JP4927363B2 - 微小粒子含有組成物 - Google Patents
微小粒子含有組成物 Download PDFInfo
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- JP4927363B2 JP4927363B2 JP2005235950A JP2005235950A JP4927363B2 JP 4927363 B2 JP4927363 B2 JP 4927363B2 JP 2005235950 A JP2005235950 A JP 2005235950A JP 2005235950 A JP2005235950 A JP 2005235950A JP 4927363 B2 JP4927363 B2 JP 4927363B2
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- 239000010419 fine particle Substances 0.000 title claims abstract description 81
- 239000000203 mixture Substances 0.000 title claims abstract description 69
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 102
- 239000002245 particle Substances 0.000 claims abstract description 74
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 50
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- 239000011859 microparticle Substances 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 22
- 239000003960 organic solvent Substances 0.000 claims description 21
- 239000002184 metal Substances 0.000 claims description 14
- 239000003505 polymerization initiator Substances 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 13
- 239000003607 modifier Substances 0.000 claims description 9
- 229920000642 polymer Polymers 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 238000010539 anionic addition polymerization reaction Methods 0.000 claims description 3
- 238000010538 cationic polymerization reaction Methods 0.000 claims description 3
- 125000003700 epoxy group Chemical group 0.000 claims description 3
- 239000007870 radical polymerization initiator Substances 0.000 claims description 3
- 239000000945 filler Substances 0.000 abstract description 10
- 238000002156 mixing Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 238000005096 rolling process Methods 0.000 abstract description 2
- 238000006073 displacement reaction Methods 0.000 abstract 1
- 238000009826 distribution Methods 0.000 description 19
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 18
- 238000009835 boiling Methods 0.000 description 17
- 239000012736 aqueous medium Substances 0.000 description 13
- 239000003822 epoxy resin Substances 0.000 description 12
- 229920000647 polyepoxide Polymers 0.000 description 12
- 239000003566 sealing material Substances 0.000 description 10
- 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 9
- 239000000843 powder Substances 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 6
- 239000002612 dispersion medium Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 239000000428 dust Substances 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000002609 medium Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 239000012495 reaction gas Substances 0.000 description 3
- 239000011863 silicon-based powder Substances 0.000 description 3
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000008119 colloidal silica Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 2
- 150000002894 organic compounds Chemical group 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- QNODIIQQMGDSEF-UHFFFAOYSA-N (1-hydroxycyclohexyl)-phenylmethanone Chemical compound C=1C=CC=CC=1C(=O)C1(O)CCCCC1 QNODIIQQMGDSEF-UHFFFAOYSA-N 0.000 description 1
- LTQBNYCMVZQRSD-UHFFFAOYSA-N (4-ethenylphenyl)-trimethoxysilane Chemical compound CO[Si](OC)(OC)C1=CC=C(C=C)C=C1 LTQBNYCMVZQRSD-UHFFFAOYSA-N 0.000 description 1
- GTELLNMUWNJXMQ-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical class OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCC(CO)(CO)CO GTELLNMUWNJXMQ-UHFFFAOYSA-N 0.000 description 1
- LVNLBBGBASVLLI-UHFFFAOYSA-N 3-triethoxysilylpropylurea Chemical compound CCO[Si](OCC)(OCC)CCCNC(N)=O LVNLBBGBASVLLI-UHFFFAOYSA-N 0.000 description 1
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- YKFRUJSEPGHZFJ-UHFFFAOYSA-N N-trimethylsilylimidazole Chemical compound C[Si](C)(C)N1C=CN=C1 YKFRUJSEPGHZFJ-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- NOZAQBYNLKNDRT-UHFFFAOYSA-N [diacetyloxy(ethenyl)silyl] acetate Chemical compound CC(=O)O[Si](OC(C)=O)(OC(C)=O)C=C NOZAQBYNLKNDRT-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- SXPLZNMUBFBFIA-UHFFFAOYSA-N butyl(trimethoxy)silane Chemical compound CCCC[Si](OC)(OC)OC SXPLZNMUBFBFIA-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical class C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000004200 deflagration Methods 0.000 description 1
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 description 1
- WHGNXNCOTZPEEK-UHFFFAOYSA-N dimethoxy-methyl-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](C)(OC)CCCOCC1CO1 WHGNXNCOTZPEEK-UHFFFAOYSA-N 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- DOYSNKVXNZSWCT-UHFFFAOYSA-N disilanyl(phenyl)silane Chemical compound [SiH3][SiH2][SiH2]C1=CC=CC=C1 DOYSNKVXNZSWCT-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000008393 encapsulating agent Substances 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 1
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 description 1
- LWFWUJCJKPUZLV-UHFFFAOYSA-N n-trimethylsilylacetamide Chemical compound CC(=O)N[Si](C)(C)C LWFWUJCJKPUZLV-UHFFFAOYSA-N 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 230000009291 secondary effect Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- BCNZYOJHNLTNEZ-UHFFFAOYSA-N tert-butyldimethylsilyl chloride Chemical compound CC(C)(C)[Si](C)(C)Cl BCNZYOJHNLTNEZ-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- PYJJCSYBSYXGQQ-UHFFFAOYSA-N trichloro(octadecyl)silane Chemical compound CCCCCCCCCCCCCCCCCC[Si](Cl)(Cl)Cl PYJJCSYBSYXGQQ-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- FTVLMFQEYACZNP-UHFFFAOYSA-N trimethylsilyl trifluoromethanesulfonate Chemical compound C[Si](C)(C)OS(=O)(=O)C(F)(F)F FTVLMFQEYACZNP-UHFFFAOYSA-N 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Images
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- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
- Adhesives Or Adhesive Processes (AREA)
Description
全体の体積基準で95%以上の粒子が粒径1.0μm以下であり、
式(1):{(粒径が体積基準でのモード径以下の粒子の体積)/(残余の粒子の体積)}で表される値が1.0以上である微小粒子と、
(b)該微小粒子を分散する有機組成物からなるマトリクス材料と、を有し、
前記有機組成物はエポキシ基を化学構造中に有する高分子前駆体を含有することを特徴とする。また、本発明の微小粒子含有有機組成物は流動性をもち、硬化可能な微小粒子含有組成物である。
本発明のアンダーフィル材の製造方法は特に限定しない。例えば、表面が疎水性の微小粒子はそのまま有機組成物と混ぜることで目的とするアンダーフィル材を得ることができる。
シリカ微小粒子(100.0質量部のスノーテックスOL)と、有機組成物(24.0質量部のエポキシ樹脂としてのZX−1059、220.0質量部の有機溶媒としてのプロピレングリコールモノメチルエーテル、1.5質量部のKBM−503)とを混合した後、120℃で5時間保持することでプロピレングリコールモノメチルエーテルを揮発させて不透明でゲル状の微小粒子含有組成物を調製した。
30mm×60mmの方形のガラス板の長辺下側に厚さ50μmの両面テープを貼り付け、20mm×80mmの方形のガラス板の上に載せた。両面テープを貼り付けていない一辺(短辺)にシリンジを用いて万遍なく微小粒子含有組成物をディスペンスした。ディスペンスした直後を基準として対辺まで(20mm)到達した時間を測定した。
Claims (6)
- (a)体積平均粒径が1nm以上、100nm以下であって、
全体の体積基準で95%以上の粒子が粒径1.0μm以下であり、
式(1):{(粒径が体積基準でのモード径以下の粒子の体積)/(残余の粒子の体積)}で表される値が1.0以上である微小粒子と、
(b)該微小粒子を分散する有機組成物からなるマトリクス材料と、を有し、
前記有機組成物はエポキシ基を化学構造中に有する高分子前駆体を含有することを特徴とする流動性をもつ硬化可能な微小粒子含有有機組成物であるアンダーフィル材。 - 前記微小粒子はシリカから構成されているか、又は、シリカを含有するかのいずれかである請求項1に記載のアンダーフィル材。
- 前記有機組成物はシランカップリング剤及び/又はシリル化剤からなる表面改質剤を含有する請求1又は2に記載のアンダーフィル材。
- 前記有機組成物はラジカル重合開始剤、アニオン重合開始剤及びカチオン重合開始剤のうちから選択される1種以上の重合開始剤を含有する請求項1〜3のいずれかに記載のアンダーフィル材。
- 前記有機組成物は有機溶媒を含有する請求項1〜4のいずれかに記載のアンダーフィル材。
- 前記シリカ微小粒子は金属ケイ素と酸素とを反応させる方法にて製造されている請求項1〜5のいずれかに記載のアンダーフィル材。
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JP5042529B2 (ja) * | 2005-05-30 | 2012-10-03 | 株式会社アドマテックス | 微小粒子含有組成物及びその製造方法 |
JP5281250B2 (ja) * | 2007-03-29 | 2013-09-04 | 株式会社アドマテックス | 樹脂組成物添加用無機粉末及び樹脂組成物 |
JP5236198B2 (ja) * | 2007-03-29 | 2013-07-17 | 株式会社アドマテックス | 樹脂組成物添加用無機粉末及び樹脂組成物 |
JP2009185132A (ja) * | 2008-02-04 | 2009-08-20 | Sekisui Chem Co Ltd | 電子部品用接着剤及び電子部品用接着剤の製造方法 |
JP5123965B2 (ja) | 2010-03-03 | 2013-01-23 | 東京印刷機材トレーディング株式会社 | オフセット枚葉印刷機用圧胴・渡し胴ジャケット |
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WO2023136331A1 (ja) | 2022-01-13 | 2023-07-20 | 日産化学株式会社 | 粒度分布を有するシリカゾル及びその製造方法 |
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