TWI426106B - 可固化之聚矽氧組合物及電子組件 - Google Patents
可固化之聚矽氧組合物及電子組件 Download PDFInfo
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- TWI426106B TWI426106B TW096146566A TW96146566A TWI426106B TW I426106 B TWI426106 B TW I426106B TW 096146566 A TW096146566 A TW 096146566A TW 96146566 A TW96146566 A TW 96146566A TW I426106 B TWI426106 B TW I426106B
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- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
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- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000009429 electrical wiring Methods 0.000 description 1
- 125000005448 ethoxyethyl group Chemical group [H]C([H])([H])C([H])([H])OC([H])([H])C([H])([H])* 0.000 description 1
- 239000012765 fibrous filler Substances 0.000 description 1
- 239000005338 frosted glass Substances 0.000 description 1
- 238000005227 gel permeation chromatography Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 125000006038 hexenyl group Chemical group 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- ULYZAYCEDJDHCC-UHFFFAOYSA-N isopropyl chloride Chemical compound CC(C)Cl ULYZAYCEDJDHCC-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 238000006146 oximation reaction Methods 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000002255 pentenyl group Chemical group C(=CCCC)* 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 125000000286 phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
- 150000004714 phosphonium salts Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- 229910001285 shape-memory alloy Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000001721 transfer moulding Methods 0.000 description 1
- TUQOTMZNTHZOKS-UHFFFAOYSA-N tributylphosphine Chemical compound CCCCP(CCCC)CCCC TUQOTMZNTHZOKS-UHFFFAOYSA-N 0.000 description 1
- AUOZNINQGUNWOV-UHFFFAOYSA-N triphenyl borate;triphenylphosphane Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C=1C=CC=CC=1OB(OC=1C=CC=CC=1)OC1=CC=CC=C1 AUOZNINQGUNWOV-UHFFFAOYSA-N 0.000 description 1
- IUURMAINMLIZMX-UHFFFAOYSA-N tris(2-nonylphenyl)phosphane Chemical compound CCCCCCCCCC1=CC=CC=C1P(C=1C(=CC=CC=1)CCCCCCCCC)C1=CC=CC=C1CCCCCCCCC IUURMAINMLIZMX-UHFFFAOYSA-N 0.000 description 1
- WXAZIUYTQHYBFW-UHFFFAOYSA-N tris(4-methylphenyl)phosphane Chemical compound C1=CC(C)=CC=C1P(C=1C=CC(C)=CC=1)C1=CC=C(C)C=C1 WXAZIUYTQHYBFW-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01L23/293—Organic, e.g. plastic
- H01L23/296—Organo-silicon compounds
-
- 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
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
-
- 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
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
-
- 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
- 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
- C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
-
- 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
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
-
- 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
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- 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
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
-
- 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
- C08G77/70—Siloxanes defined by use of the MDTQ nomenclature
-
- 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
- H01L2224/10—Bump connectors; Manufacturing methods related thereto
- H01L2224/15—Structure, shape, material or disposition of the bump connectors after the connecting process
- H01L2224/16—Structure, shape, material or disposition of the bump connectors after the connecting process of an individual bump connector
- H01L2224/161—Disposition
- H01L2224/16151—Disposition the bump 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
- H01L2224/16221—Disposition the bump 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
- H01L2224/16225—Disposition the bump 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 the item being non-metallic, e.g. insulating substrate with or without metallisation
-
- 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
- H01L2224/73—Means for bonding being of different types provided for in two or more of groups H01L2224/10, H01L2224/18, H01L2224/26, H01L2224/34, H01L2224/42, H01L2224/50, H01L2224/63, H01L2224/71
- H01L2224/732—Location after the connecting process
- H01L2224/73251—Location after the connecting process on different surfaces
- H01L2224/73253—Bump and layer connectors
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L2924/0001—Technical content checked by a classifier
- H01L2924/00014—Technical content checked by a classifier the subject-matter covered by the group, the symbol of which is combined with the symbol of this group, being disclosed without further technical details
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/095—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00 with a principal constituent of the material being a combination of two or more materials provided in the groups H01L2924/013 - H01L2924/0715
- H01L2924/097—Glass-ceramics, e.g. devitrified glass
- H01L2924/09701—Low temperature co-fired ceramic [LTCC]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/15—Details of package parts other than the semiconductor or other solid state devices to be connected
- H01L2924/161—Cap
- H01L2924/1615—Shape
- H01L2924/16152—Cap comprising a cavity for hosting the device, e.g. U-shaped cap
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- Epoxy Resins (AREA)
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- Details Of Resistors (AREA)
Description
本發明係關於一種可固化之聚矽氧組合物及一種電子組件。更特定言之,本發明係關於一種可固化之聚矽氧組合物,其特徵在於優良可處理性,其不含油且當固化時形成具有優良可撓性及黏著性之固化體。本發明亦係關於一種電子組件,其係藉助於上述組合物之固化體密封或黏結且其特徵在於優良之可靠性。
用於密封及黏結電組件及電子組件之部件藉由固化習知可固化樹脂組合物(諸如可固化環氧樹脂組合物等)而獲得之固化體的特徵在於高彈性模數及由此之高剛性。因此,該等體與電組件或電子組件一起使用會帶來諸如出現高應力之問題,高應力在熱膨脹條件下出現。與使用上述組合物之固化體相關的另一問題為電組件或電子組件或基板屈曲及在固化樹脂體中形成裂痕或在固化樹脂與電組件或電子組件間之介面中形成間隙,在某些狀況下此可能導致各別組件損壞。
為降低上述固化體中可能出現的應力,已提議自含環氧基有機聚矽氧烷及有機聚矽氧烷樹脂之固化劑來製備可固化之聚矽氧組合物(參見日本未審查專利申請公開案(後文中稱為"Kokai")2005-154766、2006-306953及2006-306954)。然而,當該等可固化之聚矽氧組合物用於黏結電組件或電子組件之部件時,出現組合物之某些組份滲油至固化體外表面之問題,且此將污染組件。
本發明之一目標係提供一種特徵在於優良可處理性及可形成特徵在於降低之滲油性及優良可撓性及黏著性之固化體的可固化之聚矽氧組合物。另一目標為提供具有優良可靠性之電子組件。
更特定言之,本發明提供一種可固化之聚矽氧組合物,其包含至少以下組份:(A)(A1
)一個分子中含有至少兩個含環氧基單價有機基團且由以下通式表示之有機聚矽氧烷:(R1 3
SiO1/2
)a
(R2 2
SiO2
/2
)b
(R3
SiO3/2
)c
(其中R1
、R2
及R3
可相同或不同且表示經取代或未經取代之單價烴基或上述含環氧基之單價烴基;然而,不少於20莫耳%之R3
所表示之基團為芳基;且其中"a"、"b"及"c"為滿足以下條件之數字:0a0.8;0b0.8;0.2c0.9;a+b+c=1)及/或(A2
)以下通式之二有機聚矽氧烷:A-R5
-(R4 2
SiO)m
R4 2
Si-R5
-A{其中R4
為經取代或未經取代之不含不飽和脂族鍵之單價烴基;R5
為二價有機基團;且"A"為由以下平均單元式表示之矽氧烷殘基:(XR4 2
SiO1/2
)d
(SiO4/2
)e
(其中R4
係如上文所定義,且"X"為一單鍵、氫原子、R4
所表示之基團、含環氧基之單價有機基團或烷氧基矽烷基烷基;然而,一個分子中至少一個由"X"表示之基團為單鍵,至少兩個由"X"表示之基團為含環氧基之單價有機基團;"d"為一正數;"e"為一正數;且"d/e"為0.2至4範圍之數字)且其中"m"為等於或大於1之整數};(B)環氧樹脂之固化劑;及(C)由以下通式表示之環氧化合物:
(其中R8
為經取代或未經取代之具有1至10個碳原子之單價烴基;且"f"為0至4之整數。)
另外,本發明之電子組件為藉由使用上述可固化之聚矽氧組合物密封或黏結之電子組件。
本發明之可固化之聚矽氧組合物係有效的,因為其特徵在於優良之可處理性及由於滲油性降低而較少經受固化體表面污染。另外,該組合物之固化體可黏結於各種基板,具有優良之可撓性及黏著性,且在熱膨脹作用下呈現降低之內應力。另外,由於根據本發明製造之電子組件係使用上述可固化之聚矽氧組合物之固化體密封或黏結,因此此等組件之特徵在於優良之可靠性。
首先更詳細地分析本發明之可固化之聚矽氧組合物。
該組合物之組份(A)為組合物之主要組份。此組份為(A1
)由以下平均單元式表示之有機聚矽氧烷:(R1 3
SiO1/2
)a
(R2 2
SiO2/2
)b
(R3
SiO3/2
)c
及/或(A2
)由以下通式表示之二有機矽氧烷:A-R5
-(R4 2
SiO)m
R4 2
Si-R5
-A。
在組份(A1
)中,R1
、R2
及R3
可相同或不同且構成經取代或未經取代之單價烴基或含環氧基之單價有機基團。上述單價烴基可由以下基團代表:甲基、乙基、丙基、異丙基、正丁基、第二丁基、第三丁基、戊基、己基或類似烷基;環戊基、環己基、環庚基或類似環烷基;乙烯基、烯丙基、丁烯基、戊烯基或己烯基或類似烯基;苯基、甲苯基、二甲苯基或類似芳基;苯甲基、苯乙基、苯丙基或類似芳烷基;氯甲基、3-氯丙基、3,3,3-三氟丙基或類似鹵化烷基。最佳為烷基及芳基,尤其為甲基及苯基。含環氧基之單價有機基團可由以下基團代表:2-縮水甘油氧基乙基、3-縮水甘油氧基丙基、4-縮水甘油氧基丁基或類似縮水甘油氧基烷基;或2-(3,4-環氧基氯己基)乙基、3-(3,4-環氧基氯己基)丙基、2-(3,4-環氧基-3-甲基環己基)-2-甲基乙基或類似環氧基環烷基烷基;及4-氧基丁基、8-氧基辛基或類似氧基烷基。此等基團中之最佳者為縮水甘油氧基烷基及環氧基環烷基烷基,尤其為3-縮水甘油氧基丙基及2-(3,4-環氧基氯己基)乙基。在上式中,至少兩個由R1
、R2
及R3
表示之基團為上述含環氧基之單價有機基團。
在上式中,不少於20莫耳%,較佳不少於50莫耳%,且最佳不少於80莫耳%之所有由R3
表示之基團為芳基。若一個分子中所有由R3
表示之基團中的芳基含量低於建議下限,則此將有損黏著特性或將降低組合物固化體之機械強度。建議該等芳基包含苯基。
在上式中,"a"、"b"及"c"為滿足以下條件之數字:0a0.8、0b0.8、0.2c0.9、a+b+c=1。在此,"a"為顯示R1 3
SiO1/2
所表示之矽氧烷單元百分比之數字。當此組份僅包含R1 3
SiO1/2
所表示矽氧烷單元時,則此組份將過黏,且由於此將有損所得組合物之可處理性,因此建議"a"為滿足以下條件之數字:0<a0.8,且較佳為滿足以下條件之數字:0.3a0.8。另外,"b"為顯示R2 2
SiO2/2
所表示之矽氧烷單元百分比之數字。為提供具有最佳分子量之此組份,為防止此組份自所得固化體滲出及為提供具有優良機械強度之固化體,"b"應為滿足以下條件之數字:0b0.6。在上式中,"c"顯示由R3
SiO3/2
所表示之矽氧烷單元百分比之數字。為提供組合物之良好可處理性及為提供具有良好黏著性、良好機械特徵及可撓性之固化體,"c"應為滿足以下條件之數字:0.4c0.9。
關於組份(A1
)中含環氧基之單價有機基團之含量無特定限制;然而,建議此組份中所用此等基團之環氧當量(亦即藉由此組份之質量平均分子量除以一個分子中環氧基之數目所得之數)應在100至2,000,較佳100至1,000,且最佳100至700之範圍內。若環氧當量小於上述範圍之建議下限,則將有損自組合物獲得之固化體之可撓性。另一方面,若環氧當量大於建議上限,則將有損組合物之固化性且將降低藉由固化組合物獲得之固化體之黏著性及機械強度。另外,組份(A1
)可包含一種類型之有機聚矽氧烷或兩種或兩種以上類型之有機聚矽氧烷之混合物。關於25℃下組份(A1
)之形態無特定限制,且其可為液體或固體。當組份(A1
)為固態時,為將其與其他組份均一混合,可將組份(A1
)溶解於有機溶劑中或加熱。鑒於較佳可混配性及可處理性,較佳使用25℃下為液態之此組份。同樣,關於組份(A1
)之質量平均分子量無特定限制,但可建議此特徵範圍為500至10,000,較佳為750至3,000。
上述組份(A1
)之實例可為由以下所給式表示之有機聚矽氧烷,其中"a"、"b"及"c"係與如上所定義者相同,但其中"a"及"b"不能等於零;"c'"及"c""為滿足以下條件之數字:0.1<c'<0.8;0<c"<0.2;0.2(c'+c")0.9;及0.2c'/(c'+c");G表示3-縮水甘油氧基丙基;且E表示2-(3,4-環氧基環己基)乙基。
[G(CH3
)2
SiO1/2
]a
[C6
H5
SiO3/2
]c
[E(CH3
)2
SiO1/2
]a
[C6
H5
SiO3/2
]c
[G(CH3
)2
SiO1/2
]a
[(CH3
)2
SiO2/2
]b
[C6
H5
SiO3/2
]c
[E(CH3
)2
SiO1/2
]a
[(CH3
)2
SiO2/2
]b
[C6
H5
SiO3/2
]c
[GCH3
SiO2/2
]b
[C6
H5
SiO3/2
]c
[ECH3
SiO2/2
]b
[C6
H5
SiO3/2
]c
[G(CH3
)2
SiO1/2
]a
[C6
H5
SiO3/2
]c'
[CH3
SiO3/2
]c"
[E(CH3
)2
SiO1/2
]a
[C6
H5
SiO3/2
]c'
[CH3
SiO3/2
]c"
[C6
H5
SiO3/2
]c'
[GSiO3/2
]c"
[C6
H5
SiO3/2
]c'
[ESiO3/2
]c"
關於組份(A1
)之製備方法無特定限制。舉例而言,以下方法係可行者:(1)使苯基三烷氧基矽烷及烷氧基矽烷與含環氧基之單價有機基團(例如3-縮水甘油氧基丙基三甲氧基矽烷或2-(3,4-環氧基環己基)乙基三甲氧基矽烷)經受共水解及縮合之方法;(2)使具有上述含環氧基之單價有機基團之烷氧基矽烷與藉由使苯基三氯矽烷及苯基三烷氧基矽烷經受共水解及縮合獲得之含矽烷醇之有機聚矽氧烷經受脫醇反應之方法;(3)在具有含環氧基之有機基團之烯烴與藉由使苯基三氯矽烷及苯基三烷氧基矽烷在二甲基氯矽烷或類似具有矽合氫原子之矽烷存在下經受共水解及縮合所製備之具有矽合氫原子之有機聚矽氧烷之間進行氫化矽烷化反應之方法;(4)使二甲基矽氧烷與兩分子端由三甲基矽烷氧基封端之甲基{2-(3,4-環氧基氯己基)乙基}矽氧烷之共聚物或二甲基矽氧烷與兩分子端由三甲基矽烷氧基封端之甲基(3-縮水甘油氧基丙基)矽氧烷之共聚物與藉由使苯基三氯矽烷及苯基三烷氧基矽烷經受水解及縮合所製備之有機聚矽氧烷在鹼性催化劑存在下經受平衡反應之方法;(5)使環狀甲基{2-(3,4-環氧基環己基)乙基}矽氧烷或環狀甲基(3-縮水甘油氧基丙基)矽氧烷與包含下式C6
H5
SiO3/2
之矽氧烷單元之有機聚矽氧烷在鹼性催化劑存在下經受平衡反應之方法;及(6)使環狀二甲基矽氧烷及環狀{2-(3,4-環氧基環己基)乙基}矽氧烷或環狀甲基(3-縮水甘油氧基丙基)矽氧烷與包含下式C6
H5
SiO3/2
之矽氧烷單元之有機聚矽氧烷在酸性或鹼性催化劑存在下經受平衡反應之方法。
在組份(A2
)中,R4
所表示之基團可為經取代或未經取代之單價烴基,其不含不飽和脂族基團。R4
所表示之基團之特定實例為以下基團:甲基、乙基、丙基、異丙基、正丁基、第二丁基、第三丁基、戊基、己基或類似烷基;環戊基、環己基、環庚基或類似環烷基;苯基、甲苯基、二甲苯基或類似芳基;苯甲基、苯乙基、苯丙基或類似芳烷基;3-氯丙基、3,3,3-三氟丙基或類似鹵化烷基。最佳者為烷基,尤其為甲基。在上式中,R5
為二價有機基團,諸如伸乙基、甲基伸乙基、伸丙基、伸丁基、伸戊基、伸己基或類似伸烷基;伸乙基氧基伸乙基、伸乙基氧基伸丙基、伸乙基氧基伸丁基、伸丙基氧基伸丙基或類似伸烷基氧基伸烷基。較佳為伸烷基,尤其為伸乙基。在該式中,"m"為一整數,其等於或大於1且表示主分子鏈中所含之二有機聚矽氧烷之聚合度。鑒於組合物固化體之改良可撓性,"m"應等於或大於10。關於"m"值之上限無特定限制,但建議"m"之值不超過500。
另外,在上式中,"A"表示由以下平均單元式表示之矽氧烷殘基:(XR4 2
SiO1/2
)d
(SiO4/2
)e
其中R4
代表經取代或未經取代之不含不飽和脂族鍵之單價烴基。此基團可與上述例示者相同,其中烷基且尤其甲基為較佳者。在上式中,"X"為一單鍵、氫原子、R4
所表示之基團、含環氧基之單價有機基團或烷氧基矽烷基烷基。R4
所表示之基團之實例可與上文所給基團相同。上述含環氧基之單價有機基團可與R1
、R2
或R3
所表示之基團相同。烷氧基矽烷基烷基之實例可為以下基團:三甲氧基矽烷基乙基、三甲氧基矽烷基丙基、二甲氧基甲基矽烷基丙基、甲氧基二甲基矽烷基丙基、三乙氧基矽烷基乙基或三丙氧基矽烷基丙基。然而,一個分子中至少一個由"X"表示之基團為單鍵,其係用於鍵結上述二有機矽氧烷中之R5
所表示之基團。另外,一個分子中至少一個由"X"表示之基團應包含含環氧基之單價有機基團,較佳諸如縮水甘油氧基烷基,且最佳為3-縮水甘油氧基丙基。在上式中,"d"為一正數,"e"為一正數,且"d/e"為0.2至4範圍之數字。
關於組份(A2
)之分子量無特定限制;然而,建議質量平均分子量在500至1,000,000之範圍內。同樣,關於25℃下組份(A2
)之形態無特定限制,但液態為較佳。建議組份(A2
)在25℃下具有50至1,000,000 mPa.s範圍內之黏度。製備組份(A2
)之方法描述於(例如)Kokai H06-56999中。
在本發明之組合物中,組份(A)可包含上述組份(A1
)或組份(A2
)或兩者之混合物。關於當組份(A)係由組份(A1
)與(A2
)之混合物表示時可使用之組份(A2
)之量無特定限制,但可建議所含組份(A2
)之量為每100質量份組份(A1
)0.1至800質量份,較佳1至500質量份,且最佳10至200質量份。若所添加組份(A2
)之量少於建議下限,則將有損藉由固化組合物製得之固化體之可撓性;且另一方面,若組份(A2
)之含量超過建議上限,則所得組合物之黏度將增加。
作為環氧樹脂之固化劑之組份(B)係與組份(A)之環氧基反應且用作使組合物固化之試劑。建議此試劑為一個分子中含有兩個或兩個以上與環氧基反應之官能基的組份。上述官能基之實例可為一級胺基、二級胺基、羥基、酚羥基、羧酸基、酸酐基、巰基或矽烷醇基。鑒於較佳反應性及"適用期",較佳使用酚羥基。特定言之,建議組份(B)包含含有酚羥基之化合物,諸如苯酚清漆型酚醛樹脂、甲酚清漆型酚醛樹脂、雙酚A型化合物或類似酚型樹脂;及具有酚羥基之有機矽氧烷。較佳使用一個分子中含有至少兩個酚羥基之有機矽氧烷。建議酚羥基當量(藉由此組份之質量平均分子量除以一個分子中所含酚羥基數所得之值)不超過1,000,且為達成較佳反應性不超過500。
由於組份(B)中提供具有酚羥基之有機矽氧烷改良藉由固化組合物獲得之固化體之可撓性,因此建議由以下通式所表示之有機矽氧烷:R6 3
SiO(R6 2
SiO)n SiR6 3
。
在上式中,R6
所表示之基團可相同或不同且表示經取代或未經取代之單價烴基或含有酚羥基之單價有機基團。上述單價烴基可與上文例示者相同,其中烷基及芳基,尤其甲基及苯基為較佳者。含有酚基之有機基團之實例可為以下所給式所示之基團。在此等式中,R7
表示二價有機基團,諸如伸乙基、甲基伸乙基、伸丙基、伸丁基、伸戊基、伸己基或類似伸烷基;伸乙基氧基伸乙基、伸乙基氧基伸丙基、伸乙基氧基伸丁基、伸丙基氧基伸丙基或類似伸烷基氧基伸烷基。較佳者為伸烷基,且尤其為伸丙基。
在上式中,"n"為0至1,000之整數,較佳為0至100,且最佳為0至20。若"n"超過建議上限,則將有損與組份(A)之混配及工業可處理性。
上述組份(B)之實例為由以下所給式表示之有機矽氧烷,其中"x"為1至20之整數,且"y"為2至10之整數。
關於可用以製造組份(B)之方法無特定限制。舉例而言,此組份可藉由使含烯基之酚化合物與具有矽合氫原子之有機聚矽氧烷經受氫化矽烷化反應來獲得。
關於25℃下組份(B)之形態無特定限制,且其可呈液態或固態。鑒於更易處理性,液態為較佳。建議25℃下液態組份(B)之黏度係在1至1,000,000 mPa.s之範圍內,較佳為10至5,000 mPa.s。若25℃下之黏度低於建議下限,則所得固化體將具有降低之機械強度。另一方面,若黏度超過建議上限,則將有損組合物之工業可處理性。
關於組合物中可使用組份(B)之量無特定限制,但通常建議此組份之使用量為每100質量份組份(A)0.1至500質量份,較佳在0.1至200質量份之範圍內。當組份(B)含有酚羥基時,建議組份(B)中所含酚羥基與組合物中所含之所有環氧基的莫耳比在0.2至5之範圍內,較佳為0.3至2.5,且最佳為0.8至1.5。若組份(B)中所含酚羥基與組合物中所含之所有環氧基的莫耳比低於建議下限,則將難以確保所得組合物之完全固化。另一方面,若上述比率超過建議上限,則將有損自組合物獲得之固化體之機械特性。
作為環氧化合物之組份(C)係用於組合物中以改良黏結及限制滲油至固化體表面。組份(C)由以下通式表示:
在上式中,R8
表示經取代或未經取代之具有1至10個碳原子之單價烴基。上述單價烴基之實例可為甲基、乙基、丙基、異丙基、正丁基、第二丁基、第三丁基、戊基、己基、辛基、癸基或類似烷基;環戊基、環己基、環庚基或類似環烷基;甲氧基乙基、乙氧基乙基或類似經乙氧基取代之烷氧基;乙烯基、烯丙基、丁烯基或類似烯基;環戊烯基、環己烯基或類似環烯基;苯基、甲苯基、二甲苯基、乙基苯基、丁基苯基、第三丁基苯基、二甲基萘基或類似芳基;苯甲基、苯乙基、苯丙基或類似芳烷基;3-氯丙基、3,3,3-三氟丙基或類似鹵化烷基;甲氧基苯基、乙氧基苯基、丁氧基苯基、第三丁氧基苯基、甲氧基萘基或類似經烷氧基取代之芳基。另外,在上式中,"f"為0至4之整數。
上述組份(C)可以由Japan Epoxy Resin Company製造之以商品名Epicoat 630見知之商品形式獲得。
關於組合物中可使用組份(C)之量無特定限制,但可建議此組份之添加量為0.01至50質量%,較佳0.01至20質量%,且最佳0.01至10質量%。若組份(C)之含量低於建議下限,則將難以限制滲油至表面。另一方面,若組份(C)之含量超過建議上限,則將增加自組合物獲得之固化體之彈性模數。
本發明之組合物可含有作為任選組份之固化促進劑(D)。該組份(D)可由以下各物代表:三級胺化合物、氧化鋁、氧化鋯或類似有機金屬化合物;磷化氫或類似有機磷化合物;以及雜環胺化合物、硼錯合化合物、有機銨鹽、有機鋶鹽、有機過氧化物及上述化合物之反應產物。該等化合物之特定實例為以下化合物:三苯基膦、三丁基膦、三(對-甲基苯基)膦、三(壬基苯基)膦、三苯基膦-硼酸三苯酯、四苯基膦-硼酸四苯酯或類似磷化合物;三乙胺、苯甲基二甲胺、α-甲基苯甲基二甲胺、1,8-二氮雜雙環[5.4.0]十一烯-7或類似三級胺;2-甲基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑或類似咪唑化合物。為延長本發明組合物之適用期,固化促進劑可呈囊封形式。該經囊封固化促進劑可包含由含有胺型固化促進物質之雙酚A環氧樹脂製得之經囊封胺型固化促進劑。該經囊封固化促進劑可自Asahi Kasei Co.,Ltd以商品名HX-3088購得。
關於可添加至組合物中之組份(D)之量無特定限制,但通常可建議此組份之含量不應超過每100質量份組份(A)50質量份,尤其為0.01至50質量份之量,且最佳為0.1至5質量份。
為改良固化體之機械強度,組合物可含有填充劑(E)。該填充劑(E)可由以下物質代表:玻璃纖維、氧化鋁纖維、包含氧化鋁及二氧化矽之陶瓷纖維、硼纖維、氧化鋯纖維、碳化矽纖維、金屬纖維或類似纖維填充劑;熔融二氧化矽、結晶二氧化矽、沈澱二氧化矽、煙霧狀二氧化矽、烘焙二氧化矽、氧化鋅、烘焙黏土、碳黑、玻璃珠、氧化鋁、滑石、碳酸鈣、黏土、氫氧化鋁、氫氧化鎂、硫酸鋇、氮化鋁、氮化硼、碳化矽、氧化鎂、氧化鈦、氧化鈹、高嶺土、雲母、氧化鋯、硫酸鋇或類似無機填充劑;金粉、銀粉、銅粉、鋁粉、鎳粉、鈀粉、上述金屬之合金及黃銅之粉末、焊料粉、記憶合金粉末或其他精細金屬粉末;蒸氣沈積或經由金屬化沈積至最終粉末化陶瓷、玻璃、石英、有機樹脂等表面上之金、銀、鎳、銅或其他金屬粉末。以上填充劑可單獨使用或以兩種或兩種以上之組合使用。鑒於獲得之固化體之較佳導熱性,以下填充劑為較佳者:傳導性粉末,諸如氧化鋁、結晶二氧化矽、氮化鋁、氮化硼或類似導熱性粉末;以及由熔融二氧化矽、沈澱二氧化矽、煙霧狀二氧化矽、膠體二氧化矽等製得之強化粉末。為賦予固化體良好導熱性及導電性,較佳使用銀粉。為賦予組合物固化體導熱特性,較佳使用氧化鋁粉末。粉末顆粒可具有圓形顆粒形狀,或可為球形、纖維狀、桿狀、薄片狀、鱗狀、盤狀、捲曲狀等。關於粒度無特定限制,但通常其最大尺寸不應超過200 μm,且平均應在0.001至50 μm之範圍內。
同樣,關於組份(E)之含量無特定限制,但建議此組份之添加量不應超過每100質量份組份(A)5,000質量份,較佳在10至4,000質量份之範圍內,且甚至更佳在50至4,000質量份之範圍內。當組份(E)含有除上述精細金屬粉末或導熱性粉末材料之外之填充劑時,組份(E)之使用量應為每100質量份組份(A)不超過2,000質量份,較佳在10至2,000質量份之範圍內,且甚至更佳在50至1,000質量份之範圍內。當粉末顆粒具有盤狀或薄片狀形狀時,可藉由使用顆粒於獲得之固化體中之特定方向性來減少固化期間之收縮。
為改良組合物之固化性及可加工性及為改良組合物固化體之黏著特性,或為調整彈性模數,組合物可另外與有機環氧化合物(F)組合。關於25℃下組份(F)之形態無特定限制,且其可為液體或固體,但較佳為液態。此組份之實例可為雙酚A型環氧樹脂、雙酚F型環氧樹脂、脂環族環氧樹脂。關於可添加至組合物中之組份(F)之量無限制,但通常此組份之含量不應超過每100質量份組份(A)500質量份,且較佳應在0.1至500質量份之範圍內。
為改良組份(E)於組份(A)中之分散性或為改良獲得之固化體與半導體晶片、基板或其類似物之黏著,組合物可與偶合劑組合。此偶合劑可包含鈦酸鹽偶合劑、矽烷偶合劑或類似偶合劑。鈦酸鹽偶合劑可包含三(異硬脂酸)異丙氧基鈦。矽烷偶合劑可包含3-縮水甘油氧基丙基三甲氧基矽烷、3-縮水甘油氧基丙基甲基二乙氧基矽烷、2-(3,4-環氧基環己基)乙基三甲氧基矽烷或類似含環氧基之烷氧基矽烷;N-(2-胺基乙基)-3-胺基丙基三甲氧基矽烷、3-胺基丙基三乙氧基矽烷、N-苯基-3-胺基丙基三甲氧基矽烷或類似含胺烷氧基矽烷;3-巰基丙基三甲氧基矽烷或類似含巰基烷氧基矽烷;十八烷基三甲氧基矽烷或類似含長鏈烷基之矽烷。關於可使用上述矽烷偶合劑(F)之量無特定限制,但通常建議此試劑之添加量不超過每100質量份組份(A)10質量份,較佳0.01至10質量份。
組合物之其他任選組份之實例可為四甲氧基矽烷、四乙氧基矽烷、二甲基二甲氧基矽烷、甲基苯基二甲氧基矽烷、甲基苯基二乙氧基矽烷、苯基三甲氧基矽烷、甲基三甲氧基矽烷、甲基三乙氧基矽烷、乙烯基三甲氧基矽烷、烯丙基三甲氧基矽烷、烯丙基三乙氧基矽烷或類似烷氧基矽烷。
本發明之組合物係藉由將組份(A)、(B)及(C)混合並添加需要之其他組份來製備。關於用以混合該等組份之方法無特定限制。舉例而言,可同時混合組份(A)、(B)及(C)及需要之任選組份,或可在預混合(A)、(B)及(C)後添加上述任選組份。同樣,關於可用於混合之設備無限制。舉例而言,此設備可為單軸型或雙軸型連續混合機、雙輥研磨機、三輥研磨機、Ross混合機、Hobart混合機、牙科混合機、行星式混合機或捏合混合機。
除用作半導體晶片或電配線之保護劑外,本發明之固化體亦可用以在半導體晶片或印刷電路板上形成絕緣層或衝擊吸收層。關於自組合物獲得之固化體之形式無特定限制,且固化體可製成橡膠、硬橡膠或樹脂形式,但最佳具有不超過2 GPa之彈性複合模數。
本發明之組合物亦可用於轉注成形、射出成形、灌注、澆鑄、粉末塗佈、浸塗、逐滴塗覆等。使用方法可選自灌注、施配、篩網印刷或塗佈;然而鑒於方便使用及減少材料消耗,液體或糊狀形式之組合物為較佳者。由於本發明之組合物適於形成特徵為優良可撓性及黏著性之固化體,因此該組合物最適於用作密封劑、澆鑄劑、塗佈劑、黏著劑或其類似物以與電裝置或電子元件一起使用。
下文為本發明之電子組件的更詳細說明。本發明之電子組件之特徵在於其部件係藉由使用本發明組合物之固化體密封或黏結。該等組份之實例可為二極體、電晶體、閘流體、單片IC、混合式IC、LSI或VLSI。
本發明之電子組件之一實例以LSI橫截面之形式顯示於圖1中。此圖說明一電子組件,其中一散熱元件或一黏結元件係使用本發明之可固化之聚矽氧組合物製得。圖1中所示之電子組件具有一半導體元件1,其係安裝於一具有一配線之基板2上且藉助於半導體元件1上所提供之諸如球狀柵格3之焊料凸塊與該基板配線電連接。該基板之材料可包含玻璃強化環氧樹脂、Bakelite樹脂、酚系樹脂或類似有機樹脂;氧化鋁或類似陶瓷;銅、鋁或類似金屬。除半導體元件1外,該組件可含有電阻器、電容器、線圈或其他電子部件。圖1中顯示半導體元件1與基板2之間的空隙填充有底部填充材料,但該底部填充材料之使用係可選的。
半導體裝置1經由一散熱元件6與一熱擴散器4連接。熱擴散器4係藉助於一黏結元件5與基板2黏結。另外,熱擴散器4經由一散熱元件8與一散熱片7連接。熱擴散器4及散熱片7可由鋁、銅、鎳或類似金屬製得。在圖1所示之電子裝置中,黏結元件5係由本發明之可固化之聚矽氧組合物之固化體製得。另外,在圖1之電子組件中,散熱元件6及/或散熱元件8亦可由本發明之可固化之聚矽氧組合物之固化體製得。本發明之可固化之聚矽氧組合物之固化體可用於將半導體元件1黏結至熱擴散器4或用於將熱擴散器4黏結至基板2。為了便於維護,散熱元件8可由導熱性油脂替代。
關於製造本發明之電子組件之方法無特定限制。舉例而言,圖1所示之結構可如下製造。首先,將半導體元件1置放於基板2上,且藉助於柵格3將半導體裝置1與基板2電連接。此後,若需要,則使用底部填充材料。在下一步驟中,將半導體元件1之表面用具有導熱特性之可固化之聚矽氧組合物塗佈,附著熱擴散器4,且使可固化之聚矽氧組合物固化。由此,熱擴散器4經由具有塗佈於該熱擴散器上之固化之聚矽氧組合物黏結於基板2上。在下一步驟中,將具有導熱特性之可固化之聚矽氧組合物或導熱性油脂塗覆於熱擴散器4上,且附著散熱片7。若該熱擴散器係經可固化之聚矽氧組合物塗佈,則隨後使其固化。
現將參照應用實例及比較實例來進一步更詳細地描述本發明之可固化之聚矽氧組合物及電子組件。所有實例中所用之黏度值均係對應於25℃。質量平均分子量為藉由使用甲苯作為溶劑獲得之值且係藉由凝膠滲透層析量測且係參照聚苯乙烯計算。
此特徵係藉助於E型黏度計(數位黏度計DV-U-E II-型,Tokimec Company,Ltd.之產品)在25℃下以2.5 rpm之旋轉速度量測。
將氧化鋁板上之50-μm厚之可固化之聚矽氧組合物層黏貼於具有10 mm×10 mm正方形橫截面之矽晶片上,且接著藉由在150℃下加熱1小時使上述可固化之聚矽氧組合物固化來製得試件。將所得試件在黏結強度測試機(型號SS-100KP,Seishin Trading Company,Ltd.之產品)上藉由量測25℃及50 mm/min剝離速度下之抗剝離性(kgf/cm2
)進行測試。
在除氣後,將可固化之聚矽氧組合物裝入具有10 mm寬度、50 mm長度及2 mm深度之模穴中且使其在150℃及2.5 MPa壓力下經受加壓固化60分鐘,且接著在180℃下在烘箱中經受二次加熱2小時,藉此獲得組合物固化體之試樣。藉助於Rheometric Scientific,Inc.之ARES黏彈性分析儀量測此試樣之複合彈性模數。在25℃下使用0.05%應變及1 Hz振動頻率進行量測。
將0.2 g之量的可固化之聚矽氧組合物滴至磨砂玻璃表面上,且在25℃下保持48小時後,藉助於以下公式計算滲油特徵:100×(L1
-L0
)/L0
其中L0
為可固化之聚矽氧橡膠之直徑,且L1
為滲油所形成之直徑。
藉由混合以下各物來製備可固化之聚矽氧組合物:4.38質量份之以下平均單元式之有機聚矽氧烷:
(質量平均分子量=1,000;黏度=1,290 mPa.s;環氧當量=267);8.46質量份之由以下式表示之有機三矽氧烷:
(黏度=2,600 mPa.s;酚羥基當量=330);0.99質量份之由下式表示之環氧化合物:
0.43質量份之十八烷基三甲氧基矽烷;68.64質量份之具有8.6 μm平均粒度之球形氧化鋁顆粒;15.92質量份之具有3 μm平均粒度之不規則形狀之氧化鋁顆粒;及1.19質量份之雙酚A型環氧樹脂與雙酚F型環氧樹脂之混合物(含有35重量%之經囊封胺型催化劑(HX-3941HP,Asahi Kasei Company,Ltd.之產品))。該可固化之聚矽氧組合物及其固化體之特徵在表1中給出。
藉由混合以下各物來製備可固化之聚矽氧組合物:6.43質量份之以下平均單元式之有機聚矽氧烷:
(質量平均分子量=1,000;黏度=1,290 mPa.s;環氧當量=267);7.57質量份之由下式表示之有機三矽氧烷:
(黏度=2,600 mPa.s;酚羥基當量=330);0.43質量份之十八烷基三甲氧基矽烷;68.54質量份之具有8.6 μm平均粒度之球形氧化鋁顆粒;15.89質量份之具有3 μm平均粒度之不規則形狀之氧化鋁顆粒;及1.14質量份之雙酚A型環氧樹脂與雙酚F型環氧樹脂之混合物(含有35重量%之經囊封胺型催化劑(HX-3941HP,Asahi Kasei Company,Ltd.之產品))。該可固化之聚矽氧組合物及其固化體之特徵在表1中給出。
藉由混合以下各物來製備可固化之聚矽氧組合物:8.0質量份之以下平均單元式之有機聚矽氧烷:
(質量平均分子量=1,000;黏度=1,290 mPa.s;環氧當量=267);10.7質量份之由下式表示之有機三矽氧烷:
(黏度=2,600 mPa.s;酚羥基當量=330);0.5質量份之由下式表示之環氧化合物:
62.9質量份之具有8.6 μm平均粒度之球形氧化鋁顆粒;17.1質量份之具有3 μm平均粒度之不規則形狀之氧化鋁顆粒;及0.8質量份之雙酚A型環氧樹脂與雙酚F型環氧樹脂之混合物(含有35重量%之經囊封胺型催化劑(HX-3941HP,Asahi Kasei Company,Ltd.之產品))。該可固化之聚矽氧組合物及其固化體之特徵在表1中給出。
藉由混合以下各物來製備可固化之聚矽氧組合物:7.7質量份之以下平均單元式之有機聚矽氧烷:
(質量平均分子量=1,000;黏度=1,290 mPa.s;環氧當量=267);10.7質量份之由下式表示之有機三矽氧烷:
(黏度=2,600 mPa.s;酚羥基當量=330);1.5質量份之由下式表示之有機三矽氧烷:(CH3
)3
SiO[(CH3
)2
SiO]25
Si(CH3
)2
-Z(其中Z為由下式表示之二甲基聚矽氧烷:
(質量平均分子量=2,500;黏度=75 mPa.s);62.9質量份之具有8.6 μm平均粒度之球形氧化鋁顆粒;17.1質量份之具有3 μm平均粒度之不規則形狀之氧化鋁顆粒;及0.8質量份之雙酚A型環氧樹脂與雙酚F型環氧樹脂之混合物(含有35重量%之經囊封胺型催化劑(HX-3941HP,Asahi Kasei Company,Ltd.之產品))。該可固化之聚矽氧組合物及其固化體之特徵在表1中給出。
藉由混合以下各物來製備可固化之聚矽氧組合物:6.2質量份之以下平均單元式之有機聚矽氧烷:
(質量平均分子量=1,000;黏度=1,290 mPa.s;環氧當量=267);10.5質量份之由下式表示之有機三矽氧烷:
(黏度=2,600 mPa.s;酚羥基當量=330);2.0質量份之由下式表示之環氧化合物:(CH3
)3
SiO[(CH3
)2
SiO]25
Si(CH3
)2
-Z(其中Z為由下式表示之二甲基聚矽氧烷:
(質量平均分子量=2,500;黏度=75 mPa.s);0.5質量份之由下式表示之環氧化合物:
62.9質量份之具有8.6 μm平均粒度之球形氧化鋁顆粒;17.1質量份之具有3 μm平均粒度之不規則形狀之氧化鋁顆粒;及0.8質量份之雙酚A型環氧樹脂與雙酚F型環氧樹脂之混合物(含有35重量%之經囊封胺型催化劑(HX-3941HP,Asahi Kasei Company,Ltd.之產品))。該可固化之聚矽氧組合物及其固化體之特徵在表1中給出。
藉由混合以下各物來製備可固化之聚矽氧組合物:3.3質量份之以下平均單元式之二甲基聚矽氧烷:X-CH2
CH2
(CH3
)2
SiO[(CH3
)2
SiO]162
Si(CH3
)2
CH2
CH2
-X{其中X為以下平均單元式之有機聚矽氧烷殘基:[Y(CH3
)2
SiO1/2
]1.6
(SiO4/2
)1.0
(其中Y為一單鍵、三甲氧基矽烷基丙基或3-縮水甘油氧基丙基;一個分子中至少一個Y為單鍵,且剩餘部分之Y由以1:4之莫耳比使用之三甲氧基矽烷基丙基及3-縮水甘油氧基丙基組成)}(質量平均分子量=51,000;黏度=12,000 mPa.s);6.0質量份之以下平均單元式之有機聚矽氧烷:
(質量平均分子量=1,000;黏度=1,290 mPa.s;環氧當量=267);9.4質量份之由下式表示之有機三矽氧烷:
(黏度=2,600 mPa.s;酚羥基當量=330);0.5質量份之由下式表示之環氧化合物:
(黏度=2,600 mPa.s;酚羥基當量=330);62.9質量份之具有8.6 μm平均粒度之球形氧化鋁顆粒;17.1質量份之具有3 μm平均粒度之不規則形狀之氧化鋁顆粒;及0.8質量份之雙酚A型環氧樹脂與雙酚F型環氧樹脂之混合物(含有35重量%之經囊封胺型催化劑(HX-3941HP,Asahi Kasei Company,Ltd.之產品))。該可固化之聚矽氧組合物及其固化體之特徵在表1中給出。
由於本發明之可固化之聚矽氧組合物之特徵在於優良之可處理性,因此其適於轉注成形、射出成形、灌注、澆鑄、粉末塗覆、浸塗、逐滴塗覆等。另外,由於在固化後,該組合物形成特徵在於優良可撓性及黏著性之固化體,因此該組合物適於用作密封劑、澆鑄劑、塗佈劑、黏著劑等,與電裝置或電子裝置之部件一起使用。特定言之,當該組合物含有導熱性填充劑時,該組合物可用作散熱材料及散熱介面元件(TIM)。
1...半導體元件
2...基板
3...球狀柵格
4...熱擴散器
5...黏結元件
6...散熱元件
7...散熱片
8...散熱元件
圖1為作為本發明之電子組件之一實例的LSI之橫截面圖。
1...半導體元件
2...基板
3...球狀柵格
4...熱擴散器
5...黏結元件
6...散熱元件
7...散熱片
8...散熱元件
Claims (15)
- 一種可固化之聚矽氧組合物,其包含至少以下組份:(A):(A1 )一個分子中含有至少兩個含環氧基單價有機基團且由以下通式表示之有機聚矽氧烷:(R1 3 SiO1/2 )a (R2 2 SiO2/2 )b (R3 SiO3/2 )c 其中R1 、R2 及R3 可相同或不同且表示經取代或未經取代之單價烴基或上述含環氧基之單價烴基;然而,不少於20莫耳%之R3 所表示之基團為芳基;且其中"a"、"b"及"c"為滿足以下條件之數字:0a0.8;0b0.8;0.2c0.9;a+b+c=1)及/或(A2 )以下通式之二有機聚矽氧烷:A-R5 -(R4 2 SiO)m R4 2 Si-R5 -A其中R4 為經取代或未經取代之不含不飽和脂族鍵之單價烴基;R5 為二價有機基團;"m"為一等於或大於1之整數;且"A"為由以下平均單元式表示之矽氧烷殘基:(XR4 2 SiO1/2 )d (SiO4/2 )e 其中R4 係如上文所定義,且"X"為一單鍵、氫原子、R4 所表示之基團、含環氧基之單價有機基團或烷氧基矽烷基烷基;然而,一個分子中至少一個由"X"表示之基團為一單鍵,至少兩個由"X"表示之基團為含環氧基之單價有機基團;"d"為一正數;"e"為一正數;且"d/e"為0.2至4範圍內之一數字;(B)環氧樹脂之固化劑;及 (C)由以下通式表示之環氧化合物:
- 如請求項1之可固化之聚矽氧組合物,其中組份(B)為具有酚羥基之化合物。
- 如請求項2之可固化之聚矽氧組合物,其中組份(B)為一個分子中含有至少兩個酚羥基之有機矽氧烷。
- 如請求項3之可固化之聚矽氧組合物,其中組份(B)為以下通式之有機矽氧烷:R6 3 SiO(R6 2 SiO)n SiR6 3 其中R6 為經取代或未經取代之單價烴基或含有酚羥基之單價有機基團;然而,一個分子中至少兩個由R6 表示之基團為含有酚羥基之單價有機基團,且"n"為0至1000範圍內之一整數。
- 如請求項1之可固化之聚矽氧組合物,其中所含組份(B)之量為每100質量份組份(A)0.1至500質量份。
- 如請求項1之可固化之聚矽氧組合物,其中所含組份(C)之量為該可固化之聚矽氧組合物之0.01至50質量%。
- 如請求項1之可固化之聚矽氧組合物,其進一步含有(D)固化促進劑。
- 如請求項7之可固化之聚矽氧組合物,其中組份(D)為經囊封之胺型固化促進劑。
- 如請求項7之可固化之聚矽氧組合物,其中所含組份(D)之量不超過每100質量份組份(A)50質量份。
- 如請求項1之可固化之聚矽氧組合物,其進一步含有(E)填充劑。
- 如請求項10之可固化之聚矽氧組合物,其中所含組份(E)之量不超過每100質量份組份(A)5,000質量份。
- 如請求項10之可固化之聚矽氧組合物,其中組份(E)為導熱性填充劑。
- 如請求項1之可固化之聚矽氧組合物,其進一步含有(F)有機環氧樹脂。
- 如請求項13之可固化之聚矽氧組合物,其中所含組份(F)之量不超過每100質量份組份(A)500質量份。
- 一種電子組件,其係藉助於如請求項1至14中任一項之可固化之聚矽氧組合物之一固化體密封或黏結。
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EP2722366B1 (en) | 2011-06-17 | 2023-01-04 | LG Chem, Ltd. | Curable composition |
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