切屑附着以“×”表示,而若未观察到切屑,则以“○”表示。
[实践例1和2以及比较例1至8]
通过以表1中所示的配混量均匀地混合以下组分而制备可固化有机硅组合物。制得这些可固化有机硅组合物的固化产品并且以上述方式进行评估。此外,通过上述方法(1)至(3)使用这些可固化有机硅组合物制备半导体器件。这些结果示于表1中。
组分(A-1-1):分子两端被二甲基乙烯基甲硅烷氧基基团封端并且具有360mPa·s粘度的二甲基聚硅氧烷(乙烯基基团含量=0.44质量%)
组分(A-1-2):分子两端被二甲基乙烯基甲硅烷氧基基团封端并且具有11,000mPa·s粘度的二甲基聚硅氧烷(乙烯基基团含量=0.14质量%)
组分(A-1-3):分子两端被二甲基乙烯基甲硅烷氧基基团封端并且具有65mPa·s粘度的二甲基聚硅氧烷(乙烯基基团含量=1.5质量%)
组分(A-2-1):具有约5,500的质量平均分子量并且由以下平均单元式表示的有机聚硅氧烷树脂(乙烯基基团含量=3.4质量%)。
[(CH3)2CH2=CHSiO1/2]0.13[(CH3)3SiO1/2]0.45(SiO4/2)0.42
组分(A-2-2):具有约20,000的质量平均分子量并且由以下平均单元式表示的有机聚硅氧烷(乙烯基基团含量=4.2质量%)。
[(CH3)2CH2=CHSiO1/2]0.15[(CH3)3SiO1/2]0.38(SiO4/2)0.47
组分(B-1):具有18mm2/s的动态粘度并且由以下平均单元式表示的有机聚硅氧烷(硅键合的氢原子含量=约0.97质量%)。
[H(CH3)2SiO1/2]8(SiO4/2)4
组分(B-2):分子两端被三甲基甲硅烷氧基基团封端并且具有5mm2/s的运动粘度的甲基氢硅氧烷共聚物(硅键合的氢原子含量:大约1.4质量%)
组分(B-3):分子两端被三甲基甲硅烷氧基基团封端并且具有21mm2/s的运动粘度的聚甲基氢硅氧烷(硅键合的氢原子含量=约1.57质量%)。
组分(B-4):具有1mm2/s的运动粘度并且由以下平均组成式表示的甲基氢环硅氧垸(硅键合的氢原子含量=约1.66质量%)。
[H(CH3)SiO]4.9
组分(C-1):分子两端被二甲基乙烯基甲硅烷氧基基团封端并且具有5mm2/s的运动粘度的二甲基硅氧烷聚合物(乙烯基基团含量=约7.7质量%)。
组分(C-2):具有3.1mm2/s的运动粘度并且由以下平均组成式表示的甲基乙烯基环硅氧烷。
[(CH3)CH2=CHSiO]4
组分(C-3):具有2mm2/s的运动粘度的1,3-二乙烯基四甲基二硅氧烷。
组分(C-4):具有0.65mm2/s的运动粘度的六甲基二硅氧烷。
组分(D-1):铂的1,3-二乙烯基四甲基二硅氧烷复合物的1,3-二乙烯基四甲基二硅氧烷溶液(铂金属含量=约4,000ppm)。
组分(E-1);1-乙炔基环己-1-醇
表1
表1(续)
*在表中,SiH/Vi表示各可固化有机硅组合物中的组分(B-1)至(B-4)中的总硅键合的氢原子摩尔数/1摩尔的组分(A-1-1)至(A-2-2)中的总乙烯基基团。
工业适用性
本发明的可固化有机硅组合物形成具有低表面粘着性并且具有低摩擦系数的固化产品。因此,该可固化有机硅组合物可用作诸如发光二极管(LED)、半导体激光器、光电二极管、光电晶体管、固态成像元件、用于光耦合器的发光元件和光接收元件等半导体元件的密封剂。
标记描述
1 支撑主体
2 LED芯片
3 接合线
4 模具
5 离型膜
6 可固化有机硅组合物
7 固化产品
Claims (7)
1.一种可固化有机硅组合物,其包含:
(A)100质量份的有机聚硅氧烷,其由以下部分构成:
(A-1)30质量%至70质量%的在25℃具有10至100,000mPa·s粘度的直链有机聚硅氧烷,其在分子中具有至少两个硅键合的烯基基团,并且除烯基基团之外的各硅键合的基团独立地选自含1至10个碳原子的烷基基团,以及
(A-2)70质量%至30质量%的类树脂有机聚硅氧烷,其具有1.5质量%至5.0质量%的烯基基团,并且包含SiO4/2单元、R1 2R2SiO1/2单元和R1 3SiO1/2单元,其中各R1独立地为选自含1至10个碳原子的烷基基团的基团,并且R2为烯基基团;
(B)在分子中具有至少两个硅键合的氢原子的有机聚硅氧烷,并且除氢原子之外的各硅键合的基团独立地选自含1至10个碳原子的烷基基团,其量使得组分(B)中所含的硅键合的氢原子的含量相对1摩尔组分(A)中所含的总烯基基团在0.5至5摩尔的范围内;
(C)0.5至12质量份的直链二烷基聚硅氧烷,其在25℃具有2至10mm2/s的粘度并且具有在两个分子链末端封端的烯基基团;以及
(D)催化量的硅氢加成反应催化剂。
2.根据权利要求1所述的可固化有机硅组合物,其中组分(A-2)为类树脂有机聚硅氧烷,其每1摩尔SiO4/2单元具有总计0.5至1.4摩尔R1 2R2SiO1/2单元和R1 3SiO1/2单元。
3.根据权利要求1或2所述的可固化有机硅组合物,其中通过使所述组合物固化获得的固化产品具有根据JIS K 6253测得的大于或等于60并且小于或等于95的A型硬度计硬度。
4.一种制备半导体器件的方法,其包括通过使用根据权利要求1至3中任一项所述的可固化有机硅组合物密封半导体元件的步骤。
5.根据权利要求4所述的制备半导体器件的方法,其还包括用所述可固化有机硅组合物通过压缩模制密封所述半导体元件的步骤。
6.根据权利要求4或5所述的制备半导体器件的方法,其还包括在用所述可固化有机硅组合物密封所述半导体器件之后用刀片切割所述半导体器件以制备单个半导体器件的步骤。
7.种通过根据权利要求4至6中任一项所述的方法获得的半导体器件。
Applications Claiming Priority (3)
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JP2012198803A JP2014051636A (ja) | 2012-09-10 | 2012-09-10 | 硬化性シリコーン組成物、半導体デバイスの製造方法、および半導体デバイス |
JP2012-198803 | 2012-09-10 | ||
PCT/JP2013/074781 WO2014038728A2 (en) | 2012-09-10 | 2013-09-06 | Curable silicone composition, method for producing semiconductor device, and semiconductor device |
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CN104603181A true CN104603181A (zh) | 2015-05-06 |
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US (1) | US20150235872A1 (zh) |
EP (1) | EP2892946A2 (zh) |
JP (1) | JP2014051636A (zh) |
KR (1) | KR101907378B1 (zh) |
CN (1) | CN104603181A (zh) |
MY (1) | MY180275A (zh) |
TW (1) | TW201410745A (zh) |
WO (1) | WO2014038728A2 (zh) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108699421A (zh) * | 2016-02-23 | 2018-10-23 | 美国陶氏有机硅公司 | 选择性粘附硅橡胶 |
CN110997814A (zh) * | 2017-08-24 | 2020-04-10 | 美国陶氏有机硅公司 | 可注塑的有机硅组合物 |
Families Citing this family (4)
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JP6862334B2 (ja) * | 2017-12-05 | 2021-04-21 | 信越化学工業株式会社 | 硬化性シリコーン剥離剤組成物 |
JP7092196B2 (ja) * | 2018-08-01 | 2022-06-28 | 信越化学工業株式会社 | シリコーン粘着剤組成物及びこれを用いた粘着テープ又は粘着フィルム |
JP2021001257A (ja) * | 2019-06-20 | 2021-01-07 | 信越化学工業株式会社 | 室温硬化型シリコーンゴム組成物 |
JP7365798B2 (ja) * | 2019-07-03 | 2023-10-20 | ダウ・東レ株式会社 | シリコーンゲル組成物、その硬化物、電子部品封止剤、電子部品、および半導体チップの保護方法 |
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JP4519869B2 (ja) * | 2007-03-05 | 2010-08-04 | 株式会社東芝 | 半導体装置 |
TWI458780B (zh) | 2007-07-31 | 2014-11-01 | Dow Corning Toray Co Ltd | 提供高透明矽酮硬化物之硬化性矽酮組合物 |
JP5136963B2 (ja) * | 2008-03-24 | 2013-02-06 | 信越化学工業株式会社 | 硬化性シリコーンゴム組成物及び半導体装置 |
JP5475295B2 (ja) | 2009-02-02 | 2014-04-16 | 東レ・ダウコーニング株式会社 | 高透明のシリコーン硬化物を与える硬化性シリコーン組成物 |
-
2012
- 2012-09-10 JP JP2012198803A patent/JP2014051636A/ja not_active Withdrawn
-
2013
- 2013-09-06 CN CN201380044524.4A patent/CN104603181A/zh active Pending
- 2013-09-06 MY MYPI2015000456A patent/MY180275A/en unknown
- 2013-09-06 EP EP13770978.8A patent/EP2892946A2/en not_active Withdrawn
- 2013-09-06 KR KR1020157006054A patent/KR101907378B1/ko active IP Right Grant
- 2013-09-06 WO PCT/JP2013/074781 patent/WO2014038728A2/en active Application Filing
- 2013-09-06 US US14/426,890 patent/US20150235872A1/en not_active Abandoned
- 2013-09-09 TW TW102132492A patent/TW201410745A/zh unknown
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108699421A (zh) * | 2016-02-23 | 2018-10-23 | 美国陶氏有机硅公司 | 选择性粘附硅橡胶 |
CN110997814A (zh) * | 2017-08-24 | 2020-04-10 | 美国陶氏有机硅公司 | 可注塑的有机硅组合物 |
CN110997814B (zh) * | 2017-08-24 | 2022-08-23 | 美国陶氏有机硅公司 | 可注塑的有机硅组合物 |
Also Published As
Publication number | Publication date |
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KR101907378B1 (ko) | 2018-10-12 |
US20150235872A1 (en) | 2015-08-20 |
WO2014038728A2 (en) | 2014-03-13 |
EP2892946A2 (en) | 2015-07-15 |
MY180275A (en) | 2020-11-26 |
WO2014038728A3 (en) | 2014-05-01 |
JP2014051636A (ja) | 2014-03-20 |
KR20150054811A (ko) | 2015-05-20 |
TW201410745A (zh) | 2014-03-16 |
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