CN111909483A - 一种高导热含硅阻燃树脂组合物及其应用 - Google Patents
一种高导热含硅阻燃树脂组合物及其应用 Download PDFInfo
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- CN111909483A CN111909483A CN202010825201.0A CN202010825201A CN111909483A CN 111909483 A CN111909483 A CN 111909483A CN 202010825201 A CN202010825201 A CN 202010825201A CN 111909483 A CN111909483 A CN 111909483A
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- parts
- resin
- containing flame
- silicon
- resin composition
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 57
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 48
- 239000010703 silicon Substances 0.000 title claims abstract description 48
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000011342 resin composition Substances 0.000 title claims abstract description 37
- 229920005989 resin Polymers 0.000 claims abstract description 86
- 239000011347 resin Substances 0.000 claims abstract description 86
- 239000011256 inorganic filler Substances 0.000 claims abstract description 33
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 33
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 150000002978 peroxides Chemical class 0.000 claims abstract description 24
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 24
- 239000011574 phosphorus Substances 0.000 claims abstract description 24
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 24
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 24
- 239000003999 initiator Substances 0.000 claims abstract description 23
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 21
- 239000003960 organic solvent Substances 0.000 claims abstract description 15
- 229920013638 modified polyphenyl ether Polymers 0.000 claims abstract description 8
- 229920001955 polyphenylene ether Polymers 0.000 claims description 35
- 239000000203 mixture Substances 0.000 claims description 24
- 229910052751 metal Inorganic materials 0.000 claims description 22
- 239000002184 metal Substances 0.000 claims description 22
- 229920002050 silicone resin Polymers 0.000 claims description 20
- 239000011888 foil Substances 0.000 claims description 18
- 239000000126 substance Substances 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 14
- 239000004744 fabric Substances 0.000 claims description 12
- 239000003292 glue Substances 0.000 claims description 12
- 239000000835 fiber Substances 0.000 claims description 11
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- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 6
- AZDCYKCDXXPQIK-UHFFFAOYSA-N ethenoxymethylbenzene Chemical compound C=COCC1=CC=CC=C1 AZDCYKCDXXPQIK-UHFFFAOYSA-N 0.000 claims description 6
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 6
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 5
- BJELTSYBAHKXRW-UHFFFAOYSA-N 2,4,6-triallyloxy-1,3,5-triazine Chemical compound C=CCOC1=NC(OCC=C)=NC(OCC=C)=N1 BJELTSYBAHKXRW-UHFFFAOYSA-N 0.000 claims description 5
- DXIJHCSGLOHNES-UHFFFAOYSA-N 3,3-dimethylbut-1-enylbenzene Chemical compound CC(C)(C)C=CC1=CC=CC=C1 DXIJHCSGLOHNES-UHFFFAOYSA-N 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 5
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
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- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 3
- BSYJHYLAMMJNRC-UHFFFAOYSA-N 2,4,4-trimethylpentan-2-ol Chemical compound CC(C)(C)CC(C)(C)O BSYJHYLAMMJNRC-UHFFFAOYSA-N 0.000 claims description 3
- CARSMBZECAABMO-UHFFFAOYSA-N 3-chloro-2,6-dimethylbenzoic acid Chemical compound CC1=CC=C(Cl)C(C)=C1C(O)=O CARSMBZECAABMO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 3
- 239000011324 bead Substances 0.000 claims description 3
- APOXBWCRUPJDAC-UHFFFAOYSA-N bis(2,6-dimethylphenyl) hydrogen phosphate Chemical compound CC1=CC=CC(C)=C1OP(O)(=O)OC1=C(C)C=CC=C1C APOXBWCRUPJDAC-UHFFFAOYSA-N 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims description 3
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- -1 polysiloxane Polymers 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- ZTFSXSAVDJCOLB-UHFFFAOYSA-N 2-ethylhexanoyl 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOC(=O)C(CC)CCCC ZTFSXSAVDJCOLB-UHFFFAOYSA-N 0.000 claims description 2
- QCXXDZUWBAHYPA-UHFFFAOYSA-N OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.O=C1NC(=O)NC(=O)N1 Chemical compound OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.O=C1NC(=O)NC(=O)N1 QCXXDZUWBAHYPA-UHFFFAOYSA-N 0.000 claims description 2
- 239000011203 carbon fibre reinforced carbon Substances 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 239000007822 coupling agent Substances 0.000 claims description 2
- 125000000524 functional group Chemical group 0.000 claims description 2
- 239000012948 isocyanate Substances 0.000 claims description 2
- 150000002513 isocyanates Chemical class 0.000 claims description 2
- 239000005543 nano-size silicon particle Substances 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 2
- 239000003829 resin cement Substances 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 7
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 15
- 239000011889 copper foil Substances 0.000 description 15
- 238000007731 hot pressing Methods 0.000 description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 8
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- 229920000647 polyepoxide Polymers 0.000 description 3
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
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- 150000002576 ketones Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- GKTNLYAAZKKMTQ-UHFFFAOYSA-N n-[bis(dimethylamino)phosphinimyl]-n-methylmethanamine Chemical group CN(C)P(=N)(N(C)C)N(C)C GKTNLYAAZKKMTQ-UHFFFAOYSA-N 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- PTTPXKJBFFKCEK-UHFFFAOYSA-N 2-Methyl-4-heptanone Chemical compound CC(C)CC(=O)CC(C)C PTTPXKJBFFKCEK-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 239000011190 CEM-3 Substances 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- JUIBLDFFVYKUAC-UHFFFAOYSA-N [5-(2-ethylhexanoylperoxy)-2,5-dimethylhexan-2-yl] 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOC(C)(C)CCC(C)(C)OOC(=O)C(CC)CCCC JUIBLDFFVYKUAC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
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- 239000006185 dispersion Substances 0.000 description 1
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- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/08—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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Abstract
本发明属于复合材料技术领域,涉及一种高导热含硅阻燃树脂组合物及其应用。该树脂组合物具体包括含乙烯基的有机硅树脂、不饱和碳碳双键的改性聚苯醚树脂、过氧化物引发剂、助交联剂、含磷阻燃剂、无机填料以及适量有机溶剂。与现有技术相比,本发明的含硅树脂组合物制备的复合材料具有较高的导热系数、高耐热,以及较低介电常数和介电损耗等优良特性,并且满足无卤阻燃,更加适用于高功率输出使用需求的场所。
Description
技术领域
本发明属于复合材料技术领域,涉及一种高导热含硅阻燃树脂组合物及其应用。
背景技术
随着5G电子信息的飞速发展,电子器件集成技术的发展及电子器件功率也在不断增大,其工作温度也逐渐升高。相比4G,5G的数据量更大、发射频率更大、工作的频段也更高,这需要基站用PCB板有更好的传输性能和散热性能,这意味着5G基站用PCB板要使用更高频率、更高传输速度、耐热性更好的电子基材。因此为了应对市场发展需求,高耐热、高频性、高导热性是未来多年覆铜板性能应提高的主题。
导热有机树脂覆铜板的组成与结构基本相同于通用型覆铜板(FR-4、CEM-3等),只是需要选择导热性能好的基体树脂,复配导热性填充填料,形成高导热复合材料。
专利CN 109206853公开了以环氧树脂为基体树脂,添加改性的氧化铝填料,制备的高导热复合材料的热导率可以达到0.9W/m·K。专利CN 105778506公开了以有机硅树脂为基体的高性能用预浸料、层压板及铝基板。然而上述专利中涉及的树脂组合物都不能同时兼顾导热、热膨胀、耐热、介电常数、介电损耗、阻燃性等综合性能。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种高导热含硅阻燃树脂组合物及其应用。
本发明的目的可以通过以下技术方案来实现:
本发明第一方面提供一种高导热含硅阻燃树脂组合物,包含以下质量份的组分:
含不饱和碳碳双键的改性聚苯醚树脂:16~40份;
乙烯基有机硅树脂:12~25份;
过氧化物引发剂:1~6份;
含磷阻燃剂:5~15份;
助交联剂:5~10份;
无机填料:35~60份。
在本发明的一个实施方式中,所述含不饱和碳碳双键的改性聚苯醚树脂,是指通过在聚苯醚分子中引入含有碳碳双键的官能团结构后,使得聚苯醚具有可交联反应的活性点的树脂;所述含不饱和碳碳双键的改性聚苯醚树脂分子量Mn在1200~6000之间;
进一步地,所述含不饱和碳碳双键的改性聚苯醚树脂选自以下物质中的一种或几种:甲基丙烯酸封端的聚苯醚树脂、烯丙基接枝的聚苯醚树脂或乙烯苄基醚聚苯醚树脂;
进一步地,所述甲基丙烯酸封端的聚苯醚树脂包括Sabic的型号为SA9000的树脂;
进一步地,所述乙烯苄基醚聚苯醚树脂包括三菱瓦斯化学株式会社的型号为OPE-2s的树脂。
更进一步地,所述含不饱和碳碳双键的改性聚苯醚树脂优选Sabic的型号为SA9000的树脂。
在本发明的一个实施方式中,所述乙烯基有机硅树脂是含有乙烯基结构单元的树脂。优选为低R/Si值(1.0-1.5)、Ph/Me(0.6-0.9)的甲基苯基有机硅树脂,进一步优选为R/Si值1.0-1.5、Ph/Me值0.6-0.9的甲基苯基有机硅树脂。
本发明中,所述过氧化物引发剂起到引发交联反应和加速反应速度的效果。
在本发明的一个实施方式中,所述过氧化物引发剂选自以下物质中的一种或几种:过氧化二苯甲酰(BPO)、过氧化二异丙苯(DCP)、过氧苯甲酸叔丁酯、二叔丁基过氧化二异丙苯、2,5-二叔丁基过氧化-2,5-二甲基己烷、叔丁基过氧化氢、2,5-二(2-乙基己酰过氧化)-2,5-二甲基己烷、叔丁基过氧化-3,5,5三甲基己酸酯。优选为过氧化二异丙苯(DCP)。
在本发明的一个实施方式中,所述含磷阻燃剂选自以下物质中的一种或几种的组合:磷腈或改性磷腈、三聚氰胺氰尿酸盐、间苯二酚双[二(2,6-二甲基苯基)磷酸酯]、9,10-二氢-9氧杂-10-磷杂菲-10-氧化物(DOPO)或DOPO含磷聚硅氧烷衍生物系列阻燃剂。
进一步地,所述含磷阻燃剂优选日本大冢化学的磷腈聚合物,牌号为SPB-100。
在本发明的一个实施方式中,所述助交联剂选自以下物质中的一种或几种:三聚氰酸三烯丙酯(TAC)、三烯丙基异三聚氰酸酯(TAIC)、三甲代烯丙基异氰酸酯(TMAIC)、异氰尿酸三丙烯酸酯(THEICTA)、三羟甲基丙烷三丙烯酸酯(TMPTA)、三羟甲基丙烷三甲基丙烯酸酯(TMPTMA)、叔丁基苯乙烯(TBS)或二乙烯基苯(DVB)。优选为三羟甲基丙烷三丙烯酸酯(TMPTA)。
本发明所述无机填料的主要作用在于改善树脂组合物的尺寸稳定性,降低热膨胀率,增加热传导效率等目的。
在本发明的一个实施方式中,所述无机填料选自以下物质中的一种或几种的组合:空心玻璃微珠、二氧化硅、氧化铝、氮化铝、氮化硼、碳化硅、二氧化钛或纳米二氧化硅等。
优选地,所述无机填料的形状可以为球形、片状、不规则形貌的磨碎粉等,优选为球形,粒径中度值0.5~15μm,优选为1~10μm。
优选地,所述无机填料表面经过偶联剂处理,以达到更好的界面结合效果和分散效果。
在本发明的一个实施方式中,在不影响本发明的树脂组合物低介电效果的前提下,可进一步包含以下添加物:硅烷偶联剂。
在含不饱和碳碳双键的改性聚苯醚树脂16~40份、乙烯基有机硅树脂12~25份、过氧化物引发剂1~6份、含磷阻燃剂5~15份、助交联剂5~10份、无机填料35~60份的加入比例下,硅烷偶联剂加入质量份为0.5~2份。
本发明第二方面提供一种树脂胶液,其是将本发明第一方面所述高导热含硅阻燃树脂组合物溶解或分散在有机溶剂中得到。
在组合物中组分以这样的重量份计数:含不饱和碳碳双键的改性聚苯醚树脂:16~40份;乙烯基有机硅树脂:12~25份;过氧化物引发剂:1~6份;含磷阻燃剂:5~15份;助交联剂:5~10份;无机填料:35~60份;
所述有机溶剂的添加量为40~100份。
进一步地,所述有机溶剂选自芳香烃类溶剂、氯代烃类溶剂、环烷烃类溶剂、甲苯、二甲苯、酮类、酯类、二甲基甲酰胺或双异丁基酮中的至少一种或几种。
更进一步地,所述有机溶剂优选为甲苯。
本发明第三方面提供一种半固化片,将纤维织物增强材料浸渍本发明第二方面所述树脂胶液后,在80~150℃下烘烤2~10min后得到。
具体的,经过短时间的加热除去溶剂,得到低溶剂或无溶剂的半固化片。
加热温度和时间根据所选溶剂种类调整,优选为90~130℃,时间优选为4~7min,时间过长容易导致引发剂的分解消耗,半固化片过度交联;时间过短则无法有效除去溶剂。
本发明第四方面提供一种层压板,该层压板是由金属箔与所述半固化片热压而成。
具体而言,将至少1片以上半固化片叠在一起,上下表面放置金属箔,在一定压力和温度条件下热压得到双面覆金属箔的层压板。
所述的金属箔可为本领域任意常用金属箔,优选铜箔。
还可以进一步对铜箔表面进行镀锌或者锌合金,以增加其与半固化片的结合力。
进一步地,上述层压板可以通过进一步的线路蚀刻工艺得到印刷线路板。
本发明中,有机硅树脂是一类具有一定交联结构的热固性聚硅氧烷树脂,整个分子以Si-O-Si键骨架结构为主,硅原子上连接有机基团的半无机高聚物,导热性优于环氧树脂,热稳定高,尺寸稳定性好。其有机基团可根据材料性能要求进行人为的设计和修饰,由此赋予有机硅树脂优异的物理和化学性能。
乙烯基有机硅树脂与含不饱和碳碳双键的改性聚苯醚树脂可以在过氧化物的反应下,发生化学交联而形成热固性树脂。该树脂的导热性比环氧树脂要好,同时具有较高的耐热性、尺寸稳定性佳,较低的介电常数和介电损耗等优势,尤其适用于高频高功率的信号传输设备中。
与现有技术相比,本发明的含硅树脂组合物制备的复合材料具有较高的导热系数、高耐热,以及较低介电常数和介电损耗等优良特性,并且满足无卤阻燃,更加适用于高功率输出使用需求的场所。基于本发明的半固化片、层压板、多层印刷线路板具有高导热、高耐热、无卤阻燃、低吸水率以及高频低介电等优良特性,特别适用于高功率无卤阻燃的5G基站所要求的线路板基材。
具体实施方式
下面结合具体实施例对本发明进行详细说明。
实施例1-9
高导热含硅阻燃树脂组合物的制备
按照表1和表2列出的配方,首先将树脂组分和无机填料在甲苯中混合分散,得到树脂组合物,实施例1-9分别对应表1中组分1-9。接着以该组合物浸渍1078玻纤布(宏和电子),在115℃条件下加热干燥6min得到树脂含量为65%-68%的半固化片。
分别将5片半固化片叠在一起,将2张厚度35微米的铜箔分别置于上下表面,在220℃和4MPa的压力条件下热压120min得到双面覆铜的层压板。
通过蚀刻的方法将铜箔除去,用于评价介电常数,介电损耗,导热性能,玻璃化转变温度,热膨胀系数,阻燃性等。
下列实施例中使用的化学品名如下:
SA9000:末端甲基聚丙烯酸酯的双酚A聚苯醚树脂,Sabic公司;
DC2105:有机硅树脂,Dow Corning;
KRF266:有机硅树脂,日本信越化学
SPB-100:磷腈聚合物,大冢化学;
DCP:过氧化二异丙苯,上海高桥;
TMPTA:国药集团化学试剂有限公司;
ZH-H:导热无机填料(纳米氧化铝),合肥中航纳米技术发展有限公司;
A-171:乙烯基硅烷偶联剂,迈图高新材料(中国)有限公司。
下列实施例中的测试方法:
导热系数:参照ASTM 5470测试,50℃,W/(m·K);
玻璃化转变温度(Tg):参照IPC-TM-6502.4.24测试;
热膨胀系数测试(CTE):参照标准IPC-TM-650 2.4.24.5规范;
耐热性T28:参照标准IPC-TM-650 2.4.24.1方法,使用6.5mm×6.5mm的层压板,在288℃的温度下,测试层压板不发生爆板的时间;
介电常数和介电损耗:按照SPDR测试,10GHz;
阻燃性测试:根据UL94规范的方法测试。
表1高导热含硅阻燃树脂组合物配方表(单位:质量份)
表2高导热含硅阻燃树脂组合物性能测试(单位:质量份)
从表中实施例1-9的物性数据可以看出,有机硅树脂含量增多有助于导热系数的提高,同时导热无机填料的增多有利于导热系数的提高,但会对介电常数与介电损耗有不利影响。有机硅树脂含量在一定程度下会降低阻燃性,但是通过适当提高阻燃剂含量可以满足阻燃使用要求,但是不会对耐热性能有任何不良影响。
实施例10
一种高导热含硅阻燃树脂组合物,包含以下质量份的组分:
含不饱和碳碳双键的改性聚苯醚树脂:16份;
乙烯基有机硅树脂:12份;
过氧化物引发剂:1份;
含磷阻燃剂:5份;
助交联剂:5份;
无机填料:35份。
本实施例中,所述含不饱和碳碳双键的改性聚苯醚树脂选自:烯丙基接枝的聚苯醚树脂;
本实施例中,所述乙烯基有机硅树脂为甲基苯基有机硅树脂,其R/Si在1.0-1.5之间,Ph/Me值0.6-0.9之间。
本实施例中,所述过氧化物引发剂选自以下物质:过氧化二苯甲酰(BPO)。
本实施例中,所述含磷阻燃剂选自以下物质:磷腈或改性磷腈。
本实施例中,所述助交联剂选自以下物质:三聚氰酸三烯丙酯(TAC)。
本实施例中,所述无机填料选自以下物质:空心玻璃微珠。
本实施例中,所述无机填料的形状为球形,粒径中度值0.5μm。
本实施例还提供一种树脂胶液,其是将所述高导热含硅阻燃树脂组合物溶解或分散在有机溶剂(芳香烃类溶剂)中得到。
在组合物中组分以这样的重量份计数:含不饱和碳碳双键的改性聚苯醚树脂:16份;乙烯基有机硅树脂:12份;过氧化物引发剂:1份;含磷阻燃剂:5份;助交联剂:5份;无机填料:35份;
所述有机溶剂的添加量为40份。
本实施例还提供一种半固化片,将纤维织物增强材料浸渍所述树脂胶液后,在80℃下烘烤10min后得到。
本实施例还提供一种层压板,该层压板是由金属箔与所述半固化片热压而成,具体而言,将至少1片以上半固化片叠在一起,上下表面放置金属箔,在一定压力和温度条件下热压得到双面覆金属箔的层压板,层压板可以通过进一步的线路蚀刻工艺得到印刷线路板。
本实施例中,所述金属箔选择铜箔。
实施例11
一种高导热含硅阻燃树脂组合物,包含以下质量份的组分:
含不饱和碳碳双键的改性聚苯醚树脂:40份;
乙烯基有机硅树脂:25份;
过氧化物引发剂:6份;
含磷阻燃剂:15份;
助交联剂:10份;
无机填料:60份。
本实施例中,所述含不饱和碳碳双键的改性聚苯醚树脂选自:乙烯苄基醚聚苯醚树脂(三菱瓦斯化学株式会社的型号为OPE-2s的树脂);
本实施例中,所述乙烯基有机硅树脂为甲基苯基有机硅树脂,其R/Si在1.0-1.5之间,Ph/Me值在0.6-0.9之间。
本实施例中,所述过氧化物引发剂选自以下物质:二叔丁基过氧化二异丙苯。
本实施例中,所述含磷阻燃剂选自以下物质:三聚氰胺氰尿酸盐。
本实施例中,所述助交联剂选自以下物质:三烯丙基异三聚氰酸酯(TAIC)。
本实施例中,所述无机填料选自以下物质:氮化硼。
本实施例中,所述无机填料的形状为球状,粒径中度值15μm。
本实施例中,高导热含硅阻燃树脂组合物还包含以下添加物:硅烷偶联剂,硅烷偶联剂加入质量份为0.5份。
本实施例还提供一种树脂胶液,其是将所述高导热含硅阻燃树脂组合物溶解或分散在有机溶剂(氯代烃类溶剂)中得到。
在组合物中组分以这样的重量份计数:含不饱和碳碳双键的改性聚苯醚树脂:40份;乙烯基有机硅树脂:25份;过氧化物引发剂:6份;含磷阻燃剂:15份;助交联剂:10份;无机填料:60份;
所述有机溶剂的添加量为100份。
本实施例还提供一种半固化片,将纤维织物增强材料浸渍所述树脂胶液后,在150℃下烘烤2min后得到。
本实施例还提供一种层压板,该层压板是由金属箔与所述半固化片热压而成,具体而言,将至少1片以上半固化片叠在一起,上下表面放置金属箔,在一定压力和温度条件下热压得到双面覆金属箔的层压板,层压板可以通过进一步的线路蚀刻工艺得到印刷线路板。
本实施例中,所述金属箔选择铜箔。
本实施例中,还进一步对铜箔表面进行镀锌或者锌合金,以增加其与半固化片的结合力。
实施例12
一种高导热含硅阻燃树脂组合物,包含以下质量份的组分:
含不饱和碳碳双键的改性聚苯醚树脂:28份;
乙烯基有机硅树脂:18份;
过氧化物引发剂:4份;
含磷阻燃剂:10份;
助交联剂:8份;
无机填料:48份。
本实施例中,所述含不饱和碳碳双键的改性聚苯醚树脂选自:乙烯苄基醚聚苯醚树脂(三菱瓦斯化学株式会社的型号为OPE-2s的树脂);
本实施例中,所述乙烯基有机硅树脂为甲基苯基有机硅树脂,其R/Si在1.0-1.5之间,Ph/Me值在0.6-0.9之间。
本实施例中,所述过氧化物引发剂选自以下物质:2,5-二(2-乙基己酰过氧化)-2,5-二甲基己烷。
本实施例中,所述含磷阻燃剂选自以下物质:间苯二酚双[二(2,6-二甲基苯基)磷酸酯]。
本实施例中,所述助交联剂选自以下物质:异氰尿酸三丙烯酸酯(THEICTA)。
本实施例中,所述无机填料选自以下物质中的一种或几种的组合:碳化硅。
本实施例中,所述无机填料的形状为球形,粒径中度值5μm。
本实施例中,高导热含硅阻燃树脂组合物还包含以下添加物:硅烷偶联剂,硅烷偶联剂加入质量份为2份。
本实施例还提供一种树脂胶液,其是将所述高导热含硅阻燃树脂组合物溶解或分散在有机溶剂(环烷烃类溶剂)中得到。
在组合物中组分以这样的重量份计数:含不饱和碳碳双键的改性聚苯醚树脂28份、乙烯基有机硅树脂18份、过氧化物引发剂4份、含磷阻燃剂10份、助交联剂8份、无机填料48份。
所述有机溶剂的添加量为70份。
本实施例还提供一种半固化片,将纤维织物增强材料浸渍所述树脂胶液后,在110℃下烘烤5min后得到。
本实施例还提供一种层压板,该层压板是由金属箔与所述半固化片热压而成,具体而言,将至少1片以上半固化片叠在一起,上下表面放置金属箔,在一定压力和温度条件下热压得到双面覆金属箔的层压板,层压板可以通过进一步的线路蚀刻工艺得到印刷线路板。
本实施例中,所述金属箔选择铜箔。
本实施例中,还进一步对铜箔表面进行镀锌或者锌合金,以增加其与半固化片的结合力。
实施例13
一种高导热含硅阻燃树脂组合物,包含以下质量份的组分:
含不饱和碳碳双键的改性聚苯醚树脂:30份;
乙烯基有机硅树脂:16份;
过氧化物引发剂:4份;
含磷阻燃剂:8份;
助交联剂:6份;
无机填料:40份。
本实施例中,所述含不饱和碳碳双键的改性聚苯醚树脂选自:乙烯苄基醚聚苯醚树脂(三菱瓦斯化学株式会社的型号为OPE-2s的树脂);
本实施例中,所述乙烯基有机硅树脂为甲基苯基有机硅树脂,其R/Si在1.0-1.5之间,Ph/Me值在0.6-0.9之间。
本实施例中,所述过氧化物引发剂选自以下物质:叔丁基过氧化-3,5,5三甲基己酸酯。
本实施例中,所述含磷阻燃剂选自以下物质:9,10-二氢-9氧杂-10-磷杂菲-10-氧化物(DOPO)。
本实施例中,所述助交联剂选自以下物质:叔丁基苯乙烯(TBS)。
本实施例中,所述无机填料选自以下物质:二氧化钛。
本实施例中,所述无机填料的形状为片状。
本实施例中,高导热含硅阻燃树脂组合物还包含以下添加物:硅烷偶联剂,硅烷偶联剂加入质量份为1份。
本实施例还提供一种树脂胶液,其是将所述高导热含硅阻燃树脂组合物溶解或分散在有机溶剂(酮类)中得到。
在组合物中组分以这样的重量份计数:含不饱和碳碳双键的改性聚苯醚树脂30份、乙烯基有机硅树脂16份、过氧化物引发剂4份、含磷阻燃剂8份、助交联剂6份、无机填料40份。
所述有机溶剂的添加量为58份。
本实施例还提供一种半固化片,将纤维织物增强材料浸渍所述树脂胶液后,在90℃下烘烤7min后得到。
本实施例还提供一种层压板,该层压板是由金属箔与所述半固化片热压而成,具体而言,将至少1片以上半固化片叠在一起,上下表面放置金属箔,在一定压力和温度条件下热压得到双面覆金属箔的层压板,层压板可以通过进一步的线路蚀刻工艺得到印刷线路板。
本实施例中,所述金属箔选择铜箔。
本实施例中,还进一步对铜箔表面进行镀锌或者锌合金,以增加其与半固化片的结合力。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和使用发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改,并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此,本发明不限于上述实施例,本领域技术人员根据本发明的揭示,不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。
Claims (11)
1.一种高导热含硅阻燃树脂组合物,其特征在于,包含以下质量份的组分:
含不饱和碳碳双键的改性聚苯醚树脂:16~40份;
乙烯基有机硅树脂:12~25份;
过氧化物引发剂:1~6份;
含磷阻燃剂:5~15份;
助交联剂:5~10份;
无机填料:35~60份。
2.根据权利要求1所述高导热含硅阻燃树脂组合物,其特征在于,所述含不饱和碳碳双键的改性聚苯醚树脂,是指通过在聚苯醚分子中引入含有碳碳双键的官能团结构后,使得聚苯醚具有可交联反应的活性点的树脂;所述含不饱和碳碳双键的改性聚苯醚树脂分子量Mn在1200~6000之间;
进一步地,所述含不饱和碳碳双键的改性聚苯醚树脂选自以下物质中的一种或几种:甲基丙烯酸封端的聚苯醚树脂、烯丙基接枝的聚苯醚树脂或乙烯苄基醚聚苯醚树脂。
3.根据权利要求1所述高导热含硅阻燃树脂组合物,其特征在于,所述乙烯基有机硅树脂是含有乙烯基结构单元的树脂;
优选为R/Si值1.0-1.5、Ph/Me值0.6-0.9的甲基苯基有机硅树脂。
4.根据权利要求1所述高导热含硅阻燃树脂组合物,其特征在于,所述过氧化物引发剂选自以下物质中的一种或几种:过氧化二苯甲酰、过氧化二异丙苯、过氧苯甲酸叔丁酯、二叔丁基过氧化二异丙苯、2,5-二叔丁基过氧化-2,5-二甲基己烷、叔丁基过氧化氢、2,5-二(2-乙基己酰过氧化)-2,5-二甲基己烷、叔丁基过氧化-3,5,5三甲基己酸酯;优选为过氧化二异丙苯。
5.根据权利要求1所述高导热含硅阻燃树脂组合物,其特征在于,所述含磷阻燃剂选自以下物质中的一种或几种的组合:磷腈或改性磷腈、三聚氰胺氰尿酸盐、间苯二酚双[二(2,6-二甲基苯基)磷酸酯]、9,10-二氢-9氧杂-10-磷杂菲-10-氧化物(DOPO)或DOPO含磷聚硅氧烷衍生物系列阻燃剂。
6.根据权利要求1所述高导热含硅阻燃树脂组合物,其特征在于,所述助交联剂选自以下物质中的一种或几种:三聚氰酸三烯丙酯、三烯丙基异三聚氰酸酯、三甲代烯丙基异氰酸酯、异氰尿酸三丙烯酸酯、三羟甲基丙烷三丙烯酸酯、三羟甲基丙烷三甲基丙烯酸酯、叔丁基苯乙烯或二乙烯基苯;优选为三羟甲基丙烷三丙烯酸酯。
7.根据权利要求1所述高导热含硅阻燃树脂组合物,其特征在于,所述无机填料选自以下物质中的一种或几种的组合:空心玻璃微珠、二氧化硅、氧化铝、氮化铝、氮化硼、碳化硅、二氧化钛或纳米二氧化硅;
优选地,所述无机填料表面经过偶联剂处理。
8.根据权利要求1-7中任一项所述高导热含硅阻燃树脂组合物,其特征在于,还包含以下添加物:硅烷偶联剂;
在含不饱和碳碳双键的改性聚苯醚树脂16~40份、乙烯基有机硅树脂12~25份、过氧化物引发剂1~6份、含磷阻燃剂5~15份、助交联剂5~10份、无机填料35~60份的加入比例下,硅烷偶联剂加入质量份为0.5~2份。
9.一种树脂胶液,其特征在于,其是将如权利要求1-7中任一项所述高导热含硅阻燃树脂组合物溶解或分散在有机溶剂中得到:
在组合物中组分以这样的重量份计数:含不饱和碳碳双键的改性聚苯醚树脂:16~40份;乙烯基有机硅树脂:12~25份;过氧化物引发剂:1~6份;含磷阻燃剂:5~15份;助交联剂:5~10份;无机填料:35~60份;
所述有机溶剂的添加量为40~100份。
10.一种半固化片,其特征在于,其是将纤维织物增强材料浸渍如权利要求9所述的树脂胶液后,在80~150℃下烘烤2~10min后得到。
11.一种层压板,其特征在于,包含至少一片以上如权利要求10所述的半固化片,与金属箔进行热压成型制备所得。
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CN115433397B (zh) * | 2022-08-26 | 2023-08-11 | 上海材料研究所有限公司 | 一种低介电常数的树脂组合物及其应用 |
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