JPH01172433A - Filler for semiconductor sealing material - Google Patents
Filler for semiconductor sealing materialInfo
- Publication number
- JPH01172433A JPH01172433A JP32963687A JP32963687A JPH01172433A JP H01172433 A JPH01172433 A JP H01172433A JP 32963687 A JP32963687 A JP 32963687A JP 32963687 A JP32963687 A JP 32963687A JP H01172433 A JPH01172433 A JP H01172433A
- Authority
- JP
- Japan
- Prior art keywords
- filler
- silica
- glass
- thermal expansion
- mol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000945 filler Substances 0.000 title claims description 49
- 239000004065 semiconductor Substances 0.000 title claims description 17
- 239000003566 sealing material Substances 0.000 title description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 16
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 14
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 14
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 9
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 8
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 5
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 4
- 239000008393 encapsulating agent Substances 0.000 claims description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 239000004480 active ingredient Substances 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 238000005538 encapsulation Methods 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims 1
- 239000011521 glass Substances 0.000 abstract description 23
- 238000010438 heat treatment Methods 0.000 abstract description 12
- 230000035939 shock Effects 0.000 abstract description 11
- 229910000679 solder Inorganic materials 0.000 abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 5
- 238000007654 immersion Methods 0.000 abstract description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 2
- GOLCXWYRSKYTSP-UHFFFAOYSA-N Arsenious Acid Chemical compound O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 abstract 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 abstract 2
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 abstract 1
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 abstract 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N nickel(II) oxide Inorganic materials [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 abstract 1
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 28
- 238000000034 method Methods 0.000 description 22
- 239000000843 powder Substances 0.000 description 17
- -1 ^' zO x Substances 0.000 description 13
- 229920005989 resin Polymers 0.000 description 13
- 239000011347 resin Substances 0.000 description 13
- 230000000694 effects Effects 0.000 description 11
- 239000000203 mixture Substances 0.000 description 11
- 238000000465 moulding Methods 0.000 description 11
- 239000003822 epoxy resin Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 229920000647 polyepoxide Polymers 0.000 description 10
- 230000008646 thermal stress Effects 0.000 description 9
- 239000013078 crystal Substances 0.000 description 8
- 229910021495 keatite Inorganic materials 0.000 description 8
- 239000011342 resin composition Substances 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 7
- 230000008025 crystallization Effects 0.000 description 6
- 239000006104 solid solution Substances 0.000 description 6
- 229910000500 β-quartz Inorganic materials 0.000 description 6
- 238000005452 bending Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 238000011049 filling Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000004593 Epoxy Substances 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000001186 cumulative effect Effects 0.000 description 4
- 230000006378 damage Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229920000728 polyester Polymers 0.000 description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical class [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N 4-methylimidazole Chemical compound CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- 239000004734 Polyphenylene sulfide Substances 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229920000800 acrylic rubber Polymers 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 239000000378 calcium silicate Substances 0.000 description 2
- 229910052918 calcium silicate Inorganic materials 0.000 description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 2
- 239000004203 carnauba wax Substances 0.000 description 2
- 235000013869 carnauba wax Nutrition 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229920003986 novolac Polymers 0.000 description 2
- 239000004843 novolac epoxy resin Substances 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 229920000069 polyphenylene sulfide Polymers 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000010583 slow cooling Methods 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 2
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 2
- WXBBHXYQNSLMDI-UHFFFAOYSA-N (2-tert-butylphenyl) 2-hydroxybenzoate Chemical compound CC(C)(C)C1=CC=CC=C1OC(=O)C1=CC=CC=C1O WXBBHXYQNSLMDI-UHFFFAOYSA-N 0.000 description 1
- MUTGBJKUEZFXGO-OLQVQODUSA-N (3as,7ar)-3a,4,5,6,7,7a-hexahydro-2-benzofuran-1,3-dione Chemical compound C1CCC[C@@H]2C(=O)OC(=O)[C@@H]21 MUTGBJKUEZFXGO-OLQVQODUSA-N 0.000 description 1
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 description 1
- RUEBPOOTFCZRBC-UHFFFAOYSA-N (5-methyl-2-phenyl-1h-imidazol-4-yl)methanol Chemical compound OCC1=C(C)NC(C=2C=CC=CC=2)=N1 RUEBPOOTFCZRBC-UHFFFAOYSA-N 0.000 description 1
- AHBGXHAWSHTPOM-UHFFFAOYSA-N 1,3,2$l^{4},4$l^{4}-dioxadis***e 2,4-dioxide Chemical compound O=[Sb]O[Sb](=O)=O AHBGXHAWSHTPOM-UHFFFAOYSA-N 0.000 description 1
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 description 1
- IEKHISJGRIEHRE-UHFFFAOYSA-N 16-methylheptadecanoic acid;propan-2-ol;titanium Chemical compound [Ti].CC(C)O.CC(C)CCCCCCCCCCCCCCC(O)=O.CC(C)CCCCCCCCCCCCCCC(O)=O.CC(C)CCCCCCCCCCCCCCC(O)=O IEKHISJGRIEHRE-UHFFFAOYSA-N 0.000 description 1
- ACUUVWABACRCCZ-UHFFFAOYSA-N 2-(2-ethyl-1h-imidazol-5-yl)propanenitrile Chemical class CCC1=NC=C(C(C)C#N)N1 ACUUVWABACRCCZ-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 1
- JMMZCWZIJXAGKW-UHFFFAOYSA-N 2-methylpent-2-ene Chemical compound CCC=C(C)C JMMZCWZIJXAGKW-UHFFFAOYSA-N 0.000 description 1
- MPKIZIGHGVKHDY-UHFFFAOYSA-N 2-tert-butyl-5-methylbenzene-1,4-diol Chemical compound CC1=CC(O)=C(C(C)(C)C)C=C1O MPKIZIGHGVKHDY-UHFFFAOYSA-N 0.000 description 1
- VEORPZCZECFIRK-UHFFFAOYSA-N 3,3',5,5'-tetrabromobisphenol A Chemical compound C=1C(Br)=C(O)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(O)C(Br)=C1 VEORPZCZECFIRK-UHFFFAOYSA-N 0.000 description 1
- XYXBMCIMPXOBLB-UHFFFAOYSA-N 3,4,5-tris(dimethylamino)-2-methylphenol Chemical compound CN(C)C1=CC(O)=C(C)C(N(C)C)=C1N(C)C XYXBMCIMPXOBLB-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
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 1
- ALEBYBVYXQTORU-UHFFFAOYSA-N 6-hydrazinyl-6-oxohexanoic acid Chemical compound NNC(=O)CCCCC(O)=O ALEBYBVYXQTORU-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 229910015900 BF3 Inorganic materials 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000004641 Diallyl-phthalate Substances 0.000 description 1
- 239000002656 Distearyl thiodipropionate Substances 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 1
- 229920000106 Liquid crystal polymer Polymers 0.000 description 1
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 description 1
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000004696 Poly ether ether ketone Substances 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004962 Polyamide-imide Substances 0.000 description 1
- 239000005062 Polybutadiene Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 description 1
- QHWKHLYUUZGSCW-UHFFFAOYSA-N Tetrabromophthalic anhydride Chemical compound BrC1=C(Br)C(Br)=C2C(=O)OC(=O)C2=C1Br QHWKHLYUUZGSCW-UHFFFAOYSA-N 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- UMHKOAYRTRADAT-UHFFFAOYSA-N [hydroxy(octoxy)phosphoryl] octyl hydrogen phosphate Chemical compound CCCCCCCCOP(O)(=O)OP(O)(=O)OCCCCCCCC UMHKOAYRTRADAT-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- HEHRHMRHPUNLIR-UHFFFAOYSA-N aluminum;hydroxy-[hydroxy(oxo)silyl]oxy-oxosilane;lithium Chemical compound [Li].[Al].O[Si](=O)O[Si](O)=O.O[Si](=O)O[Si](O)=O HEHRHMRHPUNLIR-UHFFFAOYSA-N 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910000411 antimony tetroxide Inorganic materials 0.000 description 1
- 229940045985 antineoplastic platinum compound Drugs 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 229920005549 butyl rubber Polymers 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910002026 crystalline silica Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- PWWSSIYVTQUJQQ-UHFFFAOYSA-N distearyl thiodipropionate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCCCCCC PWWSSIYVTQUJQQ-UHFFFAOYSA-N 0.000 description 1
- 235000019305 distearyl thiodipropionate Nutrition 0.000 description 1
- MCPKSFINULVDNX-UHFFFAOYSA-N drometrizole Chemical compound CC1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 MCPKSFINULVDNX-UHFFFAOYSA-N 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- GOAJGXULHASQGJ-UHFFFAOYSA-N ethene;prop-2-enenitrile Chemical group C=C.C=CC#N GOAJGXULHASQGJ-UHFFFAOYSA-N 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
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 239000012765 fibrous filler Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- CAYGQBVSOZLICD-UHFFFAOYSA-N hexabromobenzene Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1Br CAYGQBVSOZLICD-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 239000000314 lubricant Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- UJNZOIKQAUQOCN-UHFFFAOYSA-N methyl(diphenyl)phosphane Chemical compound C=1C=CC=CC=1P(C)C1=CC=CC=C1 UJNZOIKQAUQOCN-UHFFFAOYSA-N 0.000 description 1
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000006082 mold release agent Chemical class 0.000 description 1
- GKTNLYAAZKKMTQ-UHFFFAOYSA-N n-[bis(dimethylamino)phosphinimyl]-n-methylmethanamine Chemical compound CN(C)P(=N)(N(C)C)N(C)C GKTNLYAAZKKMTQ-UHFFFAOYSA-N 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 229910052670 petalite Inorganic materials 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- DOIRQSBPFJWKBE-UHFFFAOYSA-N phthalic acid di-n-butyl ester Natural products CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 150000003058 platinum compounds Chemical class 0.000 description 1
- 229920003192 poly(bis maleimide) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 229920001955 polyphenylene ether Polymers 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
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- 239000005060 rubber Substances 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 125000005480 straight-chain fatty acid group Chemical class 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000001721 transfer moulding Methods 0.000 description 1
- WLPUWLXVBWGYMZ-UHFFFAOYSA-N tricyclohexylphosphine Chemical compound C1CCCCC1P(C1CCCCC1)C1CCCCC1 WLPUWLXVBWGYMZ-UHFFFAOYSA-N 0.000 description 1
- COIOYMYWGDAQPM-UHFFFAOYSA-N tris(2-methylphenyl)phosphane Chemical compound CC1=CC=CC=C1P(C=1C(=CC=CC=1)C)C1=CC=CC=C1C COIOYMYWGDAQPM-UHFFFAOYSA-N 0.000 description 1
- MGMXGCZJYUCMGY-UHFFFAOYSA-N tris(4-nonylphenyl) phosphite Chemical compound C1=CC(CCCCCCCCC)=CC=C1OP(OC=1C=CC(CCCCCCCCC)=CC=1)OC1=CC=C(CCCCCCCCC)C=C1 MGMXGCZJYUCMGY-UHFFFAOYSA-N 0.000 description 1
- QQBLOZGVRHAYGT-UHFFFAOYSA-N tris-decyl phosphite Chemical compound CCCCCCCCCCOP(OCCCCCCCCCC)OCCCCCCCCCC QQBLOZGVRHAYGT-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、半導体封止材用充填剤、特に封止時や半導体
装置が熱履歴を受けた際に発生する熱応力を低減し熱伝
導性を向上させることにより耐熱衝撃性を改善すること
ができる半導体封止材用充填剤に関するものである。[Detailed Description of the Invention] [Field of Industrial Application] The present invention is directed to a filler for semiconductor encapsulant, which reduces thermal stress that occurs during encapsulation or when a semiconductor device undergoes thermal history, and improves thermal conductivity. The present invention relates to a filler for semiconductor encapsulant that can improve thermal shock resistance by improving properties.
従来、半導体封止材としては、エポキシ系樹脂にシリカ
系粉末を充填したものが知られており、シリカ系粉末と
しては熱膨張係数の小さい石英ガラスの粉末やこれより
熱伝導性のよい石英粉末が用いられている。Conventionally, epoxy resin filled with silica-based powder has been known as a semiconductor encapsulation material, and examples of silica-based powder include quartz glass powder with a small coefficient of thermal expansion and quartz powder with better thermal conductivity. is used.
この封止材は通常１６０〜１９０℃の高温で成形して半
導体素子を封止するが、成形後室温まで冷却される間に
封止材と半導体素子との収縮量の差に起因する応力が発
生して半導体素子に歪みを与える。このような熱応力は
半導体素子に変形、割れ、クラック等を生じたり、配線
のスライドやはなはだしい場合には断線を生じるなどの
損傷の原因となる。近年、半導体素子自体が大型チップ
化、高密度化、高精度化すると共に、成形品のパッケー
ジ構造に薄型化、小型化の傾向が強まっているため、こ
のような熱応力によって半導体装置がダメージを受ける
危険性は高まりつつある。This encapsulant is usually molded at a high temperature of 160 to 190°C to encapsulate the semiconductor element, but while it is cooled to room temperature after molding, stress due to the difference in shrinkage between the encapsulant and the semiconductor element is generated. This occurs and causes distortion to the semiconductor device. Such thermal stress causes damage such as deformation, cracking, cracking, etc. in the semiconductor element, sliding of wiring, or disconnection in extreme cases. In recent years, semiconductor devices themselves have become larger chips, more dense, and more precise, and there has been a growing trend toward thinner and smaller package structures for molded products.Semiconductor devices can be damaged by such thermal stress. The risks are increasing.
一方、高密度実装及び実装工程の合理化のため、半田浸
漬もしくは半田リフロー法で半田付けする比率が高まり
、封止材が直接的に半田熱に曝されるようになり、厳し
い耐熱衝撃性が求められると共に半田浸漬後の耐湿信頼
性の確保が重要になりつつある。On the other hand, in order to achieve high-density mounting and rationalize the mounting process, the proportion of soldering using solder immersion or solder reflow methods has increased, and the encapsulant is now directly exposed to soldering heat, requiring severe thermal shock resistance. At the same time, it is becoming important to ensure moisture resistance and reliability after solder immersion.
以上のような問題を解決するためには、イオン性の溶出
不純物の増加を防いで耐湿信頼性を確保し、封止材の熱
応力を低減化する一方で熱伝導性の向上もはかることが
必要である。この要求を実現させるのに、特に封止材中
、最も大きな体積を占める充填剤に関し、以下に示すよ
うな種々の提案がなされている。In order to solve the above problems, it is necessary to prevent the increase in ionic eluted impurities, ensure moisture resistance reliability, reduce the thermal stress of the encapsulant, and improve thermal conductivity. is necessary. In order to realize this requirement, various proposals have been made as shown below, particularly regarding the filler that occupies the largest volume in the sealing material.
■ 高充填化ニジリカガラスは、マトリックス樹脂に比
べ、熱膨張率が１／１００程度である一方熱伝導率は１
０倍ぐらいであることを利用する。高充填化することに
よる成形性の低下を充填材粒子の形状や粒度分布により
改良する技術（特開昭５８−１４５６１３号公報、同５
８−２１９２４２号、同６１−６４７５４号、特公昭６
２−７２１１号公報等）が提案されている。しかしなが
ら、高充填により、封止材の熱膨張係数を素子の倍程度
に抑えるためにはシリカガラス９３重量％位の超高充填
が必要となり根本的な解決法としては非現実的である。■ Highly filled Nijirika glass has a thermal expansion coefficient of about 1/100 compared to matrix resin, but a thermal conductivity of 1/100.
Take advantage of the fact that it is about 0 times. Technology to improve the deterioration of formability due to high filling by changing the shape and particle size distribution of filler particles (JP-A-58-145613, JP-A-58-145613;
No. 8-219242, No. 61-64754, Special Publication No. 6
No. 2-7211, etc.) have been proposed. However, in order to suppress the thermal expansion coefficient of the sealing material to about twice that of the element due to the high filling, an extremely high filling of about 93% by weight of silica glass is required, which is unrealistic as a fundamental solution.
また高充填による封止材の封止時の流動性の変化により
、素子のステージ変位が大きくなり易いという問題点の
指摘もある。一方、粒度分布は成形時に発生するパリの
調整等によっても決まるため、あまり自由に変化させら
れないなど、効果は十分とはいえない。It has also been pointed out that there is a problem that the stage displacement of the element tends to increase due to changes in the fluidity of the sealing material during sealing due to high filling. On the other hand, since the particle size distribution is also determined by the adjustment of particles generated during molding, it cannot be changed very freely, and the effect cannot be said to be sufficient.
■ 低熱膨張化：現在多用されている高純度シリカより
熱膨張率の低いＬｉｇＯ−Ａ Ｊ ｚ０３−５ｉ０２系
材料を使用する技術（特開昭６１−７８１４７号公報）
の提案があるが、これらは、本質的にＬｉ′″イオンを
高濃度で含有するため、封止材の耐湿性を著しく劣化さ
せてしまう、従って充填剤としての使用には耐え得ない
。■ Low thermal expansion: Technology that uses LigO-A J z03-5i02 material, which has a lower coefficient of thermal expansion than the currently widely used high-purity silica (Japanese Patent Laid-Open No. 78147/1983).
However, since these essentially contain Li''' ions at a high concentration, they significantly deteriorate the moisture resistance of the encapsulant, and therefore cannot withstand use as a filler.
■ 高熱伝導化ニジリカガラスの熱伝導性は、金属はも
ちろん、他のセラミックス材料に比較してもあまり良（
ないため、もっと高熱伝導性材料、例えば、＾’ ｚＯ
ｘ 、ＭｇＯ％ ５ＩＪ４ 、ＢＮ等や結晶性シリカ等
を用いて耐熱衝撃性を向上させようとするものであるが
、熱膨張係数がシリカガラスより小さくない限り、封止
材の熱膨張率も小さくならず、この点で現在までに提案
されているいずれの材料も低熱応力化への貢献はないと
いえる。■ High thermal conductivity The thermal conductivity of Nijirika glass is not very good compared to metals and other ceramic materials.
Because there is no higher thermal conductivity material, e.g. ＾' zO
x, MgO% 5IJ4, BN, etc., crystalline silica, etc. are used to improve thermal shock resistance, but unless the coefficient of thermal expansion is smaller than that of silica glass, the coefficient of thermal expansion of the sealing material is also small. In this respect, it can be said that none of the materials proposed to date contribute to reducing thermal stress.
■ 低弾性化：カルシウムシリケートの使用で封止材の
弾性率を低下させることにより、応力の低減化を図る技
術（特開昭５５−１１８９５２号公報）なども提案され
ているが、カルシウムシリケートはシリカより熱膨張係
数が大きいため、低弾性化の効果は相殺されて低熱応力
化の問題に対して本質的な解決策とはなっていない。■ Lower elasticity: Technology has been proposed to reduce stress by lowering the elastic modulus of the sealing material using calcium silicate (Japanese Patent Application Laid-open No. 118952/1983), but calcium silicate Since it has a larger coefficient of thermal expansion than silica, the effect of lowering elasticity is canceled out, and it is not an essential solution to the problem of lowering thermal stress.
以上のように、従来の技術では、半導体技術の著しい進
歩に対して十分な対応がとれず、今後の発展を考える上
で大きな技術的問題となっている。As described above, the conventional technology cannot adequately cope with the remarkable progress in semiconductor technology, which poses a major technical problem when considering future development.
本発明の目的は、現在主に用いられているシリカ系材料
よりも更に小さい熱膨張係数を有し、かつ更に高い熱伝
導率を有し、本質的にアルカリ金属イオンを含有しない
無機粉体を充填剤として用いることにより、前記問題点
に著しい効果を発揮する新たな封止材を堤供しようとす
るものである。The object of the present invention is to create an inorganic powder that has a coefficient of thermal expansion smaller than that of silica-based materials currently mainly used, has a higher thermal conductivity, and essentially does not contain alkali metal ions. The present invention aims to provide a new sealing material that, when used as a filler, exhibits a remarkable effect on the above-mentioned problems.
すなわち、本発明は、アルミニウム、シリコン及びアル
カリ金属以外の金属酸化物７〜３０モル％とアルミナ７
〜３０モル％及びシリカ４０〜８６モル％を含む熱膨張
係数０． Ｉ Ｘ １０−’に一’以下の物質を有効成
分として含有して成ることを特徴とする半導体封止材用
充填剤である。That is, in the present invention, 7 to 30 mol% of metal oxides other than aluminum, silicon, and alkali metals and alumina 7
-30 mol% and 40-86 mol% silica, thermal expansion coefficient 0. This is a filler for semiconductor encapsulant, characterized in that it contains a substance of I x 10-' or less as an active ingredient.
以下、更に詳しく本発明について説明する。The present invention will be explained in more detail below.
本発明におけるアルミニウム、シリコン及びアルカリ金
属以外の金属酸化物（以下、単に金属酸化物という）と
はＡ Ｉ Ｂｏｘ−５’ｌＯｔ系に加えて熱膨張係数０
． Ｉ Ｘ １０−’に一’以下の物質を生成するもの
であれば特に限定するものではないが、封止材として耐
湿信頼性を確保するためにアルカリ金属酸化物は好まし
くない、好ましい金属酸化物はマグネシウム、亜鉛及び
／又は銅の酸化物である。その有効量は製法によっても
異なるがアルミナ７〜３０モル％、シリカ４０〜８６モ
ル％に対して７〜３０モル％であり、好ましくは金属酸
化物及びアルミナはそれぞれ８〜２９モル％、シリカ４
２〜８４モル％であり、更に好ましくは、金属酸化物及
びアルミナはそれぞれ１０〜２８モル％、シリカ４４〜
８０モル％である。金属酸化物及びアルミナがこの範囲
より多いと熱膨張係数の大きな物質が生成し易くなり、
一方、少ないとシリカに比べて小さな熱膨張係数が得ら
れにくい。また、この範囲内で、熱膨張係数の小さな生
成物をえ易いのは（金属酸化物／アルミナ）のモル比が
０．５から２．０である。In the present invention, metal oxides other than aluminum, silicon, and alkali metals (hereinafter simply referred to as metal oxides) are those having a thermal expansion coefficient of 0 in addition to the A I Box-5'lOt system.
．． There is no particular limitation as long as it produces a substance with an I is an oxide of magnesium, zinc and/or copper. The effective amount thereof varies depending on the manufacturing method, but is 7 to 30 mol% for alumina and silica, respectively.
2 to 84 mol%, more preferably 10 to 28 mol% of metal oxide and alumina, and 44 to 28 mol% of silica.
It is 80 mol%. If the amount of metal oxides and alumina exceeds this range, substances with a large coefficient of thermal expansion are likely to be produced.
On the other hand, if the amount is small, it is difficult to obtain a coefficient of thermal expansion smaller than that of silica. Further, within this range, it is easy to obtain a product with a small coefficient of thermal expansion when the molar ratio (metal oxide/alumina) is from 0.5 to 2.0.
本発明の半導体封止材用充填°剤には、さらに以下のＡ
−Ｃ群から選ばれた成分を併用することもできる。The filler for semiconductor encapsulant of the present invention further includes the following A
-Components selected from group C can also be used together.
くＡ群〉
ＴｉＯ２、ＺｒＯ□、Ｈｆ０ｚ、 ＮｉＯ、ＣｒｚＯｓ
、ＶｚＯｓ、＾ｇｚＯ１ｔ
〈Ｂ群〉
Ｐ２Ｏ２、Ａｓ５ｅｓ 、Ｂ２Ｏ３
〈Ｃ群〉
♀
ＢａＯ％ ＳｒＯ、ＣａＯ、希土類元素の酸化物Ｍｎ０
１ａ２０ｓ
Ａ−Ｃ群の成分は、必ずしも酸化物として加える必要は
ないが、封止材としての使用の観点から、塩化物やオキ
シ塩化物、硫化物や硫酸塩、亜硫酸塩など、ＣＺ−やｓ
ｏ、’−を生じ易い化合物はあまり好ましくない、Ａ群
からの選択は比較的効果的であり、特に好ましくはＴｉ
Ｏ□、Ｚｒ０ｚ、ＨｆＯ□である。Group A〉 TiO2, ZrO□, Hf0z, NiO, CrzOs
, VzOs, ^gzO1t <Group B> P2O2, As5es, B2O3 <Group C> ♀ BaO% SrO, CaO, rare earth element oxide Mn0
1a20s The components of the A-C group do not necessarily need to be added as oxides, but from the perspective of use as sealants, they may be added as chlorides, oxychlorides, sulfides, sulfates, sulfites, etc., such as CZ- and s.
Compounds that tend to form o,'- are less preferred; selections from group A are relatively effective; particularly preferred are Ti
O□, Zr0z, and HfO□.
その有効量は０．２〜８モル％であり好ましくは０．５
〜７モル％更に好ましくは１〜６モル％である。Ｂ群か
らの選択は、Ａ群と共に用いればより効果的で０．２＜
（Ａ群成骨／Ｂ群成分）く５が好ましく更に好ましくは
０．３＜（Ａ群成骨／Ｂ群成分）〈３である。またＣ群
は、Ａ、Ｂ群の成分と共に用いられ、その効果の助長や
着色作用をもつ。Its effective amount is 0.2-8 mol%, preferably 0.5
It is 7 mol%, more preferably 1 to 6 mol%. Selection from group B is more effective when used with group A, and 0.2<
(Group A adult bone/B group component) is preferably 5, and more preferably 0.3<(A group adult bone/B group component)<3. Furthermore, Group C is used together with the components of Groups A and B, and has the effect of enhancing the effect and coloring the composition.
多量に用いるのは好ましくなく、好ましくは５モル％以
下更に好ましくは４モル％以下である。Ａ〜Ｃ群成分成
分まり多量に加えても有効成分として作用せず、逆に、
生成物の熱膨張係数の増大をまねくので、その総和は、
金属酸化物を超えない量であることが好ましく特にモル
比で３７４以下である。It is not preferable to use a large amount, and the amount is preferably 5 mol% or less, more preferably 4 mol% or less. Group A to C components do not act as active ingredients even if added in large amounts; on the contrary,
This leads to an increase in the coefficient of thermal expansion of the product, so the total amount is
The amount preferably does not exceed that of the metal oxide, particularly at a molar ratio of 374 or less.
本発明の充填剤の生成は、その組成及び熱膨張係数の測
定により確認されるが、簡易的な手法としてＸ線回折を
用いることもできる。すなわち、β−石英及び／または
キータイト型結晶構造の確認である。β−石英とキータ
イトはシリカの多形であり負の熱膨張係数を持つ物質で
ある。この結晶構造の確認は、測定した物質の主回折線
がβ−石英やキータイトのそれにｔ、を応するかどうか
を見ればよい。但し、本発明の充填剤は固溶体を形成す
るため回折線位置が移動するので注意を要する。Formation of the filler of the present invention is confirmed by measuring its composition and coefficient of thermal expansion, but X-ray diffraction can also be used as a simple method. In other words, the β-quartz and/or keatite crystal structure was confirmed. β-quartz and keatite are polymorphs of silica and are substances with negative coefficients of thermal expansion. The crystal structure can be confirmed by checking whether the principal diffraction line of the measured substance corresponds to that of β-quartz or keatite. However, since the filler of the present invention forms a solid solution, the diffraction line position shifts, so care must be taken.
Ｌｉ２０−Ａ １２０３−５ｉＯ□系のβ−ユークリプ
タイト（β−石英型）やβ−スボデューメン（キータイ
ト型）は格子定数の異なった各種固溶体のデータが比較
的入手容易であるので、これらに対応させてもよい。本
発明の充填剤は、このＸ線回折を用いた確認法によって
限定されるものではないが、熱膨張測定用試片の作製が
困難な場合などには有用な方法といえる。すなわち、主
生成相がβ−石英及び／またはキータイト型固溶体結晶
相であって、原料組成が金属酸化物７〜３０モス％、ア
ルミナ７〜３０モル％、シリカ４０〜８６モル％であれ
ば本発明の充填剤が生成できたとするものである。Li20-A 1203-5iO You may let them. Although the filler of the present invention is not limited to this confirmation method using X-ray diffraction, it can be said to be a useful method in cases where it is difficult to prepare a sample for measuring thermal expansion. That is, if the main formed phase is β-quartz and/or keatite solid solution crystal phase, and the raw material composition is 7 to 30 mos% of metal oxide, 7 to 30 mole% of alumina, and 40 to 86 mole% of silica, this is the case. It is assumed that the filler of the invention was produced.
次に本発明の充填剤の調製法について述べる。Next, a method for preparing the filler of the present invention will be described.
本発明の充填剤の調製法は特に限定するものではないが
、結晶化ガラスの利用は比較的容易な方法である。すな
わち、原料混合物を溶融後冷却してガラス化し、再び過
熱して結晶化させ、これを適当な粒度にして用いるもの
である。原料は酸化物でなくともよく、生成したガラス
が金属酸化物−アルミナ−シリカ系ガラスであればよい
。各成分は均一に分布していることが望ましい。Although the method for preparing the filler of the present invention is not particularly limited, the use of crystallized glass is a relatively easy method. That is, the raw material mixture is melted, cooled to vitrify it, heated again to crystallize it, and then used in a suitable particle size. The raw material does not need to be an oxide, and the resulting glass may be a metal oxide-alumina-silica glass. It is desirable that each component is uniformly distributed.
結晶化法としては、ガラスに金を加えておいて紫外線を
照射する方法なども知られているが、加熱による方法が
最も一般的であり、容易といえる。Although there are known crystallization methods such as adding gold to glass and irradiating it with ultraviolet rays, heating is the most common method and can be said to be easy.
加熱方法は系が均一に加熱されればどのような方法でも
よいが、あまり急激な加熱はガラスの破損を招き易く、
あまりゆっくり加熱すると時間がかかるため１〜ｂ
晶化温度はガラスの組成によっても異なるが、７５０〜
１２００℃程度である。あまり高温で加熱すると熱膨張
率の大きな相が生成し易く、あまり低温で加熱しても結
晶化は起こらないかもしくは非常に長時間を要するため
好ましくない。Any heating method may be used as long as the system is heated uniformly, but heating too rapidly can easily lead to glass breakage.
If the heating is too slow, it will take a long time, so the crystallization temperature will vary depending on the composition of the glass, but the crystallization temperature will vary depending on the composition of the glass.
The temperature is about 1200°C. Heating at too high a temperature tends to generate a phase with a large coefficient of thermal expansion, and heating at too low a temperature either does not cause crystallization or takes a very long time, which is not preferable.
効率的にかつ安定した結晶化を行なってβ−石英やキー
タイト型固溶体結晶を生成する方法として多段式の加熱
法がある。これは、まず徐冷温度から軟化温度までの間
の温度で加熱して結晶核形成を行ない、次に軟化点以上
で熱して結晶を生成させる方法である。核形成の前段階
に分相のために加熱をする場合もある。この分相や核形
成を安定して行なわせるために前述の添加成分Ａ群が効
果があり、Ｂ群成分はその働きを助ける。加熱パターン
の１例を挙げれば、Ｚｎ０−Ａ １２０３−Ｓｉ０ｇガ
ラスからβ−石英やキータイト型（亜鉛ペタライト）の
固溶体を結晶化させる場合には、まず７２５〜８００℃
で２〜６時間加熱し、次いで８００〜９５０℃に昇温し
で１〜８時間加熱する。本発明の充填剤の調製法は、こ
の方法に限定されるものではなく、例えば昇温速度のコ
ントロールによってもよい。−例を挙げれば、Ｃｕｚｏ
１２．７モル％、Ａ７！ｚＯ＋１２．７モル％、 Ｓ
ｉＯ□７４．６モル％のガラスを５℃／ｌｌｌ１ｎで室
温より１ 、０００℃まで加熱すればキータイト型固溶
体結晶が生成し、熱膨張係数は一〇、 ６ Ｘ Ｉ Ｏ
−ｂ／”Ｃとなる。ガラスの作製法も溶融法に限定され
るものではなく、ゾル−ゲル法なども用いることができ
る。また、ガラスを経由することなく、非晶質の混合塩
から直接合成することもできる。A multistage heating method is known as a method for efficiently and stably crystallizing β-quartz or keatite type solid solution crystals. This is a method in which the material is first heated at a temperature between the slow cooling temperature and the softening temperature to form crystal nuclei, and then heated above the softening point to form crystals. In some cases, heating is performed for phase separation before nucleation. In order to stably perform this phase separation and nucleation, the above-mentioned additive components of Group A are effective, and Group B components assist in this function. To give an example of a heating pattern, when crystallizing β-quartz or keatite type (zinc petalite) solid solution from Zn0-A 1203-Si0g glass, first the temperature is 725-800°C.
Heat for 2 to 6 hours, then raise the temperature to 800 to 950°C and heat for 1 to 8 hours. The method for preparing the filler of the present invention is not limited to this method, but may also be performed by controlling the heating rate, for example. -For example, Cuzo
12.7 mol%, A7! zO+12.7 mol%, S
If glass containing 74.6 mol% of iO□ is heated from room temperature to 1,000°C at 5°C/lll1n, keatite type solid solution crystals are formed, and the coefficient of thermal expansion is 10.6 X I O
-b/”C.The method for producing glass is not limited to the melting method, and a sol-gel method can also be used.Also, it is possible to produce glass from an amorphous mixed salt without going through glass. Direct synthesis is also possible.
結晶化ガラスを利用する際の結晶化度は、特に限定はし
ないが、熱伝導率を増大させるにはより結晶化させた方
が好ましい。充填剤の高熱伝導化は封止材の高熱伝導化
をもたらし、低熱応力化による耐熱衝撃性向上の効果を
より大きくし、半導体装置の放熱性を向上させる。特に
従来用いられている溶融シリカガラスは室温から７００
にの範囲で１．３８〜１．９２ Ｗ／に、ｍと熱の不良
４体である為その改善効果は大きい。結晶化による熱伝
導率の増大の１例を示せば、金属酸化物にＭｇＯとＺｎ
Ｏを用いてキータイト型固溶体結晶を析出させた場合、
Ｘ線による結晶化度の測定が５０％で、熱膨張係数がＯ
Ｋ−’、熱伝導率は３．４Ｗ／に、ｎ＋ 、７０％で、
それぞれ−〇、７ Ｘ １０−’に一’、４．１ Ｗ／
に、鵬であった。熱伝導率は、好ましくは室温〜２００
℃で２．０ Ｗ／に、ｍ以上更に好ましくは２．５ Ｗ
／に、ｍ以上更に好ましくは３． ＯＷ／に、ｍ以上で
ある。The degree of crystallization when using crystallized glass is not particularly limited, but it is preferable to make it more crystallized in order to increase thermal conductivity. High thermal conductivity of the filler brings about high thermal conductivity of the encapsulant, which further increases the effect of improving thermal shock resistance due to lower thermal stress, and improves the heat dissipation of the semiconductor device. In particular, conventionally used fused silica glass has a temperature of 700% from room temperature.
In the range of 1.38 to 1.92 W/, the improvement effect is large since there are 4 defects in m and heat. An example of an increase in thermal conductivity due to crystallization is when metal oxides include MgO and Zn.
When a keatite solid solution crystal is precipitated using O,
The degree of crystallinity measured by X-ray is 50%, and the coefficient of thermal expansion is O.
K-', thermal conductivity is 3.4 W/, n+, 70%,
-〇, 7 x 10-' to 1', 4.1 W/respectively
It was Peng. Thermal conductivity is preferably from room temperature to 200
℃ to 2.0 W/m, more preferably 2.5 W/m or more
m or more, more preferably 3. OW/is greater than or equal to m.
本発明の充填剤は以上のようにして得られた粉末やより
大きなバルクをそのまま、あるいは粒度や粒子形状を調
整して用いる。粉砕・造粒・分級等は必要に応じて結晶
化の前後、あるいはその両者で行なう。粒子形状は、通
常の破砕形状以外に、球状、繊維状、鱗片状など種々の
ものを用いるこきとができる。これは、ゾル−ゲル法で
ガラスを作る際に、ｐＨや温度を調節したり、溶融法で
ガラスの粘度や温度を調節してノズルから噴き飛ばした
り、あるいはガラスや原料を火炎、プラズマ炎、アーク
等高温帯を通過させるなどの手法により得られ、アスペ
クト比を変化させることもできる。The filler of the present invention is used in the powder or larger bulk obtained as described above, or as it is, or by adjusting the particle size and shape. Grinding, granulation, classification, etc. are performed before or after crystallization, or both, as necessary. In addition to the usual crushed shape, various particle shapes such as spherical, fibrous, and scaly shapes can be used. This is done by adjusting the pH and temperature when making glass using the sol-gel method, adjusting the viscosity and temperature of the glass using the melting method, and then blowing it out of the nozzle. It can be obtained by a method such as passing through a high temperature zone such as an arc, and the aspect ratio can also be changed.
これらの形状の粒子は、各々その目的によって使い分け
、もちろん混合して用いてもよい。すなわち、封止材と
してより高い流動性が特に樹脂組成物に求められている
場合には、長短径比の平均値が１〜１．５好ましくは１
〜１．４特に好ましくは１〜１．３である球状粉末を富
配合することが好ましく、また、リードピン曲げ時の樹
脂クランクを防止するために曲げ強度や曲げ弾性等の機
械的強度の高い樹脂組成物が必要な場合には、繊維状の
粉末を加えることが好ましく、さらには機械的強度と共
に耐湿信軌性を更に高めたい場合には、鱗片状の粉末の
併用することもできる。繊維状充填剤の直径は０．０１
〜１５μｍ好ましくは０．０５〜ｌＯμｍ特に好ましく
は０．１〜５μｍであり、長さは０．５〜５００μｍ好
ましくは１〜１５０μｍ特に好ましくは３〜７５μｍで
ある。鱗片状充填剤の厚みとしては０．０１〜１０μｍ
好ましくは０．０３〜５μｍ特に好ましくは０．０５〜
３μｍであり、アスペクト比は５以上好ましくは８以上
特に好ましくは１０以上である。Particles having these shapes can be used depending on their purpose, and of course, they may be used in combination. That is, when the resin composition is particularly required to have higher fluidity as a sealing material, the average value of the length/breadth axis ratio is 1 to 1.5, preferably 1.
~1.4 It is preferable to blend a rich amount of spherical powder, particularly preferably 1 to 1.3, and a resin with high mechanical strength such as bending strength and bending elasticity to prevent resin cranking when bending the lead pin. If the composition requires a fibrous powder, it is preferable to add a fibrous powder, and if it is desired to further improve the mechanical strength and moisture resistance, a scaly powder can also be used in combination. The diameter of the fibrous filler is 0.01
The length is preferably 0.05 to 10 μm, particularly preferably 0.1 to 5 μm, and the length is preferably 0.5 to 500 μm, preferably 1 to 150 μm, particularly preferably 3 to 75 μm. The thickness of the scale-like filler is 0.01 to 10 μm.
Preferably 0.03 to 5 μm, particularly preferably 0.05 to 5 μm
3 μm, and the aspect ratio is 5 or more, preferably 8 or more, particularly preferably 10 or more.
これらの繊維状及び鱗片状の粉末の充填剤中の割合は０
〜７０重量％好ましくは０〜５０重量％特に好ましくは
θ〜３０ｆｆｉ量％である。７０％を超えると素子表面
や素子保護膜を傷つけたり、ボンディングワイヤの変形
や切断をおこしたり、さらには成形異方性が大きくなっ
て局部的に大きな応力が発生したり、かえって耐熱衝撃
性や耐湿信輔性の低下、粒度分布の調整困難、流動性の
低下、成形時のパリの増加、気泡の巻き込みなどの欠点
があられれるようになる。The proportion of these fibrous and scaly powders in the filler is 0.
70% by weight, preferably 0 to 50% by weight, particularly preferably θ to 30% by weight. If it exceeds 70%, it may damage the element surface or element protective film, cause deformation or breakage of the bonding wire, or even increase molding anisotropy, causing large local stress, or even deteriorate thermal shock resistance. This leads to disadvantages such as a decrease in moisture resistance, difficulty in adjusting the particle size distribution, a decrease in fluidity, an increase in frustness during molding, and the inclusion of air bubbles.
本発明の充填剤は、金属酸化物７〜３０モル％、ＡＩ、
０，７〜３０モル％、５ｉＯｚ４０〜８６モル％を含む
熱膨張係数０． Ｉ Ｘ １０−”Ｋ’以下の物質を有
効成分として含有するものであり、金属酸化物としては
、ＭｇＯ、、ＺｎＯ、ＣｕｚＯ又はＣｕＯを好ましく挙
げることができるが、これらの金属酸化物は低熱膨張性
物質の生成に好適なばかりではなく、マグネシウムの含
有はイオン性不純物によるアルミニウム電極の腐蝕を防
止する効果をもたらし、また、亜鉛や銅の酸化物の含有
は高充填物の成形時に生じる金型摩耗の問題に効果があ
る。更に、これらを含ませることによって、充填剤の曲
げ弾性が増加するのでパッケージの薄型化による封止材
の曲げ強度増加の要求に対する改善効果をもたらす、又
、前述したように、結晶相の生成は高熱伝導化をもたら
すが、ＭｇＯ、ＺｎＯ、Ｃｕ、Ｏ又はＣｕＯを用いた場
合にはその効果が大きくなる。The filler of the present invention contains 7 to 30 mol% of metal oxides, AI,
Thermal expansion coefficient 0.7-30 mol%, containing 5iOz 40-86 mol%. Contains a substance of I In addition to being suitable for the production of chemical substances, the inclusion of magnesium has the effect of preventing corrosion of aluminum electrodes caused by ionic impurities, and the inclusion of zinc and copper oxides prevents molds that occur when molding highly filled materials. It is effective in solving the problem of wear.Furthermore, by including these fillers, the bending elasticity of the filler increases, which improves the demand for increasing the bending strength of the encapsulant due to the thinning of the package. As described above, the formation of a crystalline phase brings about higher thermal conductivity, but this effect becomes greater when MgO, ZnO, Cu, O, or CuO is used.
本発明の充填剤は、他の充填剤との併用も可能であるが
、その際に水溶性や著しい吸湿性を示すもの、アルカリ
や塩素、硫酸イオンをはじめとしたイオン性溶出物を生
じやすいもの、絶縁性の低いもの、樹脂中３００℃以下
で不安定なものなどは好ましくない、その他は特に限定
するものではなく要求される封止材の特性に応じて併用
すれば種々の効果をあげることができる。すなわち、よ
り高熱伝導化したい場合には、窒化珪素、窒化アルミニ
ウム、窒化ホウ素、サイアロン、シリコンオキシナイト
ライドなどをはじめとした高熱伝導性粉末と共に用いれ
ばよく、低熱膨張性が重要であれば、溶融シリカ、シリ
カ−チタニア、シリカ−ジルコニアガラスなどと併用す
る。又、現在入手の容易さやコストの点からしばしば用
いられている石英粉末充填剤などに加えることにより低
熱応力化改質剤としても用いることもできる。The filler of the present invention can be used in combination with other fillers, but in that case, they tend to be water-soluble, exhibit significant hygroscopicity, and tend to generate ionic eluates such as alkali, chlorine, and sulfate ions. Materials with low insulation properties, materials that are unstable in resin at temperatures below 300℃ are undesirable, and other materials are not particularly limited, and various effects can be achieved if used in combination depending on the required properties of the sealing material. be able to. In other words, if you want higher thermal conductivity, you can use it together with high thermal conductive powders such as silicon nitride, aluminum nitride, boron nitride, sialon, silicon oxynitride, etc. If low thermal expansion is important, you can use molten powder. Used in combination with silica, silica-titania, silica-zirconia glass, etc. It can also be used as a modifier for reducing thermal stress by adding it to quartz powder fillers, which are currently often used due to ease of availability and cost.
本発明の充填剤の最大粒径としては、小さいほど成形時
における素子表面の配線、パッツベーション膜、ボンデ
ィングワイヤ等に傷をつけたり破損をさせたりすること
が少なくなるが、トランスファー成形時のゲージ詰りを
考慮した最大粒径は、５００μｍ以下好ましくは１４９
μｍ以下特に好ましくは７４μｍ以下である。なお、グ
イボンディング接着用や１５４ ｆｆａ接着用には、４
４μｍ以下さらに必要により２０μｍ、以下とすること
により、平滑性と接着性を向上させた封止材とすること
ができる。The smaller the maximum particle size of the filler of the present invention, the less likely it is to damage or damage the wiring, passivation film, bonding wire, etc. on the surface of the element during molding, but it may cause gauge clogging during transfer molding. The maximum particle size considering this is 500 μm or less, preferably 149
It is preferably 74 μm or less, particularly preferably 74 μm or less. In addition, for Gui bonding adhesive and 154 ffa adhesive, 4
By setting the thickness to 4 μm or less, and further to 20 μm or less if necessary, a sealing material with improved smoothness and adhesiveness can be obtained.
また、本発明の充填剤の平均粒径としては、０．３〜１
００μｍ好ましくは１〜７０μｍさらに好ましくは３〜
５０μｍであり、また、粒度分布としては、ボールミル
、振動ミル、アトライター。Further, the average particle size of the filler of the present invention is 0.3 to 1
00 μm, preferably 1 to 70 μm, more preferably 3 to 70 μm
50μm, and the particle size distribution is ball mill, vibration mill, attritor.
ローラーミル、ジェットミル、ロールクラッシャー等に
よる粉砕品をそのまま篩で粗粒子を除去したり必要に応
じて分級したものでもよいが、好ましくは、ＲＲ３粒度
線図において最大粒径からの累積重量％の１θ〜３０重
量％の１点と７０〜９０重量％の１点とを結んだ直線の
勾配力筒、１以下特に好ましくは０．９５以下である。The product crushed by a roller mill, jet mill, roll crusher, etc. may be directly sieved to remove coarse particles or classified as necessary, but preferably, the cumulative weight percentage from the maximum particle size in the RR3 particle size diagram is The slope of the straight line connecting one point of 1θ to 30% by weight and one point of 70 to 90% by weight is 1 or less, particularly preferably 0.95 or less.
勾配力筒、１以下特に０．９５以下であると、成形時の
パリの発生が少ないのでパリ取り工程の自動化が容易と
なる。When the gradient force is 1 or less, especially 0.95 or less, there is little occurrence of burrs during molding, making it easy to automate the burr removal process.
さらには、流動性が良好でかつ成形物への気泡の巻きこ
みも少ないため、充填剤をより高充填することにより、
−段と熱伝導性、耐熱衝撃性及び耐湿信頼性を高めるこ
とができ、しかもピンホール等に起因する電気絶縁不良
等を抑制することができる。Furthermore, since it has good fluidity and less air bubbles are trapped in the molded product, by filling it with a higher filler,
- It is possible to significantly improve thermal conductivity, thermal shock resistance, and moisture resistance reliability, and to suppress electrical insulation defects caused by pinholes and the like.
ここでＲＲ３粒度線図とは、Ｒｏｓｉｎ−Ｒａｍｍｌｅ
ｒの次式に従う粒度分布を表わす粒度線図のことである
。Here, the RR3 particle size diagram is Rosin-Rammle
This is a particle size diagram showing the particle size distribution of r according to the following equation.
Ｒ（Ｄｐ） ＝１００ｅｘｐ（−ｂ Ｄｐ’）（但し、
式中Ｒ（Ｄｐ）は最大粒径から粒径Ｄｐまでの累積重量
％、ｈは粒径、ｂ及びｎは定数である）ＲＲ３粒度線図
における勾配とは、ＲＲ３粒度線図の最大粒径からの累
積重量％が１０〜３０重量％の１点と７０〜９０重璽％
の１点とを結んだ直線で代表されるＲｏｓｉｎ−Ｒａｍ
ｍｌｅｒの式のｎ値のことをいう。なお、実際の粒度測
定において、最大粒径からの累積重量％の１０〜３０重
景％の範囲の１点と７０〜９０重量％の範囲の１点を結
ぶ直線が２本以上引き得る場合には、これらの直線のう
ちで最小の勾配で代表させることとする。R(Dp) = 100exp(-b Dp') (However,
(In the formula, R(Dp) is the cumulative weight percent from the maximum particle size to the particle size Dp, h is the particle size, and b and n are constants.) The slope in the RR3 particle size diagram is the maximum particle size in the RR3 particle size diagram. 1 point with a cumulative weight% of 10-30% and 70-90%
Rosin-Ram represented by a straight line connecting one point of
It refers to the n value in the mler formula. In addition, in actual particle size measurement, if two or more straight lines can be drawn connecting one point in the range of 10 to 30 weight percent and one point in the range of 70 to 90 weight percent of the cumulative weight percent from the maximum particle size. is represented by the minimum slope among these straight lines.
さらに、本発明の充填剤の比表面積としては、１５ｒｄ
／ｇ以下であればよいが好ましくは７４７ｇ以下特に５
ｒｒｒ／ｇ以下である。１５ｒｒｆ／ｇを越えると、充
填剤が嵩ぼるため充填剤の混合に長時間を要し樹脂が硬
化して成形性が低下するか、または高充填することがで
きなくなって熱伝専性や耐熱衝撃性が低下する。Furthermore, the specific surface area of the filler of the present invention is 15rd
/g or less, but preferably 747g or less, especially 5
rrr/g or less. If it exceeds 15rrf/g, the filler will become bulky and it will take a long time to mix the filler, and the resin will harden, resulting in poor moldability, or it will not be possible to fill it to a high degree, resulting in poor heat transfer properties and heat resistance. Impact resistance decreases.
本発明の充填剤に含まれるイオン性不純物としては、Ｆ
ｅ” ５０００ ｐｐｍ以下、Ｎａ” 、Ｌｉ” 、Ｋ
”等のアルカリ金属の合計量１００ｐｐｎ＋以下、ＣＣ
１−５０ｐｐ以下であり、好ましくはＦｅ”１０００ｐ
ｐｍ以下、アルカリ金属の合計ｉ３０ｐｐｍ以下、ｃｘ
−２０ｐｐｎ＋以下、特に好ましくはＦｅ” １００ｐ
ｐｍ以下、アルカリ金属の合計量１０ｐｐｍ以下、Ｃ１
−ｔｏｐｐｍ以下である。特にＮａ”が１１００ｐｐを
越えたりＣｊｌｌ−が５０ｐｐｍを越えたりすると耐湿
信頼性が劣る。The ionic impurities contained in the filler of the present invention include F
e" 5000 ppm or less, Na", Li", K
”Total amount of alkali metals such as 100ppn+ or less, CC
1-50pp or less, preferably Fe”1000p
pm or less, total alkali metal i30ppm or less, cx
−20ppn+ or less, particularly preferably Fe” 100p
pm or less, total amount of alkali metals 10 ppm or less, C1
−toppm or less. In particular, if Na'' exceeds 1100 ppm or Cjll- exceeds 50 ppm, the moisture resistance reliability will be poor.
本発明の充填剤の樹脂組成物中の含有率は、２６〜９７
重量％好ましくは３０〜９５重量％特に好ましくは４０
〜９０重量％である。樹脂充填剤の含有率が２０重量％
未満であると、樹脂組成物の成形性は優れるが、熱応力
が大きく耐熱衝撃性や耐湿信頼性が低下する。一方、９
７重量％を越えると、樹脂組成物の成形性、及び／又は
硬化特性が低下する。The content of the filler of the present invention in the resin composition is 26 to 97
% by weight, preferably 30-95% by weight, particularly preferably 40% by weight
~90% by weight. Resin filler content is 20% by weight
If it is less than 1, the moldability of the resin composition is excellent, but thermal stress is large and thermal shock resistance and moisture resistance reliability are reduced. On the other hand, 9
If it exceeds 7% by weight, the moldability and/or curing properties of the resin composition will deteriorate.
本発明の充填剤が使用される樹脂としては、ビスフェノ
ール型エポキシ樹脂、フェノールノボラック型エポキシ
樹脂、脂環型エポキシ樹脂、複素環型エポキシ樹脂、グ
リシジルエステル型エポキシ樹脂、グリシジルアミン型
エポキシ樹脂、ハロゲン化エポキシ樹脂などのエポキシ
樹脂、シリコン樹脂、フェノール樹脂、メラミン樹脂、
ユリア樹脂、不飽和ポリエステル、ポリアミノビスマレ
イミド、ジアリルフタレート樹脂、フッ素樹脂、ＴＰＸ
樹脂（メチルペンテンポリマー「三菱瓦斯化学社製商品
名」）、ポリイミド、ポリアミドイミド、ポリエーテル
イミド、６ローナイロン及びＭＸＤ−ナイロン等のポリ
アミド、ポリブチレンテレフタレート及びポリエチレン
テレフタレート等のポリエステル、ポリフェニレンスル
フィド、ポリフェニレンエーテルボリアリレート、全芳
香族ポリエステル、ポリスルホン、液晶ポリマー、ポリ
エーテルエーテルケトン、ポリエーテルスルホン、ポリ
カーボネート、マレイミド変性樹脂、ＡＢＳ樹脂、ＡＡ
Ｓ （アクリロニトリル・アクリルゴム・スチレン）樹
脂、ＡＥＳ （アクリロニトリル−エチレン・プロピレ
ン・ジエンゴム−スチレン）樹脂等が挙げられるが、特
にエポキシ樹脂、ＢＴ樹脂（三菱瓦斯化学社製商品名）
等のポリアミノビスマレミド、ポリフェニレンスルフィ
ド等が好ましい。熱衝撃性を高めるために、ブチルゴム
、アクリルゴム、エチレンプロピレンゴム、シリコーン
ゴム、ポリエステルエラストマー、ポリブタジェン等の
ゴム成分をこれら樹脂中に含有させることもできる。The resins to which the filler of the present invention can be used include bisphenol-type epoxy resins, phenol novolak-type epoxy resins, alicyclic-type epoxy resins, heterocyclic-type epoxy resins, glycidyl ester-type epoxy resins, glycidylamine-type epoxy resins, and halogenated epoxy resins. Epoxy resin such as epoxy resin, silicone resin, phenolic resin, melamine resin,
Urea resin, unsaturated polyester, polyamino bismaleimide, diallyl phthalate resin, fluororesin, TPX
Resin (methylpentene polymer "trade name manufactured by Mitsubishi Gas Chemical Co., Ltd."), polyimide, polyamideimide, polyetherimide, polyamide such as 6-row nylon and MXD-nylon, polyester such as polybutylene terephthalate and polyethylene terephthalate, polyphenylene sulfide, polyphenylene Ether polyarylate, fully aromatic polyester, polysulfone, liquid crystal polymer, polyether ether ketone, polyether sulfone, polycarbonate, maleimide modified resin, ABS resin, AA
S (acrylonitrile/acrylic rubber/styrene) resin, AES (acrylonitrile-ethylene/propylene/diene rubber-styrene) resin, etc., but especially epoxy resin, BT resin (trade name manufactured by Mitsubishi Gas Chemical Co., Ltd.)
Preferred are polyamino bismalemide, polyphenylene sulfide, etc. In order to improve thermal shock resistance, rubber components such as butyl rubber, acrylic rubber, ethylene propylene rubber, silicone rubber, polyester elastomer, polybutadiene, etc. can also be included in these resins.
本発明の充填剤を使用した樹脂組成物には、必要に応じ
て、２．４−ジヒドラジン−６−メチルアミノ−ｓ−）
リアジン、２−メチルイミダゾール、２−エチル−４−
メチルイミダゾール、１−シアノエチル−２−エチル−
４−メチルイミダゾール等のイミダゾール誘導体、弗化
ホウ素の各種アミン錯体、トリスジメチルアミノメチル
フェノール、１．８−ジアザ・ビシクロ（５，４，０）
−ウンデセン−７、ベンジルジメチルアミン等の第３級
アミン化合物、ジシアンジアミド、アジピン酸ヒドラジ
ド等の含窒素硬化（促進）剤、フェノールノボラック、
タレゾールノボランク等のフェノール系硬化剤、無水テ
トラヒドロフタル酸。In the resin composition using the filler of the present invention, if necessary, 2,4-dihydrazine-6-methylamino-s-)
riazine, 2-methylimidazole, 2-ethyl-4-
Methylimidazole, 1-cyanoethyl-2-ethyl-
Imidazole derivatives such as 4-methylimidazole, various amine complexes of boron fluoride, trisdimethylaminomethylphenol, 1,8-diaza bicyclo(5,4,0)
-Undecene-7, tertiary amine compounds such as benzyldimethylamine, nitrogen-containing curing (accelerator) agents such as dicyandiamide and adipic acid hydrazide, phenol novolak,
Phenolic curing agents such as Talesol Novolanc, tetrahydrophthalic anhydride.
無水へキサヒドロフタル酸、無水メチルへキサヒドロフ
タル酸等の酸無水物系硬化剤、トリフェニルホスフィン
、トリシクロヘキシルホスフィン。Acid anhydride curing agents such as hexahydrophthalic anhydride and methylhexahydrophthalic anhydride, triphenylphosphine, tricyclohexylphosphine.
メチルジフェニルホスフィン、トリトリルホスフィン、
１．２−ビス（ジフェニルホスフィノ）エタン、ビス（
ジフェニルホスフィノ）メタン等の有機ホスフィン系硬
化（促進）剤、白金化合物等の重合触媒、カルナウバワ
ックス、モンタナワックス、ポリエステルオリゴマー、
シ１ノコン油、低分子量ポリエチレン、パラフィン、直
鎖脂肪酸の金属塩、酸アミド、エステル等の滑剤・離型
剤、２．６−ジーｔ−ブチル−４−メチルフェノール。Methyldiphenylphosphine, tritolylphosphine,
1.2-Bis(diphenylphosphino)ethane, bis(
Organic phosphine curing (accelerator) agents such as diphenylphosphino)methane, polymerization catalysts such as platinum compounds, carnauba wax, montana wax, polyester oligomers,
Silk oil, low molecular weight polyethylene, paraffin, metal salts of straight chain fatty acids, lubricants and mold release agents such as acid amides and esters, 2,6-di-t-butyl-4-methylphenol.
１．３．５−１−リス（２−メチル−４−ヒドロキシ−
５−ｔ−ブチルフェノール）ブタン、ジステアリルチオ
ジプロピオネート、トリノニルフェニルホスファイト
トリデシルホスファイト等の安定剤、２．２′−ジヒド
ロキシ−４−メトキシベゾフェノン、２（２’−ヒドロ
キシ−５−メチルフェニル）ベンゾトリアゾール、４−
ｔ−ブチルフェニルサリチレート、エチル−２−シアノ
−３゜３−ジフェニルアクリレート等の光安定剤、ベン
ガラ、カーボンブランク等の着色剤、三酸化アンチモン
、四酸化アンチモン、トリフェニルスチピン、水和アル
ミナ、フェロセン、ホスファゼン。1.3.5-1-Lis(2-methyl-4-hydroxy-
5-tert-butylphenol)butane, distearylthiodipropionate, trinonylphenyl phosphite
Stabilizers such as tridecyl phosphite, 2,2'-dihydroxy-4-methoxybezophenone, 2(2'-hydroxy-5-methylphenyl)benzotriazole, 4-
Light stabilizers such as t-butylphenyl salicylate, ethyl-2-cyano-3゜3-diphenylacrylate, colorants such as red iron, carbon blank, antimony trioxide, antimony tetroxide, triphenylstipine, hydrated Alumina, ferrocene, phosphazene.
ヘキサブロモベンゼン、テトラブロモフタル酸無水物、
トリクレジルホスフェート、テトラブロモビスフェノー
ルＡ、臭素化エポキシ誘４体等の難燃剤、ビニルトリメ
トキシシラン、γ−グリシドキシプロピルトリメトキシ
シラン、γ−ウレイドプロピルトリエトキシシラン、Ｎ
−β−（アミノエチル）−γ−アミノプロピルトリメト
キシシラン、β−（３，４−エポキシシクロヘキシル）
エチルトリメトキシシラン等のシラン系カップリング剤
、イソプロピルトリイソステアロイルチタネート、ジク
ミルフェニルオキシアセテートチタネート ビス（ジオ
クチルパイロホスフェート）オキシアセテートチタネー
ト、イソプロピルトリデシルベンゼンスルホニルチタネ
ート等のチタン系カップリング剤、アセトアルコキシア
ルミニウムジイソプロピレート等のアルミ系カップリン
グ剤等を配合することができる。なお、カップリング剤
はインテグラルブレンドでもよいが、前もって本発明の
充填剤と混合・熱処理しておいた方が耐湿信頼性が向上
する。hexabromobenzene, tetrabromophthalic anhydride,
Flame retardants such as tricresyl phosphate, tetrabromobisphenol A, brominated epoxy derivatives, vinyltrimethoxysilane, γ-glycidoxypropyltrimethoxysilane, γ-ureidopropyltriethoxysilane, N
-β-(aminoethyl)-γ-aminopropyltrimethoxysilane, β-(3,4-epoxycyclohexyl)
Silane coupling agents such as ethyltrimethoxysilane, titanium coupling agents such as isopropyltriisostearoyl titanate, dicumylphenyloxyacetate titanate, bis(dioctylpyrophosphate)oxyacetate titanate, isopropyltridecylbenzenesulfonyl titanate, acetalkoxy Aluminum coupling agents such as aluminum diisopropylate and the like can be blended. Although the coupling agent may be an integral blend, moisture resistance reliability is improved if it is mixed with the filler of the present invention and heat-treated in advance.
本発明の充填剤を含有する樹脂組成物は、前記に示した
各成分の所定量をヘンシェルミキサー等により充分混合
後、ロール、バンバリーミキサ−。The filler-containing resin composition of the present invention is prepared by thoroughly mixing predetermined amounts of each of the above-mentioned components using a Henschel mixer or the like, and then using a roll or Banbury mixer.
ニーグー、らいかい機、アジホモミキサー、２軸押用機
、ｌ軸押出機等の混練手段により加熱混練して製造する
ことができる。It can be produced by heating and kneading using a kneading means such as a Nigu, a rice cracker, an Ajihomo mixer, a twin-screw extruder, and a l-screw extruder.
本発明を実施例により具体的に説明するが、本発明は以
下の実施例に限定されるものではない。EXAMPLES The present invention will be specifically explained with reference to Examples, but the present invention is not limited to the following Examples.
まず充填剤を以下のようにして調整した。原料は高純度
試薬（いずれも９９．９％以上）を用いた。First, the filler was prepared as follows. High purity reagents (all 99.9% or higher) were used as raw materials.
ただしＬｉｚＯはＬｉｚＣＯ，を用いた。組成は表−１
の６組成（モル％）である（ＬｉｚＯはＬｉ２Ｃ０，３
を換算）。However, LizCO was used as LizO. The composition is shown in Table 1.
(LizO is Li2C0,3
(converted).
いずれもよく混合した後白金坩堝に入れて電気炉を用い
て１．６００℃で２時間（ｈ）加熱溶融し、取り出して
溶融物を流し出して急冷し、徐冷炉で６５０°Ｃから室
温まで放冷してガラスを得た。また、ガラスＥは１０５
μｍ全通までボールミルで粉砕後、酸素−水素バーナー
中を通過させて球状のガラス粉Ｇを得た。After mixing them well, they were placed in a platinum crucible, heated and melted at 1.600°C for 2 hours (h) using an electric furnace, taken out, poured out and rapidly cooled, and left in a slow cooling furnace from 650°C to room temperature. After cooling, a glass was obtained. Also, glass E is 105
After pulverizing in a ball mill to a full μm diameter, the glass powder G was passed through an oxygen-hydrogen burner to obtain a spherical glass powder G.
次に、ガラスＡ−Ｇを電気炉を用いて表−２の条件で熱
処理し、１０５μｍ全通まで粉砕して充填剤ｌ〜８を得
た、組成はいずれも原料組成とほぼ同じであることが確
認された。Next, Glasses A-G were heat-treated using an electric furnace under the conditions shown in Table 2, and crushed to a diameter of 105 μm to obtain fillers 1 to 8, all of which had the same composition as the raw material. was confirmed.
この充填剤１〜８を用いて以下封止材を作製した。すな
わち、重量で、タレゾールノボラックエポキシ樹脂（エ
ポキシ当１２１５）１５０部、臭素化タレゾールノボラ
ックエポキシ樹脂（エポキシ当９３５０）４５部、フェ
ノールノボラック樹脂（フェノール当量１０７）８７部
から成る樹脂組成物に１〜８の充填剤（表−４に示す割
合）、三酸化アンチモン５．６部、カーボンブラック３
部、カルナバワックス４．４部、及び硬化促進剤として
２−フェニル−４−メチル−５−ヒドロキシメチルイミ
ダゾール２．５部、γ−グリシドキシプロピルトリメト
キシシラン５部、をミキシングロールで混練後、粉砕し
て封止材とした。これらの樹脂組成物を次に示す評価試
験を実施した。The following sealing materials were produced using these fillers 1 to 8. That is, in a resin composition consisting of 150 parts of Talesol novolac epoxy resin (1215 parts per epoxy), 45 parts of brominated Talesol novolac epoxy resin (9350 parts per epoxy), and 87 parts of phenol novolac resin (107 parts per epoxy) by weight, 1. ~8 filler (proportion shown in Table 4), antimony trioxide 5.6 parts, carbon black 3
After kneading with a mixing roll, 4.4 parts of carnauba wax, 2.5 parts of 2-phenyl-4-methyl-5-hydroxymethylimidazole as a curing accelerator, and 5 parts of γ-glycidoxypropyltrimethoxysilane. , was crushed and used as a sealing material. These resin compositions were subjected to the following evaluation tests.
（１） 平均粒径
レーザー回折式法による粒度測定（シーラス社製Ｇｒｏ
ｎｕｌｏｍｅｔｅｒモデル７１５型）。(1) Average particle size Particle size measurement using laser diffraction method (Gro manufactured by Cirrus)
nulometer model 715).
（２） 比表面積
カンタソープを使用し、ＢＥＴＩ点法で測定（カンター
タロム社製比表面積測定ａ）。(2) Specific surface area Measured by the BETI point method using Canthathorp (Specific Surface Area Measurement a manufactured by Cantatarom).
（３１Ｌｉ” 、Ｎａ” 、Ｋ”不純物粉末の一定量を
純水中に浸漬し１００℃の温度で２４Ｈｒ放置した際に
水中に抽出されたＬｉ”、Ｎａ” 、Ｋ”を原子吸光法
にて測定。(31 Li", Na", K" extracted into water when a certain amount of Li", Na", K" impurity powder was immersed in pure water and left at a temperature of 100°C for 24 hours was analyzed using atomic absorption method. measurement.
（４）流動性（スパイラルフロー）
ＥＭＭＩ規格に準じた金型を使用し成形温度１７０℃、
成形圧カフ０ｋｇ／ｃｆｆｌで測定した。この値は大き
いほど成形性が優れていることを示すものである。(4) Fluidity (spiral flow) Using a mold that complies with EMMI standards, the molding temperature is 170℃,
Measurement was made with a molding pressure cuff of 0 kg/cffl. The larger this value is, the better the moldability is.
（５） パリ
２．５．１０，３０ｃｒｍの所定厚みのスリットを持つ
金型を用い成形温度１７０℃、成形圧カフ０ｋｇ／ａｊ
で流動長を測定し、その最大値を示した。(5) Using a mold with a slit of a predetermined thickness of Paris 2.5.10.30 crm, the molding temperature is 170°C, and the molding pressure is 0 kg/aj.
The flow length was measured and its maximum value is shown.
（６） 耐熱衝撃性（耐Ｔ／Ｓ性）
アイランドサイズ４ Ｘ ７．５ ｎの１６とンリード
フレームを各組成物によりトランスファー成形し、その
１６ピンＤＩＰ型成形体を一１９６℃の液体と２６０℃
の液体に３０秒ずつ浸漬を２００回繰り返し、２５個以
上の成形体表面にクランクが発生するまでの回数を求め
た。試料価数は５０個である。(6) Thermal Shock Resistance (T/S Resistance) A 16-pin lead frame with an island size of 4 x 7.5 n was transfer molded using each composition, and the 16-pin DIP molded product was heated with a liquid at -196°C. 260℃
The immersion was repeated 200 times for 30 seconds each in the liquid, and the number of times until cranking occurred on the surface of 25 or more molded objects was determined. The number of samples is 50.
（７）耐湿信頼性
アルミニウム配線を有する１６ピンモニターＩＣをトラ
ンスファー成形し硬化後２６０℃のハンダ浴に１０秒間
浸漬したのち１２０℃、２気圧の水蒸気中でＩＯＶ印加
してアルミニウム配線のオープン不良率（断線率）とリ
ーク不良率（アルミニウム線間の漏れ電流値が１ｏｎＡ
以上になった率）との和が５０％以上になるまでの時間
を求めた。試料価数は２０個である。(7) Moisture-resistant reliability A 16-pin monitor IC with aluminum wiring was transfer-molded, and after curing, it was immersed in a solder bath at 260°C for 10 seconds, and then IOV was applied in water vapor at 120°C and 2 atm to open failure rate of the aluminum wiring. (wire breakage rate) and leak defect rate (leakage current value between aluminum wires is 1 onA)
The time required for the sum to reach 50% or more was calculated. The number of samples is 20.
（８）熱伝導率
熱伝導率測定装置（アグネ社製ｒＡＲＣ−ＴＣ−１型」
）を用い、室温において温度傾斜法で測定した。(8) Thermal conductivity Thermal conductivity measuring device (Agne rARC-TC-1 type)
) was measured by the temperature gradient method at room temperature.
（９） 生°成相
ＮｉフィルターＣｕＫＯ線を用いた粉末Ｘ線回折法によ
って、２θでｌＯから５０’の回折線図形から生成の同
定を行なった。(9) Formation phase Formation was identified from the diffraction line pattern at 50' from 1O at 2θ by powder X-ray diffraction using Ni filter CuKO radiation.
表−３に示す如く、本発明の充填剤ａ ｗ ｆと比較例
ｇ −、−ｉの充填剤を用いて、表−４の（イ）〜（ヲ
）の１２種の封止材を作製した結果、本発明品は、従来
の封止材（ヌ）に比べて高い耐Ｔ／Ｓ性を示し、耐湿信
頼性はほぼ同等の値を示すことがわかる。As shown in Table 3, 12 types of sealing materials (A) to (W) in Table 4 were prepared using the filler aw f of the present invention and the fillers of Comparative Examples g- and -i. As a result, it can be seen that the product of the present invention exhibits higher T/S resistance than the conventional sealing material (N), and exhibits almost the same moisture resistance reliability.
これに対し、比較例（ル）は熱伝導率は改善されている
ものの耐Ｔ／Ｓ性に劣り封止材としての使用は難しい。On the other hand, although Comparative Example (R) has improved thermal conductivity, it has poor T/S resistance and is difficult to use as a sealing material.
さらに比較例（ヲ）はアルカリを多量に含有する充填剤
（１）を用いたため耐湿信頼性に著しく劣っている。Furthermore, Comparative Example (2) used filler (1) containing a large amount of alkali, and therefore was significantly inferior in moisture resistance reliability.
本発明の実施例（イ）〜（す）は熱伝導率でも従来技術
（ヌ）に比べ改善されており、ハイブリッドＩＣやパワ
ーＩＣなどの高集積度化に対して十分に対応できること
が示された。Examples (A) to (S) of the present invention have improved thermal conductivity compared to the conventional technology (N), and are shown to be fully compatible with higher integration such as hybrid ICs and power ICs. Ta.
表−１ （注）ＧとＥは球状品である。Table-1 (Note) G and E are spherical products.
本発明の充填剤を使用した封止材は、耐熱衝撃性と高熱
伝導性に優れ、半田浸漬後の耐湿信鎖性も十分に確保さ
れたものとなる。The sealing material using the filler of the present invention has excellent thermal shock resistance and high thermal conductivity, and has sufficient moisture resistance after solder immersion.
特許出願人 電気化学工業株式会社Patent applicant: Denki Kagaku Kogyo Co., Ltd.
Claims (1)
属酸化物７〜３０モル％、アルミナ７〜３０モル％及び
シリカ４０〜８６モル％を含む熱膨張係数０．１×１０
＾−＾６Ｋ＾−＾１以下の物質を有効成分として含有し
て成ることを特徴とする半導体封止材用充填剤。 ２）アルミニウム、シリコン及びアルカリ金属以外の金
属酸化物がマグネシウム、亜鉛及び／又は銅の酸化物で
あることを特徴とする特許請求の範囲第１項記載の半導
体封止用充填剤。[Claims] 1) A thermal expansion coefficient of 0.1 x 10 containing 7 to 30 mol% of metal oxides other than aluminum, silicon and alkali metals, 7 to 30 mol% of alumina, and 40 to 86 mol% of silica.
A filler for a semiconductor encapsulant, characterized by containing a substance of ^-^6K^-^1 or less as an active ingredient. 2) The filler for semiconductor encapsulation according to claim 1, wherein the metal oxide other than aluminum, silicon, and alkali metal is an oxide of magnesium, zinc, and/or copper.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32963687A JPH01172433A (en) | 1987-12-28 | 1987-12-28 | Filler for semiconductor sealing material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32963687A JPH01172433A (en) | 1987-12-28 | 1987-12-28 | Filler for semiconductor sealing material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01172433A true JPH01172433A (en) | 1989-07-07 |
Family
ID=18223555
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32963687A Pending JPH01172433A (en) | 1987-12-28 | 1987-12-28 | Filler for semiconductor sealing material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01172433A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019052051A (en) * | 2017-09-13 | 2019-04-04 | デンカ株式会社 | Spherical silica powder for filler and manufacturing method thereof |
-
1987
- 1987-12-28 JP JP32963687A patent/JPH01172433A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019052051A (en) * | 2017-09-13 | 2019-04-04 | デンカ株式会社 | Spherical silica powder for filler and manufacturing method thereof |
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