JP7386755B2 - thermal conductive sheet - Google Patents
thermal conductive sheet Download PDFInfo
- Publication number
- JP7386755B2 JP7386755B2 JP2020084645A JP2020084645A JP7386755B2 JP 7386755 B2 JP7386755 B2 JP 7386755B2 JP 2020084645 A JP2020084645 A JP 2020084645A JP 2020084645 A JP2020084645 A JP 2020084645A JP 7386755 B2 JP7386755 B2 JP 7386755B2
- Authority
- JP
- Japan
- Prior art keywords
- thermally conductive
- conductive sheet
- volume
- zinc oxide
- meth
- 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.)
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 130
- 239000011787 zinc oxide Substances 0.000 claims description 75
- 239000011231 conductive filler Substances 0.000 claims description 51
- -1 phosphate ester compound Chemical class 0.000 claims description 45
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 41
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 30
- 239000003522 acrylic cement Substances 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 22
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 17
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 16
- 229910019142 PO4 Inorganic materials 0.000 claims description 15
- 230000002378 acidificating effect Effects 0.000 claims description 15
- 239000010452 phosphate Substances 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- 125000000217 alkyl group Chemical group 0.000 claims description 10
- 125000003342 alkenyl group Chemical group 0.000 claims description 2
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 78
- 235000014692 zinc oxide Nutrition 0.000 description 72
- 239000011248 coating agent Substances 0.000 description 58
- 238000000576 coating method Methods 0.000 description 58
- 239000007788 liquid Substances 0.000 description 54
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 42
- 230000001070 adhesive effect Effects 0.000 description 30
- 239000000853 adhesive Substances 0.000 description 29
- 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 28
- 238000002360 preparation method Methods 0.000 description 26
- 239000000178 monomer Substances 0.000 description 23
- 238000000034 method Methods 0.000 description 13
- 239000003431 cross linking reagent Substances 0.000 description 12
- 239000006087 Silane Coupling Agent Substances 0.000 description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 11
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 10
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 10
- 239000004014 plasticizer Substances 0.000 description 10
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 10
- 239000000126 substance Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 150000003505 terpenes Chemical class 0.000 description 7
- 235000007586 terpenes Nutrition 0.000 description 7
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 6
- 150000002148 esters Chemical class 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 229910052582 BN Inorganic materials 0.000 description 5
- 239000004593 Epoxy Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 5
- 229920006243 acrylic copolymer Polymers 0.000 description 5
- 239000012948 isocyanate Substances 0.000 description 5
- 150000002513 isocyanates Chemical class 0.000 description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000011256 inorganic filler Substances 0.000 description 4
- 229910003475 inorganic filler Inorganic materials 0.000 description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- JQCXWCOOWVGKMT-UHFFFAOYSA-N diheptyl phthalate Chemical compound CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC JQCXWCOOWVGKMT-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 2
- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 description 2
- 239000004971 Cross linker Substances 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Chemical compound CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000010335 hydrothermal treatment Methods 0.000 description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
- 239000001095 magnesium carbonate Substances 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 239000010450 olivine Substances 0.000 description 2
- 229910052609 olivine Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 229920001690 polydopamine Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 230000000379 polymerizing effect Effects 0.000 description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- OZFIGURLAJSLIR-UHFFFAOYSA-N 1-ethenyl-2h-pyridine Chemical compound C=CN1CC=CC=C1 OZFIGURLAJSLIR-UHFFFAOYSA-N 0.000 description 1
- LNKDTZRRFHHCCV-UHFFFAOYSA-N 1-ethenyl-2h-pyrimidine Chemical compound C=CN1CN=CC=C1 LNKDTZRRFHHCCV-UHFFFAOYSA-N 0.000 description 1
- OSSNTDFYBPYIEC-UHFFFAOYSA-N 1-ethenylimidazole Chemical compound C=CN1C=CN=C1 OSSNTDFYBPYIEC-UHFFFAOYSA-N 0.000 description 1
- DCRYNQTXGUTACA-UHFFFAOYSA-N 1-ethenylpiperazine Chemical compound C=CN1CCNCC1 DCRYNQTXGUTACA-UHFFFAOYSA-N 0.000 description 1
- PBGPBHYPCGDFEZ-UHFFFAOYSA-N 1-ethenylpiperidin-2-one Chemical compound C=CN1CCCCC1=O PBGPBHYPCGDFEZ-UHFFFAOYSA-N 0.000 description 1
- CTXUTPWZJZHRJC-UHFFFAOYSA-N 1-ethenylpyrrole Chemical compound C=CN1C=CC=C1 CTXUTPWZJZHRJC-UHFFFAOYSA-N 0.000 description 1
- XLPJNCYCZORXHG-UHFFFAOYSA-N 1-morpholin-4-ylprop-2-en-1-one Chemical compound C=CC(=O)N1CCOCC1 XLPJNCYCZORXHG-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 1
- LJKDOMVGKKPJBH-UHFFFAOYSA-N 2-ethylhexyl dihydrogen phosphate Chemical compound CCCCC(CC)COP(O)(O)=O LJKDOMVGKKPJBH-UHFFFAOYSA-N 0.000 description 1
- DPNXHTDWGGVXID-UHFFFAOYSA-N 2-isocyanatoethyl prop-2-enoate Chemical compound C=CC(=O)OCCN=C=O DPNXHTDWGGVXID-UHFFFAOYSA-N 0.000 description 1
- 125000004200 2-methoxyethyl group Chemical group [H]C([H])([H])OC([H])([H])C([H])([H])* 0.000 description 1
- SVBLDLLXNRGMBG-UHFFFAOYSA-N 2-methylpropyl dihydrogen phosphate Chemical compound CC(C)COP(O)(O)=O SVBLDLLXNRGMBG-UHFFFAOYSA-N 0.000 description 1
- VXRAAUKUZQYZRW-UHFFFAOYSA-N 3'-N'-Acetylfusarochromanone Chemical compound O1C(C)(C)CC(=O)C2=C(N)C(C(=O)CC(CO)NC(=O)C)=CC=C21 VXRAAUKUZQYZRW-UHFFFAOYSA-N 0.000 description 1
- ALKCLFLTXBBMMP-UHFFFAOYSA-N 3,7-dimethylocta-1,6-dien-3-yl hexanoate Chemical compound CCCCCC(=O)OC(C)(C=C)CCC=C(C)C ALKCLFLTXBBMMP-UHFFFAOYSA-N 0.000 description 1
- ZWDBXSPOFPFDFZ-UHFFFAOYSA-N 3-(1-phenylpentoxycarbonyl)benzoic acid Chemical compound CCCCC(OC(=O)c1cccc(c1)C(O)=O)c1ccccc1 ZWDBXSPOFPFDFZ-UHFFFAOYSA-N 0.000 description 1
- UJTRCPVECIHPBG-UHFFFAOYSA-N 3-cyclohexylpyrrole-2,5-dione Chemical compound O=C1NC(=O)C(C2CCCCC2)=C1 UJTRCPVECIHPBG-UHFFFAOYSA-N 0.000 description 1
- NIAXWFTYAJQENP-UHFFFAOYSA-N 3-ethenyl-2h-1,3-oxazole Chemical compound C=CN1COC=C1 NIAXWFTYAJQENP-UHFFFAOYSA-N 0.000 description 1
- QOXOZONBQWIKDA-UHFFFAOYSA-N 3-hydroxypropyl Chemical group [CH2]CCO QOXOZONBQWIKDA-UHFFFAOYSA-N 0.000 description 1
- SSMDYRHBKZVGNR-UHFFFAOYSA-N 3-propan-2-ylpyrrole-2,5-dione Chemical compound CC(C)C1=CC(=O)NC1=O SSMDYRHBKZVGNR-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- DBATVPMIFJTVOQ-UHFFFAOYSA-N 4-(1-phenylpentoxycarbonyl)benzoic acid Chemical compound C=1C=CC=CC=1C(CCCC)OC(=O)C1=CC=C(C(O)=O)C=C1 DBATVPMIFJTVOQ-UHFFFAOYSA-N 0.000 description 1
- SXIFAEWFOJETOA-UHFFFAOYSA-N 4-hydroxy-butyl Chemical group [CH2]CCCO SXIFAEWFOJETOA-UHFFFAOYSA-N 0.000 description 1
- PRKPGWQEKNEVEU-UHFFFAOYSA-N 4-methyl-n-(3-triethoxysilylpropyl)pentan-2-imine Chemical compound CCO[Si](OCC)(OCC)CCCN=C(C)CC(C)C PRKPGWQEKNEVEU-UHFFFAOYSA-N 0.000 description 1
- GPZYYYGYCRFPBU-UHFFFAOYSA-N 6-Hydroxyflavone Chemical compound C=1C(=O)C2=CC(O)=CC=C2OC=1C1=CC=CC=C1 GPZYYYGYCRFPBU-UHFFFAOYSA-N 0.000 description 1
- OZFLRNPZLCUVFP-UHFFFAOYSA-N 8-methylnonyl dihydrogen phosphate Chemical compound CC(C)CCCCCCCOP(O)(O)=O OZFLRNPZLCUVFP-UHFFFAOYSA-N 0.000 description 1
- 238000000815 Acheson method Methods 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 1
- 229910000873 Beta-alumina solid electrolyte Inorganic materials 0.000 description 1
- RWPICVVBGZBXNA-BGYRXZFFSA-N Bis(2-ethylhexyl) terephthalate Natural products CCCC[C@H](CC)COC(=O)C1=CC=C(C(=O)OC[C@H](CC)CCCC)C=C1 RWPICVVBGZBXNA-BGYRXZFFSA-N 0.000 description 1
- 229920002799 BoPET Polymers 0.000 description 1
- JYFHYPJRHGVZDY-UHFFFAOYSA-N Dibutyl phosphate Chemical compound CCCCOP(O)(=O)OCCCC JYFHYPJRHGVZDY-UHFFFAOYSA-N 0.000 description 1
- LQLQDKBJAIILIQ-UHFFFAOYSA-N Dibutyl terephthalate Chemical compound CCCCOC(=O)C1=CC=C(C(=O)OCCCC)C=C1 LQLQDKBJAIILIQ-UHFFFAOYSA-N 0.000 description 1
- ZVFDTKUVRCTHQE-UHFFFAOYSA-N Diisodecyl phthalate Chemical compound CC(C)CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC(C)C ZVFDTKUVRCTHQE-UHFFFAOYSA-N 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- GYCMBHHDWRMZGG-UHFFFAOYSA-N Methylacrylonitrile Chemical compound CC(=C)C#N GYCMBHHDWRMZGG-UHFFFAOYSA-N 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- KRADHMIOFJQKEZ-UHFFFAOYSA-N Tri-2-ethylhexyl trimellitate Chemical compound CCCCC(CC)COC(=O)C1=CC=C(C(=O)OCC(CC)CCCC)C(C(=O)OCC(CC)CCCC)=C1 KRADHMIOFJQKEZ-UHFFFAOYSA-N 0.000 description 1
- GTVWRXDRKAHEAD-UHFFFAOYSA-N Tris(2-ethylhexyl) phosphate Chemical compound CCCCC(CC)COP(=O)(OCC(CC)CCCC)OCC(CC)CCCC GTVWRXDRKAHEAD-UHFFFAOYSA-N 0.000 description 1
- MEESPVWIOBCLJW-KTKRTIGZSA-N [(z)-octadec-9-enyl] dihydrogen phosphate Chemical compound CCCCCCCC\C=C/CCCCCCCCOP(O)(O)=O MEESPVWIOBCLJW-KTKRTIGZSA-N 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 125000005396 acrylic acid ester group Chemical group 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- ARCGXLSVLAOJQL-UHFFFAOYSA-N anhydrous trimellitic acid Natural products OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 1
- 125000001204 arachidyl 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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([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
- 230000015572 biosynthetic process Effects 0.000 description 1
- SAOKZLXYCUGLFA-UHFFFAOYSA-N bis(2-ethylhexyl) adipate Chemical compound CCCCC(CC)COC(=O)CCCCC(=O)OCC(CC)CCCC SAOKZLXYCUGLFA-UHFFFAOYSA-N 0.000 description 1
- WXZOXVVKILCOPG-UHFFFAOYSA-N bis(2-ethylhexyl) benzene-1,3-dicarboxylate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC(C(=O)OCC(CC)CCCC)=C1 WXZOXVVKILCOPG-UHFFFAOYSA-N 0.000 description 1
- RWPICVVBGZBXNA-UHFFFAOYSA-N bis(2-ethylhexyl) benzene-1,4-dicarboxylate Chemical compound CCCCC(CC)COC(=O)C1=CC=C(C(=O)OCC(CC)CCCC)C=C1 RWPICVVBGZBXNA-UHFFFAOYSA-N 0.000 description 1
- PEIIRIVDOVFUIW-UHFFFAOYSA-N bis(7-methyloctyl) benzene-1,4-dicarboxylate Chemical compound CC(C)CCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCC(C)C)C=C1 PEIIRIVDOVFUIW-UHFFFAOYSA-N 0.000 description 1
- CRPXFUDVZZLWAP-UHFFFAOYSA-N bis(8-methylnonyl) benzene-1,3-dicarboxylate Chemical compound CC(C)CCCCCCCOC(=O)C1=CC=CC(C(=O)OCCCCCCCC(C)C)=C1 CRPXFUDVZZLWAP-UHFFFAOYSA-N 0.000 description 1
- DUQLDVZUQAAAMU-UHFFFAOYSA-N bis(8-methylnonyl) benzene-1,4-dicarboxylate Chemical compound CC(C)CCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCC(C)C)C=C1 DUQLDVZUQAAAMU-UHFFFAOYSA-N 0.000 description 1
- WFFZELZOEWLYNK-CLFAGFIQSA-N bis[(z)-octadec-9-enyl] hydrogen phosphate Chemical compound CCCCCCCC\C=C/CCCCCCCCOP(O)(=O)OCCCCCCCC\C=C/CCCCCCCC WFFZELZOEWLYNK-CLFAGFIQSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001951 carbamoylamino group Chemical group C(N)(=O)N* 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- BAAAEEDPKUHLID-UHFFFAOYSA-N decyl(triethoxy)silane Chemical compound CCCCCCCCCC[Si](OCC)(OCC)OCC BAAAEEDPKUHLID-UHFFFAOYSA-N 0.000 description 1
- NZYLTTOTIRRHQA-UHFFFAOYSA-N decyl-diethoxy-methylsilane Chemical compound CCCCCCCCCC[Si](C)(OCC)OCC NZYLTTOTIRRHQA-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- GOPWOUQJIMLDDM-UHFFFAOYSA-N dibutyl benzene-1,3-dicarboxylate Chemical compound CCCCOC(=O)C1=CC=CC(C(=O)OCCCC)=C1 GOPWOUQJIMLDDM-UHFFFAOYSA-N 0.000 description 1
- JLVWYWVLMFVCDI-UHFFFAOYSA-N diethyl benzene-1,3-dicarboxylate Chemical compound CCOC(=O)C1=CC=CC(C(=O)OCC)=C1 JLVWYWVLMFVCDI-UHFFFAOYSA-N 0.000 description 1
- ONIHPYYWNBVMID-UHFFFAOYSA-N diethyl benzene-1,4-dicarboxylate Chemical compound CCOC(=O)C1=CC=C(C(=O)OCC)C=C1 ONIHPYYWNBVMID-UHFFFAOYSA-N 0.000 description 1
- NRVRCDIOAWDMJQ-UHFFFAOYSA-N diheptyl benzene-1,3-dicarboxylate Chemical compound CCCCCCCOC(=O)C1=CC=CC(C(=O)OCCCCCCC)=C1 NRVRCDIOAWDMJQ-UHFFFAOYSA-N 0.000 description 1
- RXDQUKGEPHJIJN-UHFFFAOYSA-N diheptyl benzene-1,4-dicarboxylate Chemical compound CCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCC)C=C1 RXDQUKGEPHJIJN-UHFFFAOYSA-N 0.000 description 1
- HBGGXOJOCNVPFY-UHFFFAOYSA-N diisononyl phthalate Chemical compound CC(C)CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC(C)C HBGGXOJOCNVPFY-UHFFFAOYSA-N 0.000 description 1
- OEIWPNWSDYFMIL-UHFFFAOYSA-N dioctyl benzene-1,4-dicarboxylate Chemical compound CCCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCC)C=C1 OEIWPNWSDYFMIL-UHFFFAOYSA-N 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- YCZJVRCZIPDYHH-UHFFFAOYSA-N ditridecyl benzene-1,2-dicarboxylate Chemical compound CCCCCCCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCCCCCCC YCZJVRCZIPDYHH-UHFFFAOYSA-N 0.000 description 1
- SGYIXWKATZXTIG-UHFFFAOYSA-N ditridecyl benzene-1,3-dicarboxylate Chemical compound CCCCCCCCCCCCCOC(=O)C1=CC=CC(C(=O)OCCCCCCCCCCCCC)=C1 SGYIXWKATZXTIG-UHFFFAOYSA-N 0.000 description 1
- VWGDGKCVAVATJB-UHFFFAOYSA-N ditridecyl benzene-1,4-dicarboxylate Chemical compound CCCCCCCCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCCCCCCC)C=C1 VWGDGKCVAVATJB-UHFFFAOYSA-N 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000010332 dry classification Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-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
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- CZWLNMOIEMTDJY-UHFFFAOYSA-N hexyl(trimethoxy)silane Chemical compound CCCCCC[Si](OC)(OC)OC CZWLNMOIEMTDJY-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 1
- 125000005462 imide group Chemical group 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- LDHQCZJRKDOVOX-IHWYPQMZSA-N isocrotonic acid Chemical compound C\C=C/C(O)=O LDHQCZJRKDOVOX-IHWYPQMZSA-N 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-L isophthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC(C([O-])=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-L 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000010410 layer Substances 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
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 125000002960 margaryl 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])C([H])([H])C([H])([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
- 238000005259 measurement Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- XMYQHJDBLRZMLW-UHFFFAOYSA-N methanolamine Chemical group NCO XMYQHJDBLRZMLW-UHFFFAOYSA-N 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-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
- KBJFYLLAMSZSOG-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)aniline Chemical compound CO[Si](OC)(OC)CCCNC1=CC=CC=C1 KBJFYLLAMSZSOG-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 125000001196 nonadecyl 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])C([H])([H])C([H])([H])C([H])([H])C([H])([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
- 125000001400 nonyl 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])C([H])([H])[H] 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- AICOOMRHRUFYCM-ZRRPKQBOSA-N oxazine, 1 Chemical compound C([C@@H]1[C@H](C(C[C@]2(C)[C@@H]([C@H](C)N(C)C)[C@H](O)C[C@]21C)=O)CC1=CC2)C[C@H]1[C@@]1(C)[C@H]2N=C(C(C)C)OC1 AICOOMRHRUFYCM-ZRRPKQBOSA-N 0.000 description 1
- 125000000913 palmityl 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])C([H])([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
- 125000002958 pentadecyl 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])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
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000012926 reference standard material Substances 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 125000004079 stearyl 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])C([H])([H])C([H])([H])C([H])([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
- 238000003860 storage Methods 0.000 description 1
- 125000005504 styryl group Chemical group 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000003784 tall oil Substances 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XZHNPVKXBNDGJD-UHFFFAOYSA-N tetradecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCOC(=O)C=C XZHNPVKXBNDGJD-UHFFFAOYSA-N 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- XOALFFJGWSCQEO-UHFFFAOYSA-N tridecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCOC(=O)C=C XOALFFJGWSCQEO-UHFFFAOYSA-N 0.000 description 1
- 150000005691 triesters Chemical class 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 description 1
- JNXDCMUUZNIWPQ-UHFFFAOYSA-N trioctyl benzene-1,2,4-tricarboxylate Chemical compound CCCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCC)C(C(=O)OCCCCCCCC)=C1 JNXDCMUUZNIWPQ-UHFFFAOYSA-N 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- FJFYFBRNDHRTHL-UHFFFAOYSA-N tris(8-methylnonyl) benzene-1,2,4-tricarboxylate Chemical compound CC(C)CCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCC(C)C)C(C(=O)OCCCCCCCC(C)C)=C1 FJFYFBRNDHRTHL-UHFFFAOYSA-N 0.000 description 1
- 125000002948 undecyl 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])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 238000010333 wet classification Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
Description
本発明は、パソコン、携帯電話、ＰＤＡなどの電子機器や、ＬＥＤ、ＥＬなどの照明及び表示機器など、種々の装置の放熱に利用される熱伝導性シートに関する。 The present invention relates to a thermally conductive sheet used for heat dissipation in various devices such as electronic devices such as personal computers, mobile phones, and PDAs, and lighting and display devices such as LEDs and EL.
近年、演算素子や発光素子の著しい性能向上に伴い、パソコン、携帯電話、ＰＤＡなどの電子機器や、ＬＥＤ、ＥＬ等の照明及び表示機器などの性能向上は著しい。一方、演算素子や発光素子の性能向上に伴い発熱量も著しく増加していることから、電子機器、照明及び表示機器等における放熱をどのように行うかは重要な課題となっている。熱対策として、演算素子や発光素子の発生する熱をできるだけ迅速に広い面積に拡散させて放熱する方法は冷却効率を上げることを目的としたもので、積極的に冷却をするものではないが、携帯電話やパソコンなどの小型電子機器や照明における冷却方法としては最も現実的なものである。特にバインダーとして、アクリル粘着剤を用いた熱伝導性シートは簡易に貼るだけで、冷却効果を得ることでき、かつ同時に発熱材料と放熱材料を接着できる簡便性を有している。 In recent years, with the remarkable improvement in the performance of arithmetic elements and light emitting elements, the performance of electronic devices such as personal computers, mobile phones, and PDAs, and lighting and display devices such as LEDs and ELs has been significantly improved. On the other hand, as the performance of arithmetic elements and light emitting elements improves, the amount of heat generated is also increasing significantly, so how to dissipate heat in electronic equipment, lighting, display equipment, etc. has become an important issue. As a heat countermeasure, the method of dissipating the heat generated by arithmetic elements and light emitting elements by spreading it over a wide area as quickly as possible is aimed at increasing cooling efficiency, and does not actively cool the device. This is the most practical method for cooling small electronic devices such as mobile phones and computers, as well as lighting. In particular, a thermally conductive sheet using an acrylic adhesive as a binder can provide a cooling effect by simply pasting it, and at the same time has the convenience of bonding a heat generating material and a heat dissipating material.
このような熱を拡散させる熱伝導性シートの使用量は急速に拡大している。熱伝導性シートは一般的に、粘着性を有するバインダー成分中に熱伝導性フィラーを分散した複合材料であって、熱伝導性フィラーとしてはシリカやアルミナが多く用いられている。しかし、シリカとアルミナの熱伝導率は各々１Ｗ／ｍ・Ｋ、３０Ｗ／ｍ・Ｋ程度であり、例えばアルミナを含有する熱伝導性シートでも、その熱伝導率は一般的に１～２Ｗ／ｍ・Ｋ程に留まっている。近年では熱伝導性のフィラーとして窒化アルミニウムや窒化ホウ素が用いられる場合も出てきたが、これら窒化アルミニウムや窒化ホウ素は価格が高く、熱伝導性シートのコストが高くなるという問題があった。 The amount of use of such thermally conductive sheets that diffuse heat is rapidly increasing. A thermally conductive sheet is generally a composite material in which a thermally conductive filler is dispersed in an adhesive binder component, and silica and alumina are often used as the thermally conductive filler. However, the thermal conductivity of silica and alumina is about 1 W/m・K and 30 W/m・K, respectively, and even a thermally conductive sheet containing alumina, for example, generally has a thermal conductivity of 1 to 2 W/m.・It remains at about K. In recent years, aluminum nitride and boron nitride have been used as thermally conductive fillers in some cases, but these aluminum nitrides and boron nitrides are expensive and have the problem of increasing the cost of thermally conductive sheets.
酸化亜鉛は、一般的な熱伝導性フィラーであるアルミナや窒化アルミニウムのほぼ中間の値の熱伝導率を有し、線膨張係数、硬度等の粉体物性、価格の面で比較的バランスの取れた材料であることから、熱伝導性シートの材料として種々検討がなされている。例えば、特許文献１には熱伝導性粘着シート形成用粘着剤組成物に、窒素含有モノマーを含む各種モノマー成分、カルボキシル基含有モノマー由来単位及び／または単官能アクリル酸エステルモノマー由来単位を含むプレポリマー、熱伝導性粒子及び分散剤を、それぞれ特定の割合で配合することにより、優れた粘着力と再剥離性を兼ね備えた熱伝導性を有する粘着シートが得られることが記載されており、特許文献２には酸化亜鉛と酸化亜鉛以外の第二熱伝導性フィラーを含有することにより、良好な密着性と高い熱伝導性を両立した熱伝導性発泡シートが得られることが記載されている。 Zinc oxide has a thermal conductivity that is approximately intermediate between common thermally conductive fillers such as alumina and aluminum nitride, and is relatively well-balanced in terms of linear expansion coefficient, powder properties such as hardness, and price. Since it is a material with high temperature, various studies have been conducted as a material for thermally conductive sheets. For example, in Patent Document 1, a prepolymer containing various monomer components including a nitrogen-containing monomer, a unit derived from a carboxyl group-containing monomer, and/or a unit derived from a monofunctional acrylic acid ester monomer is disclosed in Patent Document 1. , it is stated that by blending thermally conductive particles and a dispersant in specific proportions, a thermally conductive adhesive sheet with excellent adhesive strength and removability can be obtained, and Patent Document No. 2 describes that a thermally conductive foam sheet having both good adhesion and high thermal conductivity can be obtained by containing zinc oxide and a second thermally conductive filler other than zinc oxide.
また、熱伝導性シートを構成する熱伝導性フィラー以外の材料についても種々目的に応じて検討がなされている。例えば、特許文献３には粘着剤の主成分が酸価５ｍｇＫＯＨ／ｇ以下のアクリル系粘着剤と熱伝導性粒子を含有する熱伝導性粘着組成物によりゲル化するおそれがなく、しかも粘着性及びタック性が不十分になるおそれのない熱伝導性粘着シートが記載されている。また、特許文献４にはリン酸トリエステル体を含有するリン酸エステル系分散剤、及び熱伝導性粒子を含有するアクリル系粘着剤層を有することにより熱伝導性と共に、優れた電気絶縁性を有する熱伝導性粘着シートが記載され、特許文献５には窒化アルミニウム粒子、窒化ホウ素粒子または酸化マグネシウム粒子を特定の酸性リン酸エステルにより表面修飾することによって、良好な成型性と高い熱伝導率を有する放熱用樹脂組成物が記載されている。 Further, materials other than the thermally conductive filler constituting the thermally conductive sheet are also being studied depending on various purposes. For example, Patent Document 3 discloses a thermally conductive adhesive composition in which the main components of the adhesive include an acrylic adhesive with an acid value of 5 mgKOH/g or less and thermally conductive particles, which has no risk of gelation, and has excellent adhesive properties. A thermally conductive pressure-sensitive adhesive sheet that does not have insufficient tackiness is described. In addition, Patent Document 4 discloses that by having a phosphoric acid ester dispersant containing a phosphoric triester and an acrylic adhesive layer containing thermally conductive particles, it has excellent electrical insulation as well as thermal conductivity. Patent Document 5 describes a thermally conductive adhesive sheet that has good moldability and high thermal conductivity by surface-modifying aluminum nitride particles, boron nitride particles, or magnesium oxide particles with a specific acidic phosphate ester. A heat dissipating resin composition is described.
更に、より過酷な環境下での低熱抵抗化の要求の高まりから、例えば、特許文献６には、特定の粒径を有するアルミナ粉末と酸化亜鉛粉末に対してアルキルアルコキシシランを添加することによって高温高湿条件で使用した場合の耐久性に優れる熱伝導性材料が記載され、特許文献７には、無機充填剤とシリコーンオイルを含む熱伝導性シートによって、高温・高湿度環境下における絶縁安定性に優れた半導体装置が記載されている。 Furthermore, due to the increasing demand for lower heat resistance under harsher environments, for example, Patent Document 6 discloses that high temperature resistance is achieved by adding alkyl alkoxysilane to alumina powder and zinc oxide powder having specific particle sizes. A thermally conductive material with excellent durability when used in high-humidity conditions is described, and Patent Document 7 describes that a thermally conductive sheet containing an inorganic filler and silicone oil provides insulation stability under high-temperature and high-humidity environments. An excellent semiconductor device has been described.
酸化亜鉛は前述の通り、熱伝導性やコストのバランスが取れていて良好な材料である。しかしながら、一般的に熱伝導性シートの熱伝導性フィラーとして用いられるのはアルミナや窒化ホウ素がほとんどで、特にアクリル粘着剤をバインダーとして用いる熱伝導性シートにおいて、酸化亜鉛はほとんど用いられていないのが現状であり、例えばアクリル粘着剤を含有する熱伝導性シートに熱伝導性フィラーとして酸化亜鉛を用いた場合、アルミナなどと比較して粘着力が低くなったり、あるいは高温高湿下で保管することで、粘着力が低下して、貼合できなくなったりする場合があった。アクリル粘着剤はアクリルモノマーを含む複数のモノマー成分を重合したアクリル共重合体を主成分とし、これに粘着付与物質等を混合したもので、酸に腐食されやすい部材、例えばＩＴＯを使用したタッチパネル用部材などに使用する場合は、アクリル酸を始めとする酸成分が入っていない、いわゆる酸フリーのアクリル粘着剤が好ましく用いられる。しかしながら、アクリル粘着剤の粘着力は極性基に依存する部分が大きく、その代表的な極性基であるカルボキシル基を含有しない酸フリーのアクリル粘着剤は一般的に粘着力が低くなる傾向があり、上述した酸化亜鉛との組み合わせでは高温高湿下において高い粘着力を維持することがより困難となる場合があった。 As mentioned above, zinc oxide is a good material with a good balance of thermal conductivity and cost. However, alumina and boron nitride are generally used as thermally conductive fillers in thermally conductive sheets, and zinc oxide is rarely used, especially in thermally conductive sheets that use acrylic adhesives as binders. For example, if zinc oxide is used as a thermally conductive filler in a thermally conductive sheet containing an acrylic adhesive, the adhesive strength will be lower than that of alumina, or the sheet will be stored under high temperature and high humidity. As a result, the adhesive strength may decrease, making it impossible to bond. Acrylic adhesives are mainly composed of acrylic copolymers made by polymerizing multiple monomer components including acrylic monomers, and are mixed with tackifying substances, etc., and are used for materials that are easily corroded by acids, such as touch panels using ITO. When used for parts, so-called acid-free acrylic adhesives that do not contain acid components such as acrylic acid are preferably used. However, the adhesive strength of acrylic adhesives largely depends on polar groups, and acid-free acrylic adhesives that do not contain carboxyl groups, which are typical polar groups, generally tend to have low adhesive strength. In combination with the above-mentioned zinc oxide, it may be more difficult to maintain high adhesive strength under high temperature and high humidity conditions.
本発明の目的は、高い熱伝導性を有し、粘着力が強く、高温高湿下で保管しても熱伝導性や粘着力の劣化のない熱伝導性シートを提供することにある。 An object of the present invention is to provide a thermally conductive sheet that has high thermal conductivity, strong adhesive strength, and does not deteriorate in thermal conductivity or adhesive strength even when stored under high temperature and high humidity conditions.
本発明者は、上記課題を解決するために鋭意検討した結果、以下の構成の熱伝導性シートによって解決できることを見出した。 As a result of intensive studies to solve the above problem, the inventors of the present invention found that the problem can be solved by a thermally conductive sheet having the following configuration.
（１）少なくとも酸化亜鉛とアクリル粘着剤を含有する熱伝導性シートであって、該酸化亜鉛の算術平均粒子径が８μｍ以上、該酸化亜鉛の含有量は全熱伝導性フィラーの体積中５０～９０体積％であり、該アクリル粘着剤の酸価が２ｍｇＫＯＨ／ｇ以下であり、更に該熱伝導性シートが下記一般式で示される酸性リン酸エステル化合物を含有することを特徴とする熱伝導性シート。 (1) A thermally conductive sheet containing at least zinc oxide and an acrylic adhesive, wherein the zinc oxide has an arithmetic mean particle diameter of 8 μm or more, and the zinc oxide content is 50 to 50% of the total volume of the thermally conductive filler. 90% by volume, the acid value of the acrylic adhesive is 2 mgKOH/g or less, and the thermally conductive sheet further contains an acidic phosphate ester compound represented by the following general formula. sheet.
式中Ｒ１はアルキル基またはアルケニル基を表す。また式中ｌは０以上の整数を表し、ｍは１もしくは２を表す。 In the formula, R 1 represents an alkyl group or an alkenyl group. In the formula, l represents an integer of 0 or more, and m represents 1 or 2.
（２）上記した熱伝導性シートが更に、無水炭酸マグネシウム、炭化ケイ素、アルミナから選ばれる少なくとも１種を含有することを特徴とする、上記（１）記載の熱伝導性シート。
（３）上記した無水炭酸マグネシウム、炭化ケイ素、およびアルミナの算術平均粒子径が８μｍ以上であることを特徴とする、上記（２）記載の熱伝導性シート。
(2) The thermally conductive sheet described in (1) above, wherein the thermally conductive sheet further contains at least one selected from anhydrous magnesium carbonate, silicon carbide, and alumina.
(3) The thermally conductive sheet described in (2) above, wherein the arithmetic mean particle diameter of the anhydrous magnesium carbonate, silicon carbide, and alumina is 8 μm or more.
本発明によって、高い熱伝導性を有し、粘着力が強く、高温高湿下で保管しても熱伝導性や粘着力の劣化のない熱伝導性シートを提供することが可能となる。 According to the present invention, it is possible to provide a thermally conductive sheet that has high thermal conductivity, strong adhesive strength, and does not deteriorate in thermal conductivity or adhesive strength even when stored under high temperature and high humidity conditions.
本発明の熱伝導性シートは、少なくとも酸化亜鉛とアクリル粘着剤を含有する熱伝導性シートであって、該酸化亜鉛の算術平均粒子径が８μｍ以上、該酸化亜鉛の含有量は全熱伝導性フィラーの体積中５０～９０体積％であり、該アクリル粘着剤の酸価が２ｍｇＫＯＨ／ｇ以下であり、更に該熱伝導性シートが上記一般式で示される酸性リン酸エステル化合物を含有する The thermally conductive sheet of the present invention is a thermally conductive sheet containing at least zinc oxide and an acrylic adhesive, wherein the zinc oxide has an arithmetic mean particle size of 8 μm or more, and the zinc oxide content has a total thermal conductivity. 50 to 90% by volume of the filler, the acid value of the acrylic adhesive is 2 mgKOH/g or less, and the thermally conductive sheet further contains an acidic phosphate ester compound represented by the above general formula.
本発明の熱伝導性シートは、熱伝導性フィラーとして少なくとも酸化亜鉛を含有する。かかる酸化亜鉛は、特開２０１４－１９３８０８号公報記載の方法や、特開２００１－３４２０２１号公報記載の方法など、公知の方法を用いて製造することができる。また酸化亜鉛は、その粒径分布において均一なものを得る必要がある場合や、粗大粒子を除去するために、粉砕あるいは篩による分級を行うものであってもよい。粉砕方法は特に限定されず、例えば、アトマイザー等を挙げることができる。また篩による分級方法としては、湿式分級、乾式分級を挙げることができる。 The thermally conductive sheet of the present invention contains at least zinc oxide as a thermally conductive filler. Such zinc oxide can be produced using a known method such as the method described in JP-A No. 2014-193808 or the method described in JP-A No. 2001-342021. Further, zinc oxide may be pulverized or classified using a sieve when it is necessary to obtain a uniform particle size distribution or to remove coarse particles. The pulverization method is not particularly limited, and examples thereof include an atomizer. Further, examples of the classification method using a sieve include wet classification and dry classification.
酸化亜鉛の形状は特には限定されず、針状、棒状、板状、球状等を挙げることができる。 The shape of zinc oxide is not particularly limited, and examples include needle-like, rod-like, plate-like, and spherical shapes.
本発明で用いる酸化亜鉛の算術平均粒子径は８μｍ以上であり、１０～３０μｍの範囲であることがより好ましい。この範囲を外れると粘着力、熱伝導性、熱抵抗などの諸性能が十分でない場合がある。なお、本発明で使用する熱伝導性フィラーの算術平均粒子径は、例えばレーザー散乱式粒度分布計を用いて測定することができる。 The arithmetic mean particle diameter of the zinc oxide used in the present invention is 8 μm or more, preferably in the range of 10 to 30 μm. Outside this range, various properties such as adhesive strength, thermal conductivity, and thermal resistance may not be sufficient. Note that the arithmetic mean particle diameter of the thermally conductive filler used in the present invention can be measured using, for example, a laser scattering particle size distribution analyzer.
本発明で用いる酸化亜鉛の好ましい市販品としては堺化学工業（株）製のＬＰＺＩＮＣ（登録商標）１１、ＬＰＺＩＮＣ２０や、ハクスイテック（株）製の焼結亜鉛華などが挙げられる。 Preferred commercial products of zinc oxide used in the present invention include LPZINC (registered trademark) 11 and LPZINC 20 manufactured by Sakai Chemical Industry Co., Ltd., and sintered zinc white manufactured by Hakusui Tech Co., Ltd.
本発明の熱伝導性シートは熱伝導性フィラーとして酸化亜鉛に加えて、無水炭酸マグネシウム、炭化ケイ素、アルミナから選ばれる少なくとも１種を含有することが好ましい。これらはコスト面、化学的安定性において良好な材料である。無水炭酸マグネシウムは例えば中性炭酸マグネシウム（ＭｇＣＯ３・ｎＨ２Ｏ、ｎは１～５程度）をオートクレーブ中で水熱処理した後に乾燥して無水炭酸マグネシウムとする方法など公知の方法で製造することができる。水熱処理としては撹拌下、最高温度が１５０～２５０℃で１～２０時間の条件などが挙げられ、水熱処理後、乾燥する際の乾燥温度としては１００℃以上でかつ、無水炭酸マグネシウムの分解温度（約２５０℃）以下で乾燥することが好ましい。かかる無水炭酸マグネシウムの市販品としては神島化学工業（株）製のマグサーモ（登録商標）ＭＳ－ＰＳなどを挙げることができる。 The thermally conductive sheet of the present invention preferably contains at least one selected from anhydrous magnesium carbonate, silicon carbide, and alumina in addition to zinc oxide as a thermally conductive filler. These materials are good in terms of cost and chemical stability. Anhydrous magnesium carbonate can be produced by known methods such as hydrothermally treating neutral magnesium carbonate (MgCO 3 .nH 2 O, where n is about 1 to 5) in an autoclave and then drying it to form anhydrous magnesium carbonate. can. Examples of hydrothermal treatment include conditions such as stirring at a maximum temperature of 150 to 250°C for 1 to 20 hours, and the drying temperature after hydrothermal treatment is 100°C or higher and the decomposition temperature of anhydrous magnesium carbonate. (approximately 250° C.) or lower. Examples of commercially available anhydrous magnesium carbonate include Magthermo (registered trademark) MS-PS manufactured by Kamishima Chemical Industry Co., Ltd.
本発明で好ましく用いられる炭化ケイ素は六方晶であるα型、あるいは立方晶であるβ型のいずれでも使用することができる。α型は硬度が高いものの安価であり、本発明においては好ましい。α型炭化ケイ素はアチソン法で合成した後、粉砕、分級するなど公知の方法で製造することができる。α型炭化ケイ素の市販品としては（株）フジミインコーポレーテッド製のＧＣ＃３２０やＧＣ＃１２００など、β型炭化ケイ素としては巴工業（株）製β－ＳｉＣ＃４００などを挙げることができる。 The silicon carbide preferably used in the present invention can be either a hexagonal α type or a cubic β type. Although the α type has high hardness, it is inexpensive and is preferred in the present invention. α-type silicon carbide can be produced by a known method such as synthesis by the Acheson method, followed by pulverization and classification. Commercial products of α-type silicon carbide include GC#320 and GC#1200 manufactured by Fujimi Incorporated, and examples of β-type silicon carbide include β-SiC#400 manufactured by Tomoe Kogyo Co., Ltd.
本発明で好ましく用いられるアルミナはαアルミナ、βアルミナ、γアルミナ等があり、いずれの結晶形を有するアルミナを用いてもよいが、化学的安定性の観点からはαアルミナを用いるのが好ましい。アルミナは、破砕された破砕アルミナであってもよく、球状である球状アルミナであってもよい。破砕アルミナは、例えば、一軸破砕機、二軸破砕機、ハンマークラッシャーまたはボールミル等を用いて、塊状のアルミナを破砕することにより得られる。破砕アルミナは、一般的に安価であることから粉砕アルミナを用いることが好ましい。アルミナの市販品としては、例えば、大平洋ランダム（株）製ＬＡ１２００、同じくＬＡ２０００、同じくＬＡ４０００、昭和電工（株）製ＡＳ－１０、（株）フジミインコーポレーテッド製ＦＥ１０Ａ等が挙げられる。 Aluminas preferably used in the present invention include α-alumina, β-alumina, γ-alumina, etc. Alumina having any crystal form may be used, but α-alumina is preferably used from the viewpoint of chemical stability. The alumina may be crushed alumina, or may be spherical alumina. Crushed alumina is obtained by crushing lump-like alumina using, for example, a single-shaft crusher, a twin-shaft crusher, a hammer crusher, a ball mill, or the like. It is preferable to use crushed alumina because it is generally inexpensive. Commercially available alumina products include, for example, LA1200, LA2000, and LA4000 manufactured by Pacific Random Co., Ltd., AS-10 manufactured by Showa Denko K.K., and FE10A manufactured by Fujimi Incorporated.
本発明で好ましく用いられる無水炭酸マグネシウム、炭化ケイ素、及びアルミナの粒径（算術平均粒径）は８μｍ以上であることが好ましく、より好ましくは１２～６０μｍである。これにより良好な粘着力を有する熱伝導性シートを得ることができる。本発明において無水炭酸マグネシウムや炭化ケイ素、アルミナの中では硬度が低く、熱伝導性の安定性の高い無水炭酸マグネシウムが最も好ましい。 The particle size (arithmetic mean particle size) of anhydrous magnesium carbonate, silicon carbide, and alumina preferably used in the present invention is preferably 8 μm or more, more preferably 12 to 60 μm. Thereby, a thermally conductive sheet having good adhesive strength can be obtained. In the present invention, among anhydrous magnesium carbonate, silicon carbide, and alumina, anhydrous magnesium carbonate is most preferable because it has low hardness and high thermal conductivity stability.
本発明の熱伝導性シートは、熱伝導性フィラーとして、酸化亜鉛、無水炭酸マグネシウム、炭化ケイ素、アルミナ以外にも他の無機フィラーを混合して用いることも可能である。他の無機フィラーとしては、窒化アルミニウム、窒化ホウ素、水酸化アルミニウム、水酸化マグネシウム、炭酸マグネシウム、ダイヤモンド、珪藻土、二酸化珪素などが挙げられる。また、一般式ＭｏＯｐ・ＸＨ２Ｏ（ここにＭは金属、ｏ、ｐは金属の原子価によって定まる１以上の整数、Ｘは含有結晶水の数を示す数）で表される水和金属化合物は難燃性を有するので、これも併せて用いることができる。これら他の無機フィラーの含有量は全熱伝導性フィラーの１体積％以上とすることが好ましい。 In addition to zinc oxide, anhydrous magnesium carbonate, silicon carbide, and alumina, the thermally conductive sheet of the present invention may also contain a mixture of other inorganic fillers as the thermally conductive filler. Examples of other inorganic fillers include aluminum nitride, boron nitride, aluminum hydroxide, magnesium hydroxide, magnesium carbonate, diamond, diatomaceous earth, and silicon dioxide. In addition, water expressed by the general formula M o O p · Since the Japanese metal compound has flame retardancy, it can also be used in combination. The content of these other inorganic fillers is preferably 1% by volume or more of the total thermally conductive filler.
本発明の熱伝導性シートが含有する熱伝導性フィラーはシランカップリング剤による表面処理など公知の処理も施すことができる。また、複数の表面処理を組み合わせて用いることも可能である。 The thermally conductive filler contained in the thermally conductive sheet of the present invention can be subjected to known treatments such as surface treatment with a silane coupling agent. It is also possible to use a combination of multiple surface treatments.
熱伝導性フィラーの表面処理に好ましく使用するシランカップリング剤としては、モノマーあるいはオリゴマーのいずれであってもよい。かかるモノマーとしては、具体的には、Ｒ２ ｑＳｉ（ＯＲ３）４－ｑの構造式で示される化合物を例示することができ、ここで、ｑは１～３の整数であり、Ｒ２は活性水素を有する基（例えばアミノ基、メルカプト基、ウレイド基など）、重合性反応基（例えばビニル基、メタクリロキシ基、アクリロキシ基、スチリル基など）、活性水素と反応し得る基（例えばエポキシ基、イソシアネート基など）、アルキル基（直鎖状、分岐状及び環状のいずれでもあってもよく、炭素原子数が２～１８の範囲内にあることが好ましい）、及びフェニル基が挙げられ、ＯＲ３はメトキシ基、エトキシ基等のアルコキシ基から選択される基であり、ｑが１～２の場合（ＯＲ３が２個以上の場合）、ＯＲ３は同一であっても異なっていてもよい。 The silane coupling agent preferably used for surface treatment of the thermally conductive filler may be either a monomer or an oligomer. Specific examples of such monomers include compounds represented by the structural formula R 2 q Si(OR 3 ) 4-q , where q is an integer from 1 to 3, and R 2 is a group having active hydrogen (e.g., amino group, mercapto group, ureido group, etc.), a polymerizable reactive group (e.g., vinyl group, methacryloxy group, acryloxy group, styryl group, etc.), or a group that can react with active hydrogen (e.g., epoxy group). , isocyanate group, etc.), alkyl groups (which may be linear, branched, or cyclic, and preferably have a carbon atom number in the range of 2 to 18), and phenyl groups, and OR 3 is a group selected from alkoxy groups such as methoxy group and ethoxy group, and when q is 1 to 2 (when OR 3 is 2 or more), OR 3 may be the same or different. .
上記したシランカップリング剤のうち、アミノ基を有するシランカップリング剤、ビニル基を有するシランカップリング剤、アルキル基を有するシランカップリング剤等が好ましい。 Among the silane coupling agents described above, silane coupling agents having an amino group, silane coupling agents having a vinyl group, silane coupling agents having an alkyl group, and the like are preferred.
アミノ基を有するシランカップリング剤の例としては、Ｎ－（２－アミノエチル）－３－アミノプロピルメチルジメトキシシラン、Ｎ－（２－アミノエチル）－３－アミノプロピルトリメトキシシラン、Ｎ－（２－アミノエチル）－３－アミノプロピルトリエトキシシラン、３－アミノプロピルトリメトキシシラン、３－アミノプロピルトリエトキシシラン、３－トリエトキシシリル－Ｎ－（１，３－ジメチルブチリデン）プロピルアミン及びＮ－フェニル－３－アミノプロピルトリメトキシシラン等が挙げられる。 Examples of silane coupling agents having an amino group include N-(2-aminoethyl)-3-aminopropylmethyldimethoxysilane, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, N-( 2-aminoethyl)-3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3-triethoxysilyl-N-(1,3-dimethylbutylidene)propylamine and Examples include N-phenyl-3-aminopropyltrimethoxysilane.
ビニル基を有するシランカップリング剤の例としては、ビニルトリメトキシシラン及びビニルトリエトキシシランなどのビニルシラン等が挙げられ、アルキル基を有するシランカップリング剤の例としてはヘキシルトリメトキシシラン、デシルトリエトキシシラン、デシルメチルジエトキシシラン等が挙げられる。中でも粘着性の良好な熱伝導材料が得られる観点からビニル基を有するシランカップリング剤がより好ましい。 Examples of silane coupling agents having a vinyl group include vinyl silanes such as vinyltrimethoxysilane and vinyltriethoxysilane, and examples of silane coupling agents having an alkyl group include hexyltrimethoxysilane, decyltriethoxysilane, etc. Examples include silane and decylmethyldiethoxysilane. Among them, a silane coupling agent having a vinyl group is more preferable from the viewpoint of obtaining a thermally conductive material with good adhesiveness.
熱伝導性フィラーのシランカップリング剤による表面の処理方法は、乾式法、湿式法のいずれであってもよい。 The method for treating the surface of the thermally conductive filler with the silane coupling agent may be either a dry method or a wet method.
本発明の熱伝導性シートは、酸化亜鉛を含有し、その含有量は全熱伝導性フィラーの体積中５０～９０体積％であり、更に好ましくは６０～８０体積％である。また、無水炭酸マグネシウム、炭化ケイ素、及びアルミナの好ましい含有量は全熱伝導性フィラーの体積中５～４０体積％であることが好ましく、更に好ましくは１３～３３体積％である。 The thermally conductive sheet of the present invention contains zinc oxide, and its content is 50 to 90% by volume, more preferably 60 to 80% by volume, based on the total volume of the thermally conductive filler. Further, the preferable content of anhydrous magnesium carbonate, silicon carbide, and alumina is preferably 5 to 40 volume %, more preferably 13 to 33 volume %, based on the total volume of the thermally conductive filler.
本発明の熱伝導性シートは、バインダー成分としてアクリル粘着剤を含有する。アクリル粘着剤としては、アクリルモノマーを含む複数のモノマー成分を重合したアクリル共重合体を用いることができる。使用できるモノマー成分としては、例えば、（メタ）アクリル酸、イタコン酸、マレイン酸、フマル酸、クロトン酸、イソクロトン酸等のカルボキシル基含有モノマーまたはその無水物（例えば無水マレイン酸等）、（メタ）アクリル酸メチル、（メタ）アクリル酸エチル、（メタ）アクリル酸プロピル、（メタ）アクリル酸イソプロピル、（メタ）アクリル酸ブチル、（メタ）アクリル酸イソブチル、（メタ）アクリル酸ｓ－ブチル、（メタ）アクリル酸ｔ－ブチル、（メタ）アクリル酸ペンチル、（メタ）アクリル酸イソペンチル、（メタ）アクリル酸ヘキシル、（メタ）アクリル酸ヘプチル、（メタ）アクリル酸オクチル、（メタ）アクリル酸２－エチルヘキシル、（メタ）アクリル酸イソオクチル、（メタ）アクリル酸ノニル、（メタ）アクリル酸イソノニル、（メタ）アクリル酸デシル、（メタ）アクリル酸イソデシル、（メタ）アクリル酸ウンデシル、（メタ）アクリル酸ドデシル、（メタ）アクリル酸トリデシル、（メタ）アクリル酸テトラデシル、（メタ）アクリル酸ペンタデシル、（メタ）アクリル酸ヘキサデシル、（メタ）アクリル酸ヘプタデシル、（メタ）アクリル酸オクタデシル、（メタ）アクリル酸イソステアリル、（メタ）アクリル酸ノナデシル、（メタ）アクリル酸エイコシル等の炭素数が１～２０の直鎖または分岐鎖状のアルキル基を有する（メタ）アクリル酸アルキルエステル、（メタ）アクリル酸２－メトキシエチル、（メタ）アクリル酸２－エトキシエチル、（メタ）アクリル酸メトキシトリエチレングリコール、（メタ）アクリル酸３－メトキシプロピル、（メタ）アクリル酸３－エトキシプロピル、（メタ）アクリル酸４－メトキシブチル、（メタ）アクリル酸４－エトキシブチル等の（メタ）アクリル酸アルコキシアルキルエステル、（メタ）アクリル酸２－ヒドロキシエチル、（メタ）アクリル酸３－ヒドロキシプロピル、（メタ）アクリル酸４－ヒドロキシブチル、（メタ）アクリル酸６－ヒドロキシヘキシル等の（メタ）アクリル酸ヒドロキシアルキル、アリルアルコール等のヒドロキシル基（水酸基）含有モノマー、（メタ）アクリルアミド、Ｎ，Ｎ－ジメチル（メタ）アクリルアミド、Ｎ－メチロール（メタ）アクリルアミド、Ｎ－メトキシメチル（メタ）アクリルアミド、Ｎ－ブトキシメチル（メタ）アクリルアミド、Ｎ－ヒドロキシエチル（メタ）アクリルアミド等のアミド基含有モノマー、（メタ）アクリル酸アミノエチル、（メタ）アクリル酸ジメチルアミノエチル、（メタ）アクリル酸ｔ－ブチルアミノエチル等のアミノ基含有モノマー、（メタ）アクリル酸グリシジル、（メタ）アクリル酸メチルグリシジル等のグリシジル基含有モノマー、アクリロニトリルやメタクリロニトリル等のシアノ基含有モノマー、Ｎ－ビニル－２－ピロリドン、（メタ）アクリロイルモルホリンの他、Ｎ－ビニルピリジン、Ｎ－ビニルピペリドン、Ｎ－ビニルピリミジン、Ｎ－ビニルピペラジン、Ｎ－ビニルピロール、Ｎ－ビニルイミダゾール、Ｎ－ビニルオキサゾール等の複素環含有ビニル系モノマー、ビニルスルホン酸ナトリウム等のスルホン酸基含有モノマー、２－ヒドロキシエチル（メタ）アクリロイルフォスフェート等のリン酸基含有モノマー、シクロヘキシルマレイミド、イソプロピルマレイミド等のイミド基含有モノマー、２－（メタ）アクリロイルオキシエチルイソシアネート等のイソシアネート基含有モノマー等が挙げられるが、（メタ）アクリル酸を始めとするカルボキシル基含有モノマーはアクリル粘着剤の酸価を２ｍｇＫＯＨ／ｇ以下とするため、実質的に使用しないことが好ましい。 The thermally conductive sheet of the present invention contains an acrylic adhesive as a binder component. As the acrylic adhesive, an acrylic copolymer obtained by polymerizing a plurality of monomer components including an acrylic monomer can be used. Examples of monomer components that can be used include carboxyl group-containing monomers such as (meth)acrylic acid, itaconic acid, maleic acid, fumaric acid, crotonic acid, and isocrotonic acid, or their anhydrides (such as maleic anhydride), (meth) Methyl acrylate, ethyl (meth)acrylate, propyl (meth)acrylate, isopropyl (meth)acrylate, butyl (meth)acrylate, isobutyl (meth)acrylate, s-butyl (meth)acrylate, (meth)acrylate ) t-Butyl acrylate, pentyl (meth)acrylate, isopentyl (meth)acrylate, hexyl (meth)acrylate, heptyl (meth)acrylate, octyl (meth)acrylate, 2-ethylhexyl (meth)acrylate , isooctyl (meth)acrylate, nonyl (meth)acrylate, isononyl (meth)acrylate, decyl (meth)acrylate, isodecyl (meth)acrylate, undecyl (meth)acrylate, dodecyl (meth)acrylate, (meth)tridecyl acrylate, (meth)tetradecyl acrylate, pentadecyl (meth)acrylate, hexadecyl (meth)acrylate, heptadecyl (meth)acrylate, octadecyl (meth)acrylate, isostearyl (meth)acrylate, (meth)acrylic acid alkyl esters having a linear or branched alkyl group having 1 to 20 carbon atoms, such as nonadecyl (meth)acrylate and eicosyl (meth)acrylate, 2-methoxyethyl (meth)acrylate , 2-ethoxyethyl (meth)acrylate, methoxytriethylene glycol (meth)acrylate, 3-methoxypropyl (meth)acrylate, 3-ethoxypropyl (meth)acrylate, 4-methoxybutyl (meth)acrylate , (meth)acrylic acid alkoxyalkyl esters such as 4-ethoxybutyl (meth)acrylate, 2-hydroxyethyl (meth)acrylate, 3-hydroxypropyl (meth)acrylate, 4-hydroxybutyl (meth)acrylate , hydroxyalkyl (meth)acrylates such as 6-hydroxyhexyl (meth)acrylate, hydroxyl group-containing monomers such as allyl alcohol, (meth)acrylamide, N,N-dimethyl (meth)acrylamide, N-methylol Amide group-containing monomers such as (meth)acrylamide, N-methoxymethyl (meth)acrylamide, N-butoxymethyl (meth)acrylamide, N-hydroxyethyl (meth)acrylamide, aminoethyl (meth)acrylate, (meth)acrylic Amino group-containing monomers such as dimethylaminoethyl acid and t-butylaminoethyl (meth)acrylate; glycidyl group-containing monomers such as glycidyl (meth)acrylate and methylglycidyl (meth)acrylate; acrylonitrile and methacrylonitrile; In addition to cyano group-containing monomers, N-vinyl-2-pyrrolidone, (meth)acryloylmorpholine, N-vinylpyridine, N-vinylpiperidone, N-vinylpyrimidine, N-vinylpiperazine, N-vinylpyrrole, N-vinylimidazole, Heterocycle-containing vinyl monomers such as N-vinyloxazole, sulfonic acid group-containing monomers such as sodium vinylsulfonate, phosphoric acid group-containing monomers such as 2-hydroxyethyl (meth)acryloyl phosphate, cyclohexyl maleimide, isopropyl maleimide, etc. Examples include imide group-containing monomers and isocyanate group-containing monomers such as 2-(meth)acryloyloxyethyl isocyanate, but carboxyl group-containing monomers such as (meth)acrylic acid have an acid value of 2 mgKOH/g of the acrylic adhesive. In order to meet the following requirements, it is preferable not to use substantially.
本発明で用いるアクリル粘着剤は粘着付与剤を含有することができる。粘着付与剤としては、ガムロジン、トール油ロジン、ウッドロジンの未変性ロジンをアルコールなどでエステル化したロジンエステルや、未変性ロジンを変性した不均化ロジン、重合ロジン、水添ロジンなどの変性ロジン、これら変性ロジンを更にアルコールなどでエステル化した不均化ロジンエステル、重合ロジンエステル、水添ロジンエステルなどの変性ロジンエステル、未変性ロジンにフェノールを付加したロジンフェノール、テルペンフェノール樹脂、ジペンテン樹脂、芳香族変性テルペン樹脂、水添テルペン樹脂、酸変性テルペン樹脂、スチレン化テルペン樹脂などのテルペン系樹脂、石油樹脂等が挙げられる。粘着付与剤は単独でも複数を組み合わせて用いてもよく、ロジン系粘着付与剤とテルペン系粘着付与剤を組み合わせて用いることもできる。粘着付与剤の量はアクリル共重合体に対して５～１００質量％の範囲で用いられることができる。 The acrylic adhesive used in the present invention can contain a tackifier. Tackifiers include rosin esters made by esterifying unmodified rosins such as gum rosin, tall oil rosin, and wood rosin with alcohol, modified rosins such as disproportionated rosins, polymerized rosins, hydrogenated rosins, etc. Modified rosin esters such as disproportionated rosin esters, polymerized rosin esters, and hydrogenated rosin esters, which are obtained by further esterifying these modified rosins with alcohol, rosin phenols obtained by adding phenol to unmodified rosins, terpene phenol resins, dipentene resins, and fragrances. Examples include terpene resins such as group-modified terpene resins, hydrogenated terpene resins, acid-modified terpene resins, and styrenated terpene resins, petroleum resins, and the like. The tackifier may be used alone or in combination, and a rosin-based tackifier and a terpene-based tackifier may also be used in combination. The amount of tackifier used can range from 5 to 100% by weight based on the acrylic copolymer.
本発明で用いるアクリル粘着剤の酸価は２ｍｇＫＯＨ／ｇ以下であり、好ましくは１ｍｇ／ＫＯＨ以下である。また、熱伝導性シートの全有機成分に対するアクリル粘着剤（アクリル共重合体と粘着付与剤の合計）の含有量は７０～９８質量％、好ましくは８０～９６質量％である。 The acid value of the acrylic adhesive used in the present invention is 2 mgKOH/g or less, preferably 1 mg/KOH or less. Further, the content of the acrylic adhesive (total of the acrylic copolymer and tackifier) relative to the total organic components of the thermally conductive sheet is 70 to 98% by mass, preferably 80 to 96% by mass.
本発明で用いるアクリル粘着剤としては、アクリル共重合体と粘着付与剤を含有した市販品を用いてもよく、例えば日本カーバイド（株）製ＫＰ－２５６３、同じくＫＰ２５６５、同じくＫＰ－２６１０、ＤＩＣ（株）製ＣＴ－６０３０、藤倉化成（株）製ＬＫＧ－１００９、同じくＬＫＧ－１０１３などが挙げられる。 As the acrylic adhesive used in the present invention, commercially available products containing an acrylic copolymer and a tackifier may be used, such as KP-2563, KP2565, KP-2610, and DIC (manufactured by Nippon Carbide Co., Ltd.). Examples include CT-6030 manufactured by Fujikura Kasei Co., Ltd., LKG-1009 manufactured by Fujikura Kasei Co., Ltd., and LKG-1013 manufactured by Fujikura Kasei Co., Ltd.
本発明においてアクリル粘着剤の凝集力をより一層向上させ、安定した熱伝導率を得る上で、熱伝導シートはアクリル粘着剤と共に架橋剤を含有することが好ましい。架橋剤としては、イソシアネート架橋剤、エポキシ架橋剤、金属キレート架橋剤、アジリジン架橋剤等を使用することができる。中でも、イソシアネート架橋剤またはエポキシ架橋剤を使用することが好ましい。 In the present invention, in order to further improve the cohesive force of the acrylic adhesive and obtain stable thermal conductivity, the thermally conductive sheet preferably contains a crosslinking agent together with the acrylic adhesive. As the crosslinking agent, an isocyanate crosslinking agent, an epoxy crosslinking agent, a metal chelate crosslinking agent, an aziridine crosslinking agent, etc. can be used. Among these, it is preferable to use an isocyanate crosslinking agent or an epoxy crosslinking agent.
本発明の粘着性シートは前記した一般式で示される酸性リン酸エステル化合物を含有する。 The adhesive sheet of the present invention contains an acidic phosphoric acid ester compound represented by the general formula described above.
前記した一般式で示される酸性リン酸エステル化合物の中でも、ｌは０～５であることが好ましく、Ｒ１として炭素数が３～２０の直鎖あるいは分岐したアルキル基を有する酸性リン酸エステル化合物が特に好ましく、この具体例としては、ｌ＝０の酸性リン酸エステル化合物としてはリン酸モノイソブチル、リン酸モノイソデシル、リン酸モノオレイル、リン酸モノ２－エチルヘキシル、リン酸ジブチル、リン酸ジオレイルなどが挙げられ、ｌが１以上の酸性リン酸エステル化合物としては、ｌが２、ｍが２、Ｒ１がＣ１２～１５のアルキルであるポリオキシエチレンエーテルリン酸、ｌが４、ｍが２、Ｒ１がＣ１２～１５のアルキルであるポリオキシエチレンエーテルリン酸などが挙げられる。また、前記した一般式で示される酸性リン酸エステル化合物の市販品としては例えばｌ＝０の酸性リン酸エステル化合物ではＤＰ－４、ＡＰ－１０（大八化学工業（株）製）、ｌが１以上の酸性リン酸エステル化合物ではニッコール（登録商標）ＤＤＰ－２、ＤＤＰ－４（日光ケミカルズ（株）製）、などが挙げられる。 Among the acidic phosphoric ester compounds represented by the general formula described above, l is preferably 0 to 5, and acidic phosphoric ester compounds having a linear or branched alkyl group having 3 to 20 carbon atoms as R 1 is particularly preferable, and specific examples of the acidic phosphoric acid ester compound with l=0 include monoisobutyl phosphate, monoisodecyl phosphate, monooleyl phosphate, mono-2-ethylhexyl phosphate, dibutyl phosphate, dioleyl phosphate, etc. Examples of acidic phosphoric acid ester compounds in which l is 1 or more include polyoxyethylene ether phosphoric acid in which l is 2, m is 2, and R 1 is a C12-15 alkyl; l is 4, m is 2, and R Examples include polyoxyethylene ether phosphoric acid in which 1 is C12-15 alkyl. In addition, as commercially available acidic phosphate ester compounds represented by the above general formula, for example, acidic phosphoric ester compounds where l=0 include DP-4, AP-10 (manufactured by Daihachi Chemical Industry Co., Ltd.), and l=0. Examples of the one or more acidic phosphate ester compounds include Nikkor (registered trademark) DDP-2 and DDP-4 (manufactured by Nikko Chemicals Co., Ltd.).
熱伝導性シートにおける上記した酸性リン酸エステル化合物の含有量は熱伝導性フィラーに対して０．０１～５質量％であることが好ましく、より好ましくは０．１～１質量％である。 The content of the above acidic phosphate ester compound in the thermally conductive sheet is preferably 0.01 to 5% by mass, more preferably 0.1 to 1% by mass based on the thermally conductive filler.
更に本発明の熱伝導性シートは可塑剤を含有することが好ましく、かつ該可塑剤の量が熱伝導シート中の有機成分に対し、１～２０質量％であることがより好ましく、３～１５質量％であることがより好ましい。このことは熱伝導シートの粘着力を高める上で好ましい。本発明において可塑剤としては、例えばフタル酸ジエチル、フタル酸ジ－ｎ－ブチル、フタル酸ジ－ｎ－ヘプチル、フタル酸ビス（２－エチルヘキシル）、フタル酸ジ－ｎ－オクチル、フタル酸ジイソノニル、フタル酸ジイソデシル、フタル酸ジトリデシル、フタル酸ｎ－ブチルベンジル、イソフタル酸ジエチル、イソフタル酸ジ－ｎ－ブチル、イソフタル酸ジ－ｎ－ヘプチル、イソフタル酸ビス（２－エチルヘキシル）、イソフタル酸ジ－ｎ－オクチル、イソフタル酸ジイソノニル、イソフタル酸ジイソデシル、イソフタル酸ジトリデシル、イソフタル酸ｎ－ブチルベンジル、テレフタル酸ジエチル、テレフタル酸ジ－ｎ－ブチル、テレフタル酸ジ－ｎ－ヘプチル、テレフタル酸ビス（２－エチルヘキシル）、テレフタル酸ジ－ｎ－オクチル、テレフタル酸ジイソノニル、テレフタル酸ジイソデシル、テレフタル酸ジトリデシル、テレフタル酸ｎ－ブチルベンジル等のフタル酸エステル系可塑剤；アジピン酸ビス（２－エチルヘキシル）、アジピン酸ジ－ｎ－オクチル、アジピン酸ジイソノニル、アジピン酸ジイソデシル等のアジピン酸エステル系可塑剤；リン酸トリエチル、リン酸トリクレジル、リン酸トリフェニル、リン酸トリス（２－エチルヘキシル）、リン酸トリキシリル等のリン酸エステル系可塑剤；トリメリット酸トリス（２－エチルヘキシル）、トリメリット酸トリ－ｎ－オクチル、トリメリット酸トリイソデシル等のトリメリット酸エステル系可塑剤；二塩基酸（例えば、セバシン酸、アジピン酸、アゼライン酸、フタル酸）及び二価アルコール（例えば、グリコール）などから合成される低分子量ポリエステルを主として含むポリエステル系可塑剤等の汎用の可塑剤を用いることができ、中でもリン酸エステル系可塑剤は難燃剤としても作用することから好ましい。 Further, the thermally conductive sheet of the present invention preferably contains a plasticizer, and the amount of the plasticizer is more preferably 1 to 20% by mass, and more preferably 3 to 15% by mass, based on the organic component in the thermally conductive sheet. It is more preferable that it is mass %. This is preferable in terms of increasing the adhesive strength of the thermally conductive sheet. In the present invention, examples of the plasticizer include diethyl phthalate, di-n-butyl phthalate, di-n-heptyl phthalate, bis(2-ethylhexyl) phthalate, di-n-octyl phthalate, diisononyl phthalate, Diisodecyl phthalate, ditridecyl phthalate, n-butylbenzyl phthalate, diethyl isophthalate, di-n-butyl isophthalate, di-n-heptyl isophthalate, bis(2-ethylhexyl) isophthalate, di-n- isophthalate Octyl, diisononyl isophthalate, diisodecyl isophthalate, ditridecyl isophthalate, n-butylbenzyl isophthalate, diethyl terephthalate, di-n-butyl terephthalate, di-n-heptyl terephthalate, bis(2-ethylhexyl) terephthalate, Phthalate ester plasticizers such as di-n-octyl terephthalate, diisononyl terephthalate, diisodecyl terephthalate, ditridecyl terephthalate, and n-butylbenzyl terephthalate; bis(2-ethylhexyl) adipate, di-n-adipate Adipate ester plasticizers such as octyl, diisononyl adipate, and diisodecyl adipate; Phosphate ester plasticizers such as triethyl phosphate, tricresyl phosphate, triphenyl phosphate, tris(2-ethylhexyl) phosphate, and trixyl phosphate. agents; trimellitic acid ester plasticizers such as tris(2-ethylhexyl) trimellitate, tri-n-octyl trimellitate, and triisodecyl trimellitate; dibasic acids (e.g., sebacic acid, adipic acid, azelaic acid, General-purpose plasticizers such as polyester plasticizers mainly containing low molecular weight polyesters synthesized from phthalic acid) and dihydric alcohols (e.g. glycols) can be used, and among them, phosphate ester plasticizers can be used as flame retardants. This is preferable because it also works.
本発明の熱伝導性シートが含有する熱伝導性フィラーが熱伝導性シートに対して占める割合は３０～８０体積％であることが高い熱伝導性と被着体に対する高い粘着力を得る上で好ましく、更に４５～７５体積％であることが好ましい。なお、熱伝導性フィラーが熱伝導性シートに対して占める体積比は、使用する各熱伝導性フィラーの質量をそれぞれの密度で割ったものの合計値と、熱伝導性シートの各構成成分の質量をそれぞれの密度で割ったものの合計値との比率である。 In order to obtain high thermal conductivity and high adhesive strength to adherends, it is preferable that the thermally conductive filler contained in the thermally conductive sheet of the present invention accounts for 30 to 80% by volume of the thermally conductive sheet. The content is preferably 45 to 75% by volume. The volume ratio of the thermally conductive filler to the thermally conductive sheet is the sum of the mass of each thermally conductive filler used divided by its density, and the mass of each component of the thermally conductive sheet. It is the ratio of the total value divided by each density.
本発明の熱伝導性シートは、更に、界面活性剤、金属石鹸、難燃剤など公知の物質を使用することができる。本発明の熱伝導性シートが有する熱伝導シートは、多孔体状や発泡体状ではなく、また泡やボイド等の欠陥を含んでいないことが熱伝導の観点で好ましく、密度が２以上あることが好ましい。 The thermally conductive sheet of the present invention may further contain known substances such as surfactants, metal soaps, and flame retardants. The thermally conductive sheet of the present invention preferably does not have a porous or foam shape, and does not contain defects such as bubbles or voids from the viewpoint of heat conduction, and has a density of 2 or more. is preferred.
本発明の熱伝導性シートは好ましくは上記した成分と共に有機溶剤を含有する塗液を離型フィルム上に塗布し、乾燥して熱伝導性シートとする。塗布後には熱伝導性シートの上にまた別の離型フィルムを貼合して使用することが好ましい。離型フィルムとしては、ポリエチレンテレフタレート（ＰＥＴ）フィルムやポリプロピレン（ＰＰ）フィルム、ポリエチレン（ＰＥ）フィルムなど、あるいはその表面にシリコーン離型剤など公知の離型剤を塗布した離型フィルムが例示される。熱伝導性シートを被着物に貼合する場合、片側の離型フィルムを剥離し、圧着することで仮貼合し、更に残る離型フィルムを剥離し、別の被着体を熱伝導性シートに圧着させることでなされる。 The thermally conductive sheet of the present invention is obtained by coating a release film with a coating liquid containing preferably the above-mentioned components and an organic solvent, and drying the coating liquid to obtain a thermally conductive sheet. After coating, it is preferable to use another release film laminated on top of the thermally conductive sheet. Examples of the release film include polyethylene terephthalate (PET) film, polypropylene (PP) film, polyethylene (PE) film, etc., or a release film whose surface is coated with a known release agent such as a silicone release agent. . When laminating a thermally conductive sheet to an adherend, the release film on one side is peeled off and pressure bonded for temporary lamination, the remaining release film is peeled off, and another adherend is attached to the thermally conductive sheet. This is done by crimping the
本発明の熱伝導性シートの厚みは５０～３００μｍであることが好ましく、より好ましくは８０～２５０μｍである。厚みが厚いと熱抵抗が増し、薄いと粘着力が不足する。 The thickness of the thermally conductive sheet of the present invention is preferably 50 to 300 μm, more preferably 80 to 250 μm. If it is thick, the heat resistance will increase, and if it is thin, the adhesive strength will be insufficient.
本発明の熱伝導性シートの熱電伝導率は高いほど好ましいが、１．５Ｗ／ｍ・Ｋ以上であることが好ましく、より好ましくは２Ｗ／ｍ・Ｋ以上であり、更に好ましくは２．５Ｗ／ｍ・Ｋ以上である。また粘着力はやはり強い方が好ましいが、少なくとも３Ｎ／２５ｍｍ以上であることが好ましく、より好ましくは５Ｎ／２５ｍｍ以上であり、更に好ましくは７Ｎ／２５ｍｍ以上である。 The higher the thermoelectric conductivity of the thermally conductive sheet of the present invention is, the more preferable it is, but it is preferably 1.5 W/m·K or more, more preferably 2 W/m·K or more, and even more preferably 2.5 W/m·K. It is more than m.K. Although the adhesive force is preferably strong, it is preferably at least 3 N/25 mm, more preferably 5 N/25 mm, and even more preferably 7 N/25 mm.
以下に本発明を実施例により更に詳細に示し、本発明を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。なお、熱伝導シートにおける各構成成分の含有量を算出するにあたり、各構成成分の比重は以下の値を用いた。酸化亜鉛５．６、無水炭酸マグネシウム２．９６、炭化ケイ素３．２２、アルミナ３．９、酸化マグネシウム３．６、水酸化アルミニウム２．４２、アクリル粘着剤１．１９、酸性リン酸エステル化合物及びリン酸エステル化合物１．８、イソシアネート架橋剤１．０、エポキシ架橋剤１．１８、リン酸トリクレジル１．１６。 EXAMPLES The present invention will be illustrated in more detail by Examples below, and the present invention will be specifically explained, but the present invention is not limited to the following Examples. In addition, in calculating the content of each component in the heat conductive sheet, the following values were used for the specific gravity of each component. Zinc oxide 5.6, anhydrous magnesium carbonate 2.96, silicon carbide 3.22, alumina 3.9, magnesium oxide 3.6, aluminum hydroxide 2.42, acrylic adhesive 1.19, acidic phosphate ester compound and Phosphate ester compound 1.8, isocyanate crosslinker 1.0, epoxy crosslinker 1.18, tricresyl phosphate 1.16.
「熱伝導性フィラーの算術平均粒径測定」
焼結亜鉛華（ハクスイテック（株）製酸化亜鉛）、ＬＰＺＩＮＣ２、ＬＰＺＩＮＣ１１、ＬＰＺＩＮＣ２０、ＬＰＺＩＮＣ３０Ｓ（以上、堺化学工業（株）製酸化亜鉛）、マグサーモＭＳＬ、マグサーモＭＳ－ＰＳ（以上、神島化学工業（株）製無水炭酸マグネシウム）、ＧＣ＃１２００，ＧＣ＃３２０、ＧＣ＃２４０（以上、（株）フジミインコーポレーテッド製炭化ケイ素）、とＡＳ－１０（昭和電工（株）製アルミナ）をそれぞれ純水中に分散し、堀場製作所（株）製ＬＡ－９２０レーザー散乱粒度分布計を使って、算術平均粒径を調べた。結果を表１に示す。
"Arithmetic mean particle size measurement of thermally conductive filler"
Sintered zinc white (zinc oxide manufactured by Hakusui Tech Co., Ltd.), LPZINC2, LPZINC11, LPZINC20, LPZINC30S (zinc oxide manufactured by Sakai Chemical Industry Co., Ltd.), Magthermo MSL, Magthermo MS-PS (all manufactured by Kamishima Chemical Industry Co., Ltd.) ), GC #1200, GC #320, GC #240 (silicon carbide manufactured by Fujimi Inc.), and AS-10 (alumina manufactured by Showa Denko K.K.) in pure water. The arithmetic mean particle size was examined using a Horiba LA-920 laser scattering particle size distribution analyzer. The results are shown in Table 1.
「熱伝導性シート１の作製」
（株）シンキー製攪拌機ＡＲ２５０に下記の熱伝導性シート塗液１を投入し、撹拌モードで１０分間撹拌した。得られた塗液を離型フィルム（アイム（株）製ＲＦ－ＣＳ００１）に乾燥膜厚が１００μｍとなるようそれぞれ塗布し、９０℃で４分間乾燥して、熱伝導性粘着剤層を得た。乾燥後直ちに該粘着剤層表面に離型フィルム（アイム（株）製ＲＦ－ＣＳ００３）を貼合し、熱伝導性シート１を得た。熱伝導性シート１の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
"Preparation of thermally conductive sheet 1"
The following thermally conductive sheet coating liquid 1 was put into a stirrer AR250 manufactured by Shinky Co., Ltd., and stirred for 10 minutes in stirring mode. The resulting coating solution was applied to a release film (RF-CS001 manufactured by Im Co., Ltd.) so that the dry film thickness was 100 μm, and dried at 90° C. for 4 minutes to obtain a thermally conductive adhesive layer. . Immediately after drying, a release film (RF-CS003 manufactured by Im Co., Ltd.) was laminated on the surface of the adhesive layer to obtain a thermally conductive sheet 1. The amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 1.
＜熱伝導性シート塗液１＞
焼結亜鉛華 ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ（日本軽金属（株）製表面処理済水酸化アルミニウム、算術平均粒径４μｍ） ０．６９ｇ
ＫＰ２５６５（日本カーバイド（株）製アクリル粘着剤、固形分４７．５質量％、酸価０ｍｇＫＯＨ／ｇ） １４．０ｇ
ＣＫ１２１５（日本カーバイド（株）製イソシアネート系架橋剤、固形分７５質量％）
０．０３５ｇ
ニッコールＤＤＰ－２（日光ケミカルズ（株）製酸性リン酸エステル化合物）
０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 1>
Sintered zinc white 24.4g
Magthermo MS-PS 3.22g
BF-13STM (surface-treated aluminum hydroxide manufactured by Nippon Light Metal Co., Ltd., arithmetic mean particle size 4 μm) 0.69 g
KP2565 (acrylic adhesive manufactured by Nippon Carbide Co., Ltd., solid content 47.5% by mass, acid value 0mgKOH/g) 14.0g
CK1215 (Isocyanate crosslinking agent manufactured by Nippon Carbide Co., Ltd., solid content 75% by mass)
0.035g
Nikkor DDP-2 (acidic phosphate ester compound manufactured by Nikko Chemicals Co., Ltd.)
0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート２の作製」
下記の熱伝導性シート塗液２を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート２を作製した。なお、熱伝導性シート２の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
"Preparation of thermally conductive sheet 2"
Thermally conductive sheet 2 was produced in the same manner as the thermally conductive sheet 1 except that the following thermally conductive sheet coating liquid 2 was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 2.
＜熱伝導性シート塗液２＞
ＬＰＺＩＮＣ２ ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 2>
LPZINC2 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート３の作製」
下記の熱伝導性シート塗液３を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート３を作製した。なお、熱伝導性シート３の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 3”
A thermally conductive sheet 3 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 3 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 3.
＜熱伝導性シート塗液３＞
ＬＰＺＩＮＣ１１ ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 3>
LPZINC11 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート４の作製」
下記の熱伝導性シート塗液４を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート４を作製した。なお、熱伝導性シート４の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 4”
A thermally conductive sheet 4 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 4 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 4.
＜熱伝導性シート塗液４＞
ＬＰＺＩＮＣ２０ ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 4>
LPZINC20 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート５の作製」
下記の熱伝導性シート塗液５を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート５を作製した。なお、熱伝導性シート５の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 5”
A thermally conductive sheet 5 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 5 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 5.
＜熱伝導性シート塗液５＞
ＬＰＺＩＮＣ３０Ｓ ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 5>
LPZINC30S 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート６の作製」
下記の熱伝導性シート塗液６を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート６を作製した。なお、熱伝導性シート６の全熱伝導性フィラーに対する酸化亜鉛は０体積％、無水炭酸マグネシウムは９５．０体積％である。
“Preparation of thermally conductive sheet 6”
A thermally conductive sheet 6 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 6 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 0% by volume and 95.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 6.
＜熱伝導性シート塗液６＞
マグサーモＭＳ－ＰＳ １６．１１ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 6>
Magthermo MS-PS 16.11g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート７の作製」
下記の熱伝導性シート塗液７を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート７を作製した。なお、熱伝導性シート７の全熱伝導性フィラーに対する酸化亜鉛は０体積％、炭化ケイ素は９５．０体積％である。
“Preparation of thermally conductive sheet 7”
A thermally conductive sheet 7 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 7 described below was used. Incidentally, zinc oxide and silicon carbide were 0% by volume and 95.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 7.
＜熱伝導性シート塗液７＞
ＧＣ＃１２００ １７．５２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 7>
GC#1200 17.52g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート８の作製」
下記の熱伝導性シート塗液８を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート８を作製した。なお、熱伝導性シート８の全熱伝導性フィラーに対する酸化亜鉛は０体積％、アルミナは９５．０体積％である。
“Preparation of thermally conductive sheet 8”
A thermally conductive sheet 8 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 8 described below was used. Note that the amount of zinc oxide and the amount of alumina are 0% by volume and 95.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 8.
＜熱伝導性シート塗液８＞
ＡＳ－１０ ２１．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 8>
AS-10 21.22g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート９の作製」
下記の熱伝導性シート塗液９を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート９を作製した。なお、熱伝導性シート９の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 9”
A thermally conductive sheet 9 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 9 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 9.
＜熱伝導性シート塗液９＞
焼結亜鉛華 ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
オリバイン（登録商標）ＢＰＳ６５７４（トーヨーケム（株）製アクリル粘着剤、酸価１９ｍｇＫＯＨ／ｇ、固形分５７．０質量％） １１．６ｇ
オリバインＢＨＳ８５１５（トーヨーケム（株）製イソシアネート架橋剤、固形分３７．５質量％） ０．０３ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 9>
Sintered zinc white 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
Olivine (registered trademark) BPS6574 (acrylic adhesive manufactured by Toyochem Co., Ltd., acid value 19 mgKOH/g, solid content 57.0% by mass) 11.6 g
Olivine BHS8515 (isocyanate crosslinking agent manufactured by Toyochem Co., Ltd., solid content 37.5% by mass) 0.03g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート１０の作製」
下記の熱伝導性シート塗液１０を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート１０を作製した。なお、熱伝導性シート１０の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 10”
A thermally conductive sheet 10 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 10 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 10.
＜熱伝導性シート塗液１０＞
焼結亜鉛華 ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＬＫＧ１００２（藤倉化成（株）製アクリル粘着剤、酸価２．３ｍｇＫＯＨ／ｇ、固形分３０．０質量％） ２２．１ｇ
１，３－ビス（Ｎ，Ｎ′－ジグリシジルアミノメチル）シクロヘキサン（エポキシ架橋剤） ０．０１ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 10>
Sintered zinc white 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
LKG1002 (acrylic adhesive manufactured by Fujikura Kasei Co., Ltd., acid value 2.3 mgKOH/g, solid content 30.0% by mass) 22.1 g
1,3-bis(N,N'-diglycidylaminomethyl)cyclohexane (epoxy crosslinking agent) 0.01g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート１１の作製」
下記の熱伝導性シート塗液１１を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート１１を作製した。なお、熱伝導性シート１１の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 11”
A thermally conductive sheet 11 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 11 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 11.
＜熱伝導性シート塗液１１＞
焼結亜鉛華 ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＬＫＧ１０１２（藤倉化成（株）製アクリル粘着剤、酸価１．９ｍｇＫＯＨ／ｇ、固形分３０．０質量％） ２２．１ｇ
１，３－ビス（Ｎ，Ｎ′－ジグリシジルアミノメチル）シクロヘキサン（エポキシ架橋剤） ０．０１ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 11>
Sintered zinc white 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
LKG1012 (acrylic adhesive manufactured by Fujikura Kasei Co., Ltd., acid value 1.9 mgKOH/g, solid content 30.0% by mass) 22.1 g
1,3-bis(N,N'-diglycidylaminomethyl)cyclohexane (epoxy crosslinking agent) 0.01g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート１２の作製」
下記の熱伝導性シート塗液１２を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート１２を作製した。なお、熱伝導性シート１２の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 12”
A thermally conductive sheet 12 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 12 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 12.
＜熱伝導性シート塗液１２＞
焼成亜鉛華 ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 12>
Calcined zinc white 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート１３の作製」
下記の熱伝導性シート塗液１３を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート１３を作製した。なお、熱伝導性シート１３の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 13”
A thermally conductive sheet 13 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 13 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 13.
＜熱伝導性シート塗液１３＞
焼成亜鉛華 ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０２ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 13>
Calcined zinc white 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.02g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート１４の作製」
下記の熱伝導性シート塗液１４を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート１４を作製した。なお、熱伝導性シート１４の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 14”
A thermally conductive sheet 14 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 14 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 14.
＜熱伝導性シート塗液１４＞
焼成亜鉛華 ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０４ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 14>
Calcined zinc white 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.04g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート１５の作製」
下記の熱伝導性シート塗液１５を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート１５を作製した。なお、熱伝導性シート１５の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 15”
A thermally conductive sheet 15 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 15 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 15.
＜熱伝導性シート塗液１５＞
焼成亜鉛華 ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．２４ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 15>
Calcined zinc white 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.24g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート１６の作製」
下記の熱伝導性シート塗液１６を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート１６を作製した。なお、熱伝導性シート１６の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 16”
A thermally conductive sheet 16 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 16 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 16.
＜熱伝導性シート塗液１６＞
焼成亜鉛華 ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．３６ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 16>
Calcined zinc white 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.36g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート１７の作製」
下記の熱伝導性シート塗液１７を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート１７を作製した。なお、熱伝導性シート１７の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 17”
A thermally conductive sheet 17 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 17 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 17.
＜熱伝導性シート塗液１７＞
焼成亜鉛華 ２４．４ｇ
マグサーモＭＳ－ＰＳ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＴＤＰ－２（日光ケミカルズ（株）製リン酸エステル化合物）
０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 17>
Calcined zinc white 24.4g
Magthermo MS-PS 3.22g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor TDP-2 (phosphate ester compound manufactured by Nikko Chemicals Co., Ltd.)
0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート１８の作製」
下記の熱伝導性シート塗液１８を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート１８を作製した。なお、熱伝導性シート１８の全熱伝導性フィラーに対する酸化亜鉛は９５．０体積％、無水炭酸マグネシウムは０体積％である。
“Preparation of thermally conductive sheet 18”
A thermally conductive sheet 18 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 18 described below was used. Note that zinc oxide and anhydrous magnesium carbonate were 95.0% by volume and 0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 18.
＜熱伝導性シート塗液１８＞
焼成亜鉛華 ３０．５ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 18>
Calcined zinc white 30.5g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート１９の作製」
下記の熱伝導性シート塗液１９を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート１９を作製した。なお、熱伝導性シート１９の全熱伝導性フィラーに対する酸化亜鉛は８５．６体積％、無水炭酸マグネシウムは９．５体積％である。
“Preparation of thermally conductive sheet 19”
A thermally conductive sheet 19 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 19 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 85.6% by volume and 9.5% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 19.
＜熱伝導性シート塗液１９＞
焼成亜鉛華 ２７．５ｇ
マグサーモＭＳ－ＰＳ １．６１ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 19>
Calcined zinc white 27.5g
Magthermo MS-PS 1.61g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート２０の作製」
下記の熱伝導性シート塗液２０を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート２０を作製した。なお、熱伝導性シート２０の全熱伝導性フィラーに対する酸化亜鉛は６６．５体積％、無水炭酸マグネシウムは２８．５体積％である。
“Preparation of thermally conductive sheet 20”
A thermally conductive sheet 20 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 20 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 66.5% by volume and 28.5% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 20.
＜熱伝導性シート塗液２０＞
焼成亜鉛華 ２１．４ｇ
マグサーモＭＳ－ＰＳ ４．８３ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 20>
Calcined zinc white 21.4g
Magthermo MS-PS 4.83g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート２１の作製」
下記の熱伝導性シート塗液２１を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート２１を作製した。なお、熱伝導性シート２１の全熱伝導性フィラーに対する酸化亜鉛は５７．０体積％、無水炭酸マグネシウムは３８．０体積％である。
“Preparation of thermally conductive sheet 21”
A thermally conductive sheet 21 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 21 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 57.0% by volume and 38.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 21.
＜熱伝導性シート塗液２１＞
焼成亜鉛華 １８．３ｇ
マグサーモＭＳ－ＰＳ ６．４４ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 21>
Calcined zinc white 18.3g
Magthermo MS-PS 6.44g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート２２の作製」
下記の熱伝導性シート塗液２２を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート２２を作製した。なお、熱伝導性シート２２の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 22”
A thermally conductive sheet 22 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 22 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 22.
＜熱伝導性シート塗液２２＞
焼成亜鉛華 ２４．４ｇ
マグサーモＭＳＬ ３．２２ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 22>
Calcined zinc white 24.4g
Magthermo MSL 3.22g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート２３の作製」
下記の熱伝導性シート塗液２３を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート２３を作製した。なお、熱伝導性シート２３の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 23”
A thermally conductive sheet 23 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 23 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 23.
＜熱伝導性シート塗液２３＞
焼成亜鉛華 ２４．４ｇ
ＧＣ＃１２００ ３．５０ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 23>
Calcined zinc white 24.4g
GC#1200 3.50g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート２４の作製」
下記の熱伝導性シート塗液２４を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート２４を作製した。なお、熱伝導性シート２４の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 24”
A thermally conductive sheet 24 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 24 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 24.
＜熱伝導性シート塗液２４＞
焼成亜鉛華 ２４．４ｇ
ＧＣ＃３２０ ３．５０ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 24>
Calcined zinc white 24.4g
GC#320 3.50g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート２５の作製」
下記の熱伝導性シート塗液２５を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート２５を作製した。なお、熱伝導性シート２５の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 25”
A thermally conductive sheet 25 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 25 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 25.
＜熱伝導性シート塗液２５＞
焼成亜鉛華 ２４．４ｇ
ＧＣ＃２４０ ３．５０ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 25>
Calcined zinc white 24.4g
GC#240 3.50g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
「熱伝導性シート２６の作製」
下記の熱伝導性シート塗液２６を用いる以外は熱伝導性シート１と同様にして、熱伝導性シート２６を作製した。なお、熱伝導性シート２６の全熱伝導性フィラーに対する酸化亜鉛は７６．０体積％、無水炭酸マグネシウムは１９．０体積％である。
“Preparation of thermally conductive sheet 26”
A thermally conductive sheet 26 was produced in the same manner as the thermally conductive sheet 1 except that the thermally conductive sheet coating liquid 26 described below was used. Note that the amount of zinc oxide and the amount of anhydrous magnesium carbonate are 76.0% by volume and 19.0% by volume, respectively, based on the total thermally conductive filler of the thermally conductive sheet 26.
＜熱伝導性シート塗液２６＞
焼成亜鉛華 ２４．４ｇ
ＡＳ－１０ ４．２５ｇ
ＢＦ－１３ＳＴＭ ０．６９ｇ
ＫＰ２５６５ １４．０ｇ
ＣＫ１２１５ ０．０３５ｇ
ニッコールＤＤＰ－２ ０．０８ｇ
リン酸トリクレジル ０．３ｇ
酢酸エチルを加えて全量を５５ｇとした。
<Thermal conductive sheet coating liquid 26>
Calcined zinc white 24.4g
AS-10 4.25g
BF-13STM 0.69g
KP2565 14.0g
CK1215 0.035g
Nikkor DDP-2 0.08g
Tricresyl phosphate 0.3g
Ethyl acetate was added to bring the total amount to 55 g.
得られた熱伝導性シート１～２６を下記方法に従い、熱伝導率と粘着力について評価した。結果を表１に示す。 The thermally conductive sheets 1 to 26 obtained were evaluated for thermal conductivity and adhesive strength according to the following method. The results are shown in Table 1.
＜熱伝導率評価＞
塗布直後の熱伝導性シートの一方の離型フィルム（ＲＦ－ＣＳ００１）を剥離し、露出した熱伝導シート表面に７５μｍ厚みルミラー（登録商標）Ｕ３４（東レ（株）製ＰＥＴフィルム）を貼合し、続いて反対面の離型フィルム（ＲＦ－ＣＳ００３）を剥離し、同じくルミラーＵ３４を貼合した。熱伝導率測定装置ａｉ－Ｐｈａｓｅ Ｍｏｂｉｌｅ３（（株）アイフェイズ製）を用いて、厚み方向の熱拡散率を測定した。また熱容量が既知である参照標準物質との比較からサンプルの比熱を算出した。更に別途水上置換法により測定した熱伝導性シートの密度とから、次式により厚み方向の熱伝導率を算出し、表２に記載した。
〔熱伝導率〕＝〔熱拡散率〕×〔密度〕×〔比熱〕
更にルミラーＵ３４貼合済熱伝導性シートを８５℃８５％Ｒ．Ｈ．の環境下で１０日間保管し、保管後に再び熱拡散率を測定して、熱伝導率を算出した。この結果も表２に記載する。
<Thermal conductivity evaluation>
Immediately after coating, the release film (RF-CS001) on one side of the thermally conductive sheet was peeled off, and 75 μm thick Lumirror (registered trademark) U34 (PET film manufactured by Toray Industries, Inc.) was laminated on the exposed surface of the thermally conductive sheet. Then, the release film (RF-CS003) on the opposite side was peeled off, and Lumirror U34 was also bonded thereon. Thermal diffusivity in the thickness direction was measured using a thermal conductivity measuring device ai-Phase Mobile 3 (manufactured by i-Phase Co., Ltd.). In addition, the specific heat of the sample was calculated from comparison with a reference standard material whose heat capacity was known. Furthermore, the thermal conductivity in the thickness direction was calculated using the following formula from the density of the thermally conductive sheet, which was separately measured by a water displacement method, and is listed in Table 2.
[Thermal conductivity] = [Thermal diffusivity] × [Density] × [Specific heat]
Furthermore, the Lumirror U34 laminated thermally conductive sheet was heated at 85°C and 85% R. H. After storage, the thermal diffusivity was measured again to calculate the thermal conductivity. The results are also listed in Table 2.
＜粘着力評価＞
塗布直後の熱伝導性シートと、塗布後５０℃８０％Ｒ．Ｈ．の環境下で４日保管した熱伝導性シートについて、熱伝導性シートの片面の離型フィルム（ＲＦ－ＣＳ００１）を剥離し、０．２ｍｍ厚みのアクリルフィルム（日東樹脂工業（株）製）に貼合し、残る離型フィルムを剥離し、剥離した面に同じ０．２ｍｍ厚みのアクリルフィルムを貼合した。得られた貼合物を幅２５ｍｍに裁断した。得られた試験片の密着強度を剥離機（（株）イマダ製Ｔ字剥離法アタッチメントとフォースゲージＤＳＴの組み合わせ）で測定した。この結果を表２に示す。
<Adhesive strength evaluation>
Thermal conductive sheet immediately after application and 50°C 80% R. H. The release film (RF-CS001) on one side of the thermally conductive sheet was peeled off after being stored for 4 days under the following conditions, and a 0.2mm thick acrylic film (manufactured by Nitto Jushi Kogyo Co., Ltd.) was attached. After lamination, the remaining release film was peeled off, and the same 0.2 mm thick acrylic film was laminated on the peeled surface. The obtained bonded product was cut into a width of 25 mm. The adhesion strength of the obtained test piece was measured using a peeling machine (a combination of a T-shaped peeling attachment manufactured by Imada Co., Ltd. and a force gauge DST). The results are shown in Table 2.
以上の結果から本発明の効果が判る。 The effects of the present invention can be seen from the above results.
Claims (3)
しくは２を表す。） A thermally conductive sheet containing at least zinc oxide and an acrylic adhesive, wherein the zinc oxide has an arithmetic mean particle diameter of 8 μm or more, and the zinc oxide content is 50 to 90% by volume based on the total volume of the thermally conductive filler. A thermally conductive sheet , wherein the acrylic adhesive has an acid value of 2 mgKOH/g or less, and the thermally conductive sheet further contains an acidic phosphate ester compound represented by the following general formula.
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| JP2015071730A (en) | 2013-10-04 | 2015-04-16 | 株式会社トクヤマ | Surface-modified particle |
| JP2016188297A (en) | 2015-03-30 | 2016-11-04 | 日本ゼオン株式会社 | Heat conductive pressure-sensitive adhesive composition, heat conductive pressure-sensitive adhesive sheet-shaped molded product, methods for producing them, and electronic equipment |
| CN108003818A (en) | 2017-12-14 | 2018-05-08 | 深圳市德镒盟电子有限公司 | Low halogen fire retardant pressure sensitive glue of a kind of heat conduction and preparation method thereof |
| WO2019230969A1 (en) | 2018-05-31 | 2019-12-05 | 積水化学工業株式会社 | Heat dissipation composition, heat dissipation member, and filler aggregate for heat dissipation member |
| JP2020015836A (en) | 2018-07-26 | 2020-01-30 | 三菱製紙株式会社 | Thermally conductive sheet |
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