CN106488949A - 粘合促进剂、固化性有机硅组合物及半导体装置 - Google Patents
粘合促进剂、固化性有机硅组合物及半导体装置 Download PDFInfo
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- CN106488949A CN106488949A CN201580035513.9A CN201580035513A CN106488949A CN 106488949 A CN106488949 A CN 106488949A CN 201580035513 A CN201580035513 A CN 201580035513A CN 106488949 A CN106488949 A CN 106488949A
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- GQUJEMVIKWQAEH-UHFFFAOYSA-N titanium(III) oxide Chemical compound O=[Ti]O[Ti]=O GQUJEMVIKWQAEH-UHFFFAOYSA-N 0.000 description 1
- JOFWLTCLBGQGBO-UHFFFAOYSA-N triazolam Chemical compound C12=CC(Cl)=CC=C2N2C(C)=NN=C2CN=C1C1=CC=CC=C1Cl JOFWLTCLBGQGBO-UHFFFAOYSA-N 0.000 description 1
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- 239000011667 zinc carbonate Substances 0.000 description 1
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Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K5/544—Silicon-containing compounds containing nitrogen
- C08K5/5455—Silicon-containing compounds containing nitrogen containing at least one group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K5/56—Organo-metallic compounds, i.e. organic compounds containing a metal-to-carbon bond
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
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- H01L23/31—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/31—Structure, shape, material or disposition of the layer connectors after the connecting process
- H01L2224/32—Structure, shape, material or disposition of the layer connectors after the connecting process of an individual layer connector
- H01L2224/321—Disposition
- H01L2224/32151—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
- H01L2224/32221—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
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Abstract
本发明涉及平均式表示的粘合促进剂;至少包含(A)一分子中具有至少2个烯基的有机聚硅氧烷、(B)一分子中具有至少2个与硅原子结合的氢原子的有机氢化聚硅氧烷、(C)所述粘合促进剂及(D)氢化硅烷化反应用催化剂的固化性有机硅组合物;以及通过所述固化性有机硅组合物的固化物对半导体元件密封而成的半导体装置。本发明提供新型的粘合促进剂、含有该粘合促进剂而对于各种基材形成粘合性优异的固化物的固化性有机硅组合物、以及使用该固化性有机硅组合物而成的可靠性优异的光半导体装置。
Description
技术领域
本发明涉及新型的粘合促进剂、含有该粘合促进剂的固化性有机硅组合物、以及使用该固化性有机硅组合物而成的半导体装置。
背景技术
一般而言,氢化硅烷化反应固化性有机硅组合物对于金属或有机树脂、特别是热塑性树脂等基材的粘合性不足,因此例如提出有:固化性有机硅组合物,其包含:具有结合于硅原子的烯基的有机聚硅氧烷、具有与硅原子结合的氢原子的有机氢化聚硅氧烷、包含异氰脲酸衍生物的粘合促进剂、以及氢化硅烷化反应用催化剂,其中,所述异氰脲酸衍生物分别具有:选自环氧基、环氧丙氧基、烷氧基甲硅烷基中的一种以上的官能团、选自交联性的乙烯基与氢化硅烷基(Si-H基团)中的一种以上的基团(参照专利文献1);固化性有机硅组合物,其包含:一分子中具有至少2个烯基的有机聚硅氧烷、一分子中具有至少2个与硅原子结合的氢原子的有机氢化聚硅氧烷、一分子中具有烯丙基、环氧基及有机甲硅烷氧基的含异氰脲环有机硅氧烷、以及氢化硅烷化反应用催化剂(参照专利文献2);以及固化性有机硅组合物,其包含:具有结合于硅原子的烯基的有机聚硅氧烷、具有结合于硅原子的氢原子的有机氢化聚硅氧烷、粘合促进剂、以及氢化硅烷化反应用催化剂,其中,所述粘合促进剂含有:分别具有烷氧基甲硅烷基和/或环氧基和2价含甲硅烷氧基单元的基团的异氰脲酸衍生物、具有烷氧基和/或环氧基且不含异氰脲环的硅烷或硅氧烷化合物(参照专利文献3)。
但是,即使是这些固化有机硅组合物,在固化过程中对于接触的基材也存在粘合力不充分的问题。
现有技术文献
专利文献
专利文献1:日本特开2010-065161号公报
专利文献2:日本特开2011-057755号公报
专利文献3:日本特开2011-208120号公报
发明内容
发明所要解决的问题
本发明的目的在于提供新型的粘合促进剂、含有该粘合促进剂、对于各种基材形成粘合性优异的固化物的固化性有机硅组合物、以及使用该固化性有机硅组合物而成的可靠性优异的半导体装置。
解决问题的技术方案
本发明的粘合促进剂由以下平均式表示:
[化学式1]
(式中,R1为相同或不同的不具有脂肪族不饱和键的碳原子数1~12的一价烃基,X为环氧丙氧基烷基、环氧基环烷基烷基或环氧烷基,m和n为满足1<m<3、1<n<3、且m+n=3的数,p为1~50的整数)。
本发明的固化性有机硅组合物含有上述的粘合促进剂,优选通过氢化硅烷化反应固化,进一步优选至少包含以下组分:
(A)一分子中具有至少2个烯基的有机聚硅氧烷100质量份;
(B)一分子中具有至少2个与硅原子结合的氢原子的有机氢化聚硅氧烷{其量为相对于(A)成分和(C)成分中所含的烯基合计每1摩尔,使提供与硅原子结合的氢原子的量为0.1~10摩尔};
(C)上述的粘合促进剂0.01~20质量份;及
(D)氢化硅烷化反应用催化剂(其量为促进本组合物的固化的量)。
本发明的半导体装置通过上述固化性有机硅组合物的固化物对半导体元件密封而成,优选该半导体元件为发光元件。
发明效果
本发明的粘合促进剂为新型的化合物,其特征在于可以对固化性有机硅组合物赋予优异的粘合性。此外,本发明的固化性有机硅组合物的特征在于,在固化过程中对于接触的各种基材形成粘合性优异的固化物。由于本发明的半导体装置通过上述组合物的固化物对半导体元件进行密封,因此其特征还在于可靠性优异。
附图说明
图1是作为本发明的半导体装置一例的LED的剖面图。
具体实施方式
首先,对本发明的粘合促进剂详细地进行说明。
本发明的粘合促进剂由平均式:
[化学式2]
表示。
式中,R1为相同或不同的不具有脂肪族不饱和键的碳原子数1~12的一价烃基。具体而言,可示例:甲基、乙基、丙基、异丙基、丁基、异丁基、叔丁基、戊基、新戊基、己基、环己基、庚基、辛基、壬基、癸基、十一烷基、十二烷基等烷基;苯基、甲苯基、二甲苯基、萘基等芳基;苄基、苯乙基、苯丙基等芳烷基;以及将这些基团的氢原子中的一部分或全部被氟原子、氯原子、溴原子等卤素原子取代的基团,优选为甲基、苯基。
式中,X为环氧丙氧基烷基、环氧基环烷基烷基或环氧烷基。作为环氧丙氧基烷基,可示例2-环氧丙氧基乙基、3-环氧丙氧基丙基、4-环氧丙氧基丁基。作为环氧基环烷基烷基,可示例2-(3,4-环氧环己基)-乙基、3-(3,4-环氧环己基)-丙基。作为环氧烷基,可示例3,4-环氧丁基、7,8-环氧辛基。
式中,m和n为满足1<m<3、1<n<3、且m+n=3的数。这是因为:当m为大于1的数、即n为小于3的数时,可以提高固化性有机硅组合物的粘合性,另一方面,当m为小于3的数、即n为大于1的数时,本粘合促进剂容易与氢化硅烷化反应固化性有机硅组合物中的与硅原子结合的氢原子进行反应。
式中,p为1~50的范围内的数,从可以提高固化性有机硅组合物的粘合性方面考虑,优选为1~30的范围内的数,进一步优选为1~10的范围内的数。
制备这种粘合促进剂的方法并没有限定,例如可举出使三烯丙基异氰脲酸酯与平均式:
[化学式3]
(式中,R1、X及p与上述相同)
表示的硅氧烷在氢化硅烷化反应用催化剂的存在下进行氢化硅烷化反应的方法。
在上述硅氧烷中,式中,R1为相同或不同的不具有脂肪族不饱和键的碳原子数1~12的一价烃基,可示例与上述同样的基团。此外,式中,X为环氧丙氧基烷基、环氧基环烷基烷基或环氧烷基,可示例与上述同样的基团。此外,式中,p为1~50的范围内的数,优选为1~30的范围内的数,进一步优选为1~10的范围内的数。
在上述的制备方法中,相对于三烯丙基异氰脲酸酯中的烯丙基,需要使上述硅氧烷中与硅原子结合的氢原子为小于当量的量进行反应,相对于三烯丙基异氰脲酸酯中的烯丙基3摩尔,优选使上述硅氧烷中与硅原子结合的氢原子为0.5摩尔~2摩尔的范围内的量、进一步优选为0.75摩尔~1.5摩尔的范围内的量进行反应。
作为上述的制备方法中所使用的氢化硅烷化反应用催化剂,可示例铂系催化剂、铑系催化剂、钯系催化剂,特别优选为铂系催化剂。作为该铂系催化剂,可示例:铂微粉末、铂黑、负载铂的二氧化硅微粉末、负载铂的活性炭、氯铂酸、氯铂酸的乙醇溶液、铂的烯烃络合物、铂的烯基硅氧烷络合物等铂系化合物。
在上述的制备方法中,可以使用有机溶剂。作为可以使用的有机溶剂,可示例:醚类、酮类、乙酸酯类、芳香族或脂肪烃、γ-丁内酯、以及它们两种以上的混合物。作为优选的有机溶剂,可示例:丙二醇单甲醚、丙二醇单甲醚乙酸酯、丙二醇单乙醚、丙二醇单丙醚、丙二醇单丁醚、丙二醇单叔丁醚、γ-丁内酯、甲苯、二甲苯。
在上述的制备方法中,通过加热而促进氢化硅烷化反应。在使用有机溶剂的情况下,优选在其回流温度下进行反应。
下面,对本发明的固化性有机硅组合物详细地进行说明。
本发明的固化性有机硅组合物的特征在于,含有上述的粘合促进剂。这种固化性有机硅组合物的固化机理并没有限定,可示例氢化硅烷化反应、缩合反应、自由基反应,优选为氢化硅烷化反应。作为该氢化硅烷化反应固化性有机硅组合物,优选至少包含以下组分:
(A)一分子中具有至少2个烯基的有机聚硅氧烷100质量份;
(B)一分子中具有至少2个与硅原子结合的氢原子的有机氢化聚硅氧烷{其量为相对于(A)成分和(C)成分中所含的烯基合计每1摩尔,使提供与硅原子结合的氢原子的量为0.1~10摩尔};
(C)上述的粘合促进剂0.01~20质量份;及
(D)氢化硅烷化反应用催化剂。
(A)成分作为本组合物的主剂,其为一分子中具有至少2个烯基的有机聚硅氧烷。作为(A)成分中的烯基,可示例:乙烯基、烯丙基、丁烯基、戊烯基、己烯基、庚烯基、辛烯基、壬烯基、癸烯基、十一烯基、十二烯基等碳原子数为2~12个烯基,优选为乙烯基。此外,作为(A)成分中除了烯基以外的结合于硅原子的基团,可示例:甲基、乙基、丙基、异丙基、丁基、异丁基、叔丁基、戊基、新戊基、己基、环己基、庚基、辛基、壬基、癸基、十一烷基、十二烷基等碳原子数为1~12个的烷基;苯基、甲苯基、二甲苯基、萘基等碳原子数为6~20个的芳基;苄基、苯乙基、苯丙基等碳原子数为7~20个的芳烷基;将这些基团的氢原子中的一部分或全部被氟原子、氯原子、溴原子等卤素原子取代的基团。予以说明,在(A)成分中的硅原子中,在不损害本发明的目的的范围内可以具有少量的羟基或甲氧基、乙氧基等烷氧基。
(A)成分的分子结构并没有特别限定,可示例直链状、具有一部分支链的直链状、支链状、环状及三维网状结构。(A)成分可以为具有这些分子结构的一种有机聚硅氧烷、或具有这些分子结构的两种以上的有机聚硅氧烷混合物。
(A)成分在25℃时的性状并没有特别限定,例如为液态状或固体状。在(A)成分为液态状的情况下,其在25℃时的粘度优选为1~1,000,000mPa·s的范围内,特别优选为10~1,000,000mPa·s的范围内。予以说明,该粘度例如可以通过根据JIS K 7117-1使用B型粘度计的测定而求出。
作为这种(A)成分,除了分子链两末端由二甲基乙烯基甲硅烷氧基封端的二甲基聚硅氧烷、分子链两末端由二甲基乙烯基甲硅烷氧基封端的二甲基硅氧烷-甲基乙烯基硅氧烷共聚物、分子链两末端由二甲基乙烯基甲硅烷氧基封端的二甲基硅氧烷-甲基苯基硅氧烷共聚物、分子链两末端由二甲基乙烯基甲硅烷氧基封端的甲基苯基聚硅氧烷、分子链两末端由三甲基甲硅烷氧基封端的二甲基硅氧烷-甲基乙烯基硅氧烷共聚物、分子链两末端由三甲基甲硅烷氧基封端的二甲基硅氧烷-甲基乙烯基硅氧烷-甲基苯基硅氧烷共聚物、包含(CH3)3SiO1/2单元和(CH3)2(CH2=CH)SiO1/2单元和SiO4/2单元的共聚物、包含(CH3)2(CH2=CH)SiO1/2单元和SiO4/2单元的共聚物之外,可示例如下的有机聚硅氧烷。予以说明,式中,Me、Vi、Ph分别表示甲基、乙烯基、苯基,x、x’分别为1~5,000的整数。
ViMe2SiO(Me2SiO)xSiMe2Vi
ViPhMeSiO(Me2SiO)xSiMePhVi
ViPh2SiO(Me2SiO)xSiPh2Vi
ViMe2SiO(Me2SiO)x(Ph2SiO)x'SiMe2Vi
ViPhMeSiO(Me2SiO)x(Ph2SiO)x'SiPhMeVi
ViPh2SiO(Me2SiO)x(Ph2SiO)x'SiPh2Vi
ViMe2SiO(MePhSiO)zSiMe2Vi
MePhViSiO(MePhSiO)xSiMePhVi
Ph2ViSiO(MePhSiO)xSiPh2Vi
ViMe2SiO(Ph2SiO)x(PhMeSiO)x'SiMe2Vi
ViPhMeSiO(Ph2SiO)x(PhMeSiO)x'SiPhMeVi
ViPh2SiO(Ph2SiO)x(PhMeSiO)x'SiPh2Vi
(B)成分为本组合物的交联剂,为一分子中具有至少2个与硅原子结合的氢原子的有机氢化聚硅氧烷。作为(B)成分的分子结构,例如可举出直链状、具有一部分支链的直链状、支链状、环状、树枝状,优选为直链状、具有一部分支链的直链状、树枝状。(B)成分中与硅原子结合的氢原子的结合位置并没有限定,例如可举出分子链的末端和/或侧链。此外,作为(B)成分中除了氢原子以外的结合于硅原子的基团,可示例:甲基、乙基、丙基等烷基;苯基、甲苯基、二甲苯基等芳基;苄基、苯乙基等芳烷基;3-氯丙基、3,3,3-三氟丙基等卤化烷基,优选为甲基、苯基。此外,(B)成分的粘度并没有限定,优选在25℃时的粘度为1~10,000mPa·s的范围内,特别优选为1~1,000mPa·s的范围内。
作为这种(B)成分,除了1,1,3,3-四甲基二硅氧烷、1,3,5,7-四甲基环四硅氧烷、三(二甲基氢甲硅烷氧基)甲基硅烷、三(二甲基氢甲硅烷氧基)苯基硅烷、1-环氧丙氧基丙基-1,3,5,7-四甲基环四硅氧烷、1,5-环氧丙氧基丙基-1,3,5,7-四甲基环四硅氧烷、1-环氧丙氧基丙基-5-三甲氧基甲硅烷基乙基-1,3,5,7-四甲基环四硅氧烷、分子链两末端由三甲基甲硅烷氧基封端的甲基氢聚硅氧烷、分子链两末端由三甲基甲硅烷氧基封端的二甲基硅氧烷-甲基氢硅氧烷共聚物、分子链两末端由二甲基氢甲硅烷氧基封端的二甲基聚硅氧烷、分子链两末端由二甲基氢甲硅烷氧基封端的二甲基硅氧烷-甲基氢硅氧烷共聚物、分子链两末端由三甲基甲硅烷氧基封端的甲基氢硅氧烷-二苯基硅氧烷共聚物、分子链两末端由三甲基甲硅烷氧基封端的甲基氢硅氧烷-二苯基硅氧烷-二甲基硅氧烷共聚物、三甲氧基硅烷的水解缩合物、包含(CH3)2HSiO1/2单元和SiO4/2单元的共聚物、以及包含(CH3)2HSiO1/2单元和SiO4/2单元和(C6H5)SiO3/2单元的共聚物之外,可示例如下的有机氢化聚硅氧烷。予以说明,式中,Me、Vi、Ph、Naph分别表示甲基、乙烯基、苯基、萘基,y、y’分别为1~100的整数,c、d、e、f为正数,其中,c、d、e、f的合计为1。
HMe2SiO(Ph2SiO)ySiMe2H
HMePhSiO(Ph2SiO)ySiMePhH
HMeNaphSiO(Ph2SiO)ySiMeNaphH
HMePhSiO(Ph2SiO)y(MePhSiO)y'SiMePhH
HMePhSiO(Ph2SiO)y(Me2SiO)y'SiMePhH
(HMe2SiO1/2)c(PhSiO3/2)d
(HMePhSiO1/2)c(PhSiO3/2)d
(HMePhSiO1/2)c(NaphSiO3/2)d
(HMe2SiO1/2)c(NaphSiO3/2)d
(HMePhSiO1/2)c(HMe2SiO1/2)d(PhSiO3/2)e
(HMe2SiO1/2)c(Ph2SiO2/2)d(PhSiO3/2)e
(HMePhSiO1/2)c(Ph2SiO2/2)d(PhSiO3/2)e
(HMe2SiO1/2)c(Ph2SiO2/2)d(NaphSiO3/2)e
(HMePhSiO1/2)c(Ph2SiO2/2)d(NaphSiO3/2)e
(HMePhSiO1/2)c(HMe2SiO1/2)d(NaphSiO3/2)e
(HMePhSiO1/2)c(HMe2SiO1/2)d(Ph2SiO2/2)e(NaphSiO3/2)f
(HMePhSiO1/2)c(HMe2SiO1/2)d(Ph2SiO2/2)e(PhSiO3/2)f
(B)成分的含量为相对于(A)成分和(C)成分中所含的烯基合计每1摩尔,使本成分中与硅原子结合的氢原子的量为0.1~10摩尔,优选的量为0.5~5摩尔。这是因为:当(B)成分的含量为上述范围的上限以下时,得到的固化物的机械特性良好,另一方面,当(B)成分的含量为上述范围的下限以上时,得到的组合物的固化性良好。
(C)成分为用于对本组合物赋予粘合性的粘合促进剂,为如上所述的化合物。(C)成分的含量相对于(A)成分100质量份为0.01~20质量份的范围内,优选为0.1~10质量份的范围内。这是因为:当(C)成分的含量为上述范围的下限以上时,可以对得到的组合物赋予充分的粘合性,另一方面,当(C)成分的含量为上述范围的上限以下时,不易阻碍得到的组合物的固化性,此外可以抑制得到的固化物的着色等。
(D)成分为用于促进本组合物的固化的氢化硅烷化反应用催化剂,可示例铂系催化剂、铑系催化剂、钯系催化剂。特别是由于可以显著地促进本组合物的固化,因此(D)成分优选为铂系催化剂。作为该铂系催化剂,可示例铂微粉末、氯铂酸、氯铂酸的乙醇溶液、铂-烯基硅氧烷络合物、铂-烯烃络合物、铂-羰基络合物,优选为铂-烯基硅氧烷络合物。
(D)成分的含量为促进本组合物的固化的量。具体而言,相对于本组合物,使(D)成分中的催化剂金属以质量单位计优选的量为0.01~500ppm的范围内,进一步优选的量为0.01~100ppm的范围内,特别优选的量为0.01~50ppm的范围内。
另外,在本组合物中,作为其它任意的成分,可以含有2-甲基-3-丁炔-2-醇、3,5-二甲基-1-己炔-3-醇、2-苯基-3-丁炔-2-醇等炔醇;3-甲基-3-戊烯-1-炔、3,5-二甲基-3-己烯-1-炔等烯炔化合物;1,3,5,7-四甲基-1,3,5,7-四乙烯基环四硅氧烷、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(E)氢化硅烷化反应抑制剂。在本组合物中,(E)成分的含量并没有限定,相对于上述(A)成分~(D)成分的合计100质量份,优选为0.0001~5质量份的范围内。
在本组合物中,为了提高相对于在固化过程中接触的基材的固化物的粘合性,还可以含有除了(C)成分以外的粘合促进剂。作为该粘合促进剂,优选一分子中具有至少1个结合于硅原子的烷氧基的有机硅化合物。作为该烷氧基,可示例甲氧基、乙氧基、丙氧基、丁氧基、甲氧基乙氧基,特别优选甲氧基。此外,作为除了结合于该有机硅化合物硅原子的烷氧基以外的基团,可示例:烷基、烯基、芳基、芳烷基、卤化烷基等取代或未取代的一价烃基;3-环氧丙氧基丙基、4-环氧丙氧基丁基等环氧丙氧基烷基;2-(3,4-环氧环己基)乙基、3-(3,4-环氧环己基)丙基等环氧环己基烷基;3,4-环氧丁基、7,8-环氧辛基等环氧烷基;3-甲基丙烯酰氧基丙基等含丙烯酸基的一价有机基团;氢原子。该有机硅化合物优选具有与硅原子结合的烯基或与硅原子结合的氢原子。作为这种有机硅化合物,可示例:有机硅烷化合物、有机硅氧烷低聚物、烷基硅酸盐。作为该有机硅氧烷低聚物或烷基硅酸盐的分子结构,可示例直链状、具有一部分支链的直链状、支链状、环状、网状,特别优选为直链状、支链状、网状。作为这种有机硅化合物,可示例:3-环氧丙氧基丙基三甲氧基硅烷、2-(3,4-环氧环己基)乙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷等硅烷化合物;一分子中分别具有至少各1个与硅原子结合的烯基或与硅原子结合的氢原子及与硅原子结合的烷氧基的硅氧烷化合物;由下列化合物构成的混合物:具有至少1个与硅原子结合的烷氧基的硅烷化合物或硅氧烷化合物、一分子中分别具有至少各1个与硅原子结合的羟基及与硅原子结合的烯基的硅氧烷化合物;甲基聚硅酸盐;乙基聚硅酸盐;含环氧基的乙基聚硅酸盐。
在本组合物中,还可以配入荧光体,其用于对从用本组成的固化物密封或包覆而成的发光元件发出的光的波长进行转换而得到所期望波长的光。作为这种荧光体,可示例被广泛利用于发光二极管(LED)的包含氧化物系荧光体、氧氮化物系荧光体、氮化物系荧光体、硫化物系荧光体、氧硫化物系荧光体等的黄色、红色、绿色、蓝色发光荧光体。作为氧化物系荧光体,可示例:包含铈离子的钇、铝、石榴石系的YAG系绿色~黄色发光荧光体、包含铈离子的铽、铝、石榴石系的TAG系黄色发光荧光体、以及包含铈或铕离子的硅酸盐系绿色~黄色发光荧光体。作为氧氮化物系荧光体,可示例包含铕离子的硅、铝、氧、氮系的赛隆(SiAlON)系红色~绿色发光荧光体。作为氮化物系荧光体,可示例包含铕离子的钙、锶、铝、硅、氮系的CASN(CaAlSiN3)系红色发光荧光体。作为硫化物系荧光体,可示例包含铜离子或铝离子的ZnS系绿色发色荧光体。作为氧硫化物系荧光体,可示例包含铕离子的Y2O2S系红色发光荧光体。这些荧光体可以使用一种或两种以上的混合物。荧光体的含量相对于(A)成分~(D)成分的合计量为0.1~70质量%的范围内,优选为1~20质量%的范围内。
另外,在本组合物中,只要不损害本发明的目的,则作为其它任意的成分,可以含有二氧化硅、玻璃、氧化铝、氧化锌等无机质填充剂;聚甲基丙烯酸酯树脂等有机树脂微粉末;耐热剂、染料、颜料、阻燃剂、溶剂等。
为了充分地抑制空气中的含硫气体导致的光半导体装置中的银电极或基板镀银的变色,还可以含有选自由表面包覆有选自由Al、Ag、Cu、Fe、Sb、Si、Sn、Ti、Zr及稀土元素构成的组中的至少一种元素的氧化物的氧化锌微粉末、以不具有烯基的有机硅化合物进行表面处理的氧化锌微粉末、以及碳酸锌的水合物微粉末构成的组中平均粒径为0.1nm~5μm的至少一种微粉末。
在表面包覆有氧化物的氧化锌微粉末中,作为稀土元素,可示例钇、铈、铕。作为氧化锌微粉末表面的氧化物,可示例:Al2O3、AgO、Ag2O、Ag2O3、CuO、Cu2O、FeO、Fe2O3、Fe3O4、Sb2O3、SiO2、SnO2、Ti2O3、TiO2、Ti3O5、ZrO2、Y2O3、CeO2、Eu2O3、以及这些氧化物的两种以上的混合物。
在以有机硅化合物进行表面处理的氧化锌微粉末中,该有机硅化合物不具有烯基,可示例:有机硅烷、有机硅氮烷、聚甲基硅氧烷、有机氢化聚硅氧烷及有机硅氧烷低聚物,具体而言,可示例:三甲基氯硅烷、二甲基氯硅烷、甲基三氯硅烷等有机氯硅烷;甲基三甲氧基硅烷、甲基三乙氧基硅烷、苯基三甲氧基硅烷、乙基三甲氧基硅烷、正丙基三甲氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷等有机三烷氧基硅烷;二甲基二甲氧基硅烷、二甲基二乙氧基硅烷、二苯基二甲氧基硅烷等二有机二烷氧基硅烷;三甲基甲氧基硅烷、三甲基乙氧基硅烷等三有机烷氧基硅烷;这些有机烷氧基硅烷的部分缩合物;六甲基二硅氮烷等有机硅氮烷;聚甲基硅氧烷、有机氢化聚硅氧烷、具有硅烷醇基或烷氧基的有机硅氧烷低聚物、包含R2SiO3/2单元(式中,R2为甲基、乙基、丙基等烷基;苯基等芳基中所示例的除烯基之外的一价烃基)或SiO4/2单元的具有硅烷醇基或烷氧基的树脂状有机聚硅氧烷。
另外,在本组合物中,从可以进一步抑制空气中的含硫气体导致的银电极或基板镀银的变色方面考虑,作为任意的成分,可以含有三唑系化合物。具体而言,可示例:1H-1,2,3-三唑、2H-1,2,3-三唑、1H-1,2,4-三唑、4H-1,2,4-三唑、2-(2'-羟基-5'-甲基苯基)苯并三唑、1H-1,2,3-三唑、2H-1,2,3-三唑、1H-1,2,4-三唑、4H-1,2,4-三唑、苯并三唑、甲苯基三唑、羧基苯并三唑、1H-苯并三唑-5-羧酸甲酯、3-氨基-1,2,4-三唑、4-氨基-1,2,4-三唑、5-氨基-1,2,4-三唑、3-巯基-1,2,4-三唑、氯苯并三唑、硝基苯并三唑、氨基苯并三唑、环己烷[1,2-d]三唑、4,5,6,7-四羟基甲苯基三唑、1-羟基苯并三唑、乙基苯并三唑、萘并三唑、1-N,N-双(2-乙基己基)-[(1,2,4-三唑-1-基)甲基]胺、1-[N,N-双(2-乙基己基)氨基甲基]苯并三唑、1-[N,N-双(2-乙基己基)氨基甲基]甲苯基三唑、1-[N,N-双(2-乙基己基)氨基甲基]羧基苯并三唑、1-[N,N-双(2-羟基乙基)-氨基甲基]苯并三唑、1-[N,N-双(2-羟基乙基)-氨基甲基]甲苯基三唑、1-[N,N-双(2-羟基乙基)-氨基甲基]羧基苯并三唑、1-[N,N-双(2-羟基丙基)氨基甲基]羧基苯并三唑、1-[N,N-双(1-丁基)氨基甲基]羧基苯并三唑、1-[N,N-双(1-辛基)氨基甲基]羧基苯并三唑、1-(2',3'-二羟基丙基)苯并三唑、1-(2',3'-二羧基乙基)苯并三唑、2-(2'-羟基-3',5'-二叔丁基苯基)苯并三唑、2-(2'-羟基-3',5'-戊基苯基)苯并三唑、2-(2'-羟基-4'-辛氧基苯基)苯并三唑、2-(2'-羟基-5'-叔丁基苯基)苯并三唑、1-羟基苯并三唑-6-羧酸、1-油酰苯并三唑、1,2,4-三唑-3-醇、5-氨基-3-巯基-1,2,4-三唑、5-氨基-1,2,4-三唑-3-羧酸、1,2,4-三唑-3-羧酰胺、4-氨基尿唑及1,2,4-三唑-5-酮。该三唑系化合物的含量并没有特别限定,使在本组合物中以质量单位计的量为0.01ppm~3%的范围内,优选的量为0.1ppm~1%的范围内。
另外,在本组合物中,为了抑制得到的固化物的热老化导致的裂纹,作为其它任意的成分,可以含有含铈有机聚硅氧烷。该含铈有机聚硅氧烷例如可以通过氯化铈或羧酸的铈盐与含硅烷醇基有机聚硅氧烷的碱金属盐的反应而制备。
作为上述羧酸的铈盐,可示例:2-乙基己酸铈、环烷酸铈、油酸铈、月桂酸铈及硬脂酸铈。
另外,作为上述含硅烷醇基有机聚硅氧烷的碱金属盐,可示例:分子链两末端由硅烷醇基封端的二有机聚硅氧烷的钾盐、分子链两末端由硅烷醇基封端的二有机聚硅氧烷的钠盐、分子链单末端由硅烷醇基封端且另一个分子链单末端由三有机甲硅烷氧基封端的二有机聚硅氧烷的钾盐、分子链单末端由硅烷醇基封端且另一个分子链单末端由三有机甲硅烷氧基封端的二有机聚硅氧烷的钠盐。予以说明,作为该有机聚硅氧烷中结合于硅原子的基团,可示例:甲基、乙基、丙基、异丙基、正丁基、异丁基、叔丁基、正戊基、新戊基、己基、环己基、庚基、辛基、壬基、癸基、十一烷基及十二烷基等碳原子数为1~12个的烷基;苯基、甲苯基、二甲苯基及萘基等碳原子数为6~20个的芳基;苄基、苯乙基及苯丙基等碳原子数为7~20个的芳烷基;以及将这些基团的氢原子中的一部分或全部被氟原子、氯原子、溴原子等卤素原子取代的基团。
上述的反应通过在甲醇、乙醇、异丙醇及丁醇等醇;甲苯及二甲苯等芳香烃;己烷及庚烷等脂肪烃;矿物油精、轻石油及石油醚等有机溶剂中、在室温下或加热而进行。此外,得到的反应产物优选根据需要蒸馏除去有机溶剂或低沸点成分、或过滤沉析物。此外,为了促进该反应,可以添加二烷基甲酰胺、六烷基磷酰胺等。这样制备的含铈有机聚硅氧烷中铈原子的含量优选为0.1~5质量%的范围内。
含铈有机聚硅氧烷的含量并没有限定,相对于本组合物,使铈原子,以质量单位计优选的量为10~2,000ppm的范围内、为20~2,000ppm的范围内的量、为20~1,000ppm的范围内的量、或为20~500ppm的范围内的量。这是因为:当含铈有机聚硅氧烷的含量为上述范围的下限以上时,可以提高得到的组合物的耐热性,另一方面,当含铈有机聚硅氧烷的含量为上述范围的上限以下时,可以减少用于光半导体器件时的发光色度变化。
本组合物在室温下或通过加热而进行固化,但为了迅速地使其固化,优选进行加热。作为该加热温度,优选为50~200℃的范围内。
接着,对本发明的半导体装置详细地进行说明。
本发明的半导体装置的特征在于,通过上述固化性有机硅组合物的固化物对半导体元件密封而成。作为这种本发明的半导体装置,可示例发光二极管(LED)、光电耦合器、CCD。此外,作为半导体元件,可示例发光二极管(LED)芯片、固态图像传感器。
作为本发明的半导体装置一例的单体表面贴装型LED的剖面图示于图1。图1所示的LED其发光元件(LED芯片)1芯片焊接在引线框架2上,该发光元件(LED芯片)1与引线框架3通过键合线4进行引线键合。在该发光元件(LED芯片)1的周围设有框架5,该框架5内侧的发光元件(LED芯片)1由本发明固化性有机硅组合物的固化物6密封。
作为制造如图1所示的表面贴装型LED的方法,可示例如下方法:将发光元件(LED芯片)1芯片焊接在引线框架2上,将该发光元件(LED芯片)1与引线框架3经金制的键合线4进行引线键合,接着,在设置于发光元件(LED芯片)1周围的框架5内侧填充本发明的固化性有机硅组合物之后,在50~200℃下进行加热,由此使其固化。
实施例
通过实施例详细地说明本发明的粘合促进剂、固化性有机硅组合物及半导体装置。予以说明,式中,Me、Vi、Ph分别表示甲基、乙烯基、苯基。
[参考例1]
在反应容器中投入苯基三甲氧基硅烷400g(2.02mol)和1,3-二乙烯基-1,3-二苯基二甲基二硅氧烷93.5g(0.30mol),预混合后,投入三氟甲磺酸1.74g(11.6mmol),在搅拌下投入水110g(6.1mol),加热回流2小时。其后,进行加热常压蒸馏使温度达到85℃。接着,投入甲苯89g和氢氧化钾1.18g(21.1mmol),进行加热常压蒸馏使反应温度达到120℃,在该温度下反应6小时。其后,冷却至室温,投入醋酸0.68g(11.4mmol)并进行中和。滤除生成的盐之后,从得到的透明溶液中加热减压除去低沸点物质,制备成平均单元式:
(MePhViSiO1/2)0.23(PhSiO3/2)0.77
表示的有机聚硅氧烷树脂347g(收率:98%)。
[实施例1]
在反应容器中投入三烯丙基异氰脲酸酯18.8g(0.075mol)、催化剂量的铂-1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷络合物的甲苯溶液,加热至80~90℃。接着,滴加式:
[化学式4]
表示的二硅氧烷18.6g(0.075mol),滴加结束后,在100℃下反应2小时。其后,利用红外线分光光度计确认反应混合物中的与硅原子结合的氢原子的消失之后,在减压下除去低沸点成分,得到浅黄色液体。NMR分析的结果可知:该液体为平均式:
[化学式5]
表示的粘合促进剂。
[实施例2]
在反应容器中投入三烯丙基异氰脲酸酯18.8g(0.075mol)、催化剂量的铂-1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷络合物的甲苯溶液,加热至80~90℃。接着,滴加式:
[化学式6]
表示的二硅氧烷28.0g(0.1125mol),滴加结束后,在100℃下反应2小时。其后,利用红外线分光光度计确认反应混合物中的与硅原子结合的氢原子的消失之后,在减压下除去低沸点成分,得到浅黄色液体。NMR分析的结果可知:该液体为平均式:
[化学式7]
表示的粘合促进剂。
[实施例3~6、比较例1~2]
使用下述成分制备如表1所示的固化性有机硅组合物。予以说明,表1中,(D)成分的含量以质量单位中的相对于固化性有机硅组合物的铂金属的含量(ppm)来表示。此外,表1中,SiH/Vi表示相对于(A)成分和(C)成分中所含的烯基合计每1摩尔,(B)成分中与硅原子结合的氢原子的摩尔数。
作为(A)成分,使用以下成分:
(A-1)成分:平均单元式:
(Me2ViSiO1/2)0.2(PhSiO3/2)0.8
表示的有机聚硅氧烷
(A-2)成分:粘度为3,000mPa·s的分子链两末端由二甲基乙烯基甲硅烷氧基封端的甲基苯基聚硅氧烷
作为(B)成分,使用以下成分:
(B-1)成分:式:
HMe2SiOPh2SiOSiMe2H
表示的有机三硅氧烷
作为(C)成分,使用以下成分:
(C-1)成分:实施例1中制备的粘合促进剂
(C-2)成分:实施例2中制备的粘合促进剂
(C-3)成分:包含在25℃时的粘度为30mPa·s的分子链两末端由硅烷醇基封端的甲基乙烯基硅氧烷低聚物和3-环氧丙氧基丙基三甲氧基硅烷的缩合反应物的粘合促进剂
作为(D)成分,使用以下成分:
(D-1)成分:铂-1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷络合物的1,3,5,7-四甲基-1,3,5,7-四乙烯基环四硅氧烷的溶液(含有铂为0.1质量%的溶液)
按照如下评价固化性有机硅组合物固化物的粘合性。
[粘合性]
将开有直径为5mm孔、厚度为2mm的氟树脂制垫片设置在铝板或施以镀银的粘合用测试板上,向上述垫片的孔中注入固化性有机硅组合物之后,在150℃的热风循环式烘箱中放置1小时,由此形成直径5mm、高度2mm的圆柱状固化物。接着,使用剪切强度测定装置以50mm/分钟的速度对该固化物进行剥离,测定此时的负荷(MPa)并评价粘合性。
使用固化性有机硅组合物按照如下制作表面贴装型的发光二极管(LED)。
[发光二极管的制作]
堵住底部的圆筒状聚邻苯二甲酰胺(PPA)树脂制框架5(内径2.0mm、深度1.0mm)中,引线框架2、3从侧壁向框架5内底部的中心部延伸,在引线框架2的中央部上载置有LED芯片1,在LED芯片1与引线框架3通过键合线4进行电连接的未密封的发光二极管内,利用点胶机注入经脱泡的固化性有机硅组合物。其后,在一次固化温度(70℃)下保持1小时,接着,在二次固化温度(150℃)下保持1小时,由此使固化性有机硅组合物固化,制作如图1所示的发光二极管。
[墨水试验]
将用上述方法制作的16个发光二极管浸渍在市售的红色墨水中,50℃下放置4小时。放置后,用显微镜观察红色墨水有无渗入,按照如下进行评价:
◎:确认有墨水渗入的发光二极管为2个以下。
△:确认有墨水渗入的发光二极管为3个~8个。
×:确认有墨水渗入的发光二极管为9个以上。
[断线]
将用上述方法制作的16个发光二极管在-40℃下30分钟、接着在125℃下30分钟的温度循环设为1次循环,进行1000次循环的温度循环试验,随后进行通电,进行发光二极管的点亮试验,按照如下进行评价:
◎:点亮的发光二极管为14个以上。
○:点亮的发光二极管为8个~13个。
△:点亮的发光二极管为7个以下。
[表1]
[实施例7、比较例3]
使用以下成分制备如表2所示的固化性有机硅组合物。予以说明,表2中,(D)成分的含量表示质量单位中的相对于固化性有机硅组合物的铂金属的含量(ppm)。此外,表2中,SiH/Vi表示相对于(A)成分和(C)成分中所含的烯基合计每1摩尔,(B)成分中与硅原子结合的氢原子的摩尔数。
作为(A)成分,使用以下成分。此外,粘度为25℃时的值,根据JIS K7117-1使用B型粘度计进行测定。此外,乙烯基的含量通过FT-IR、NMR、GPC等分析进行测定。
(A-3)成分:粘度为300mPa·s、平均式:
Me2ViSiO(Me2SiO)150SiMe2Vi
表示的分子链两末端由二甲基乙烯基甲硅烷氧基封端的二甲基聚硅氧烷(乙烯基的含量=0.48质量%)
(A-4)成分:粘度10,000mPa·s,平均式:
Me2ViSiO(Me2SiO)500SiMe2Vi
表示的分子链两末端由二甲基乙烯基甲硅烷氧基封端的二甲基聚硅氧烷(乙烯基的含量=0.15质量%)
(A-5)成分:25℃时为白色固体状、为甲苯可溶性的平均单元式:
(Me2ViSiO1/2)0.15(Me3SiO1/2)0.47(SiO4/2)0.38(HO1/2)0.0001
表示的一分子中具有2个以上乙烯基的有机聚硅氧烷树脂(乙烯基的含量=5.4质量%)
(A-6)成分:25℃时为白色固体状、为甲苯可溶性的平均单元式:
(Me2ViSiO1/2)0.15(Me3SiO1/2)0.38(SiO4/2)0.47(HO1/2)0.01
表示的一分子中具有2个以上乙烯基的有机聚硅氧烷(乙烯基的含量=4.2质量%)
作为(B)成分,
(B-2)成分:平均式:
Me3SiO(MeHSiO)55SiMe3
表示的粘度为20mPa·s的分子链两末端由三甲基甲硅烷氧基封端的聚甲基氢硅氧烷(与硅原子结合的氢原子含量=1.6质量%)
作为(C)成分,使用上述(C-1)成分和(C-3)成分。
作为(D)成分,使用以下成分:
(D-2)成分:铂的1,3-二乙烯基四甲基二硅氧烷络合物的1,3-二乙烯基四甲基二硅氧烷溶液(铂金属的含量=约5000ppm)
作为(E)成分,使用以下成分:
(E-1)成分:1-乙炔基环己烷-1-醇
使用固化性有机硅组合物按照如下制作表面贴装型的发光二极管(LED)。
[发光二极管的制作]
堵住底部的圆筒状聚邻苯二甲酰胺(PPA)树脂制框架5(内径2.0mm、深度1.0mm)中,引线框架2、3从侧壁向框架5内底部的中心部延伸,在引线框架2的中央部上载置有LED芯片1,在LED芯片1与引线框架3通过键合线4进行电连接的未密封的发光二极管内,利用点胶机注入经脱泡的固化性有机硅组合物。其后,加热烘箱中在100℃下加热30分钟,接着在150℃下加热1小时,由此使固化性有机硅组合物固化,制作如图1所示的发光二极管。
[固化物的初期剥离率]
对于用上述方法制作的8个发光二极管,用光学显微镜观察引线框架2、3、以及键合线4与固化物6之间的剥离状态,可看到剥离的发光二极管的个数比例示于表2。
[吸湿回流焊后的剥离率1]
将用上述方法制作的8个发光二极管放入85℃、85%的恒温恒湿室24小时之后,在280℃的烘箱内放置30秒,然后返回到室温(25℃),用光学显微镜观察引线框架2、3、以及键合线4与固化物6之间的剥离状态,可看到剥离的发光二极管的个数比例示于表2。
[吸湿回流焊后的剥离率2]
将用上述方法制作的8个发光二极管放入85℃、85%的恒温恒湿室72小时之后,在280℃的烘箱内放置30秒,然后返回到室温(25℃),用光学显微镜观察引线框架2、3、以及键合线4与固化物6之间的剥离状态,可看到剥离的发光二极管的个数比例示于表2。
[表2]
由表2的结果表明:实施例7的固化性有机硅组合物的固化物与比较例3的固化性有机硅组合物的固化物相比,具有高的耐剥离性。
工业上的可利用性
本发明的固化性有机硅组合物其流动性优异,经固化能够形成荧光体均匀地分散且高折射率的固化物,因此适于用作发光二极管(LED)等光半导体装置中的发光元件的密封剂或包覆剂。
符号说明
1 发光元件
2 引线框架
3 引线框架
4 键合线
5 框架
6 固化性有机硅组合物的固化物
Claims (7)
1.一种粘合促进剂,其由以下平均式表示:
[化学式8]
(式中,R1为相同或不同的不具有脂肪族不饱和键的碳原子数1~12的一价烃基,X为环氧丙氧基烷基、环氧基环烷基烷基或环氧烷基,m和n为满足1<m<3、1<n<3、且m+n=3的数,p为1~50的数。)
2.一种固化性有机硅组合物,其含有权利要求1所述的粘合促进剂。
3.根据权利要求2所述的固化性有机硅组合物,其通过氢化硅烷化反应固化。
4.根据权利要求3所述的固化性有机硅组合物,其中,通过氢化硅烷化反应固化的固化性有机硅组合物至少包含以下组分:
(A)一分子中具有至少2个烯基的有机聚硅氧烷100质量份;
(B)一分子中具有至少2个与硅原子结合的氢原子的有机氢化聚硅氧烷{其量为相对于(A)成分和(C)成分中所含的烯基合计每1摩尔,使提供与硅原子结合的氢原子的量为0.1~10摩尔};
(C)权利要求1所述的粘合促进剂0.01~20质量份;及
(D)氢化硅烷化反应用催化剂(其量为促进本组合物的固化的量)。
5.根据权利要求4所述的固化性有机硅组合物,其还含有(E)氢化硅烷化反应抑制剂{相对于(A)成分~(D)成分的合计100质量份,所述(E)氢化硅烷化反应抑制剂的量为0.0001~5质量份}。
6.一种半导体装置,其特征在于,通过权利要求2~5中任一项所述的固化性有机硅组合物的固化物对半导体元件进行密封。
7.根据权利要求6所述的半导体装置,其中,半导体元件为发光元件。
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- 2015-05-29 WO PCT/JP2015/002717 patent/WO2015186323A1/ja active Application Filing
- 2015-05-29 CN CN201580035513.9A patent/CN106488949A/zh active Pending
- 2015-05-29 KR KR1020167036548A patent/KR20170015356A/ko unknown
- 2015-05-29 EP EP15802373.9A patent/EP3153544A4/en not_active Withdrawn
- 2015-05-29 JP JP2016525684A patent/JPWO2015186323A1/ja active Pending
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CN110546229A (zh) * | 2017-04-24 | 2019-12-06 | 汉高股份有限及两合公司 | 用于加聚有机硅配制物的粘合促进剂 |
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CN111344369A (zh) * | 2017-11-16 | 2020-06-26 | 美国陶氏有机硅公司 | 氢化硅烷化-可固化硅酮组合物 |
US11495776B2 (en) | 2018-04-16 | 2022-11-08 | Shin-Etsu Chemical Co., Ltd. | Transparent desiccant for organic EL, and method for using same |
TWI791784B (zh) * | 2018-04-16 | 2023-02-11 | 日商信越化學工業股份有限公司 | 有機el用透明乾燥劑及其使用方法 |
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JPWO2015186323A1 (ja) | 2017-04-20 |
US20170190879A1 (en) | 2017-07-06 |
WO2015186323A1 (ja) | 2015-12-10 |
EP3153544A1 (en) | 2017-04-12 |
TW201606011A (zh) | 2016-02-16 |
KR20170015356A (ko) | 2017-02-08 |
EP3153544A4 (en) | 2018-01-24 |
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