CN116285378A - 一种树脂组合物及包含其的粘结片、覆金属箔层压板 - Google Patents
一种树脂组合物及包含其的粘结片、覆金属箔层压板 Download PDFInfo
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- CN116285378A CN116285378A CN202111563188.7A CN202111563188A CN116285378A CN 116285378 A CN116285378 A CN 116285378A CN 202111563188 A CN202111563188 A CN 202111563188A CN 116285378 A CN116285378 A CN 116285378A
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- 239000011342 resin composition Substances 0.000 title claims abstract description 68
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 39
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- 229920000642 polymer Polymers 0.000 claims abstract description 63
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 50
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000010703 silicon Substances 0.000 claims abstract description 43
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- -1 divinyl aromatic compound Chemical class 0.000 claims description 25
- MYRTYDVEIRVNKP-UHFFFAOYSA-N divinylbenzene Substances C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 22
- 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 claims description 20
- 239000003063 flame retardant Substances 0.000 claims description 20
- 239000011256 inorganic filler Substances 0.000 claims description 18
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 18
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000003431 cross linking reagent Substances 0.000 claims description 12
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- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 11
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- 150000001875 compounds Chemical class 0.000 claims description 10
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 10
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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 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229920006158 high molecular weight polymer Polymers 0.000 claims description 7
- 239000011889 copper foil Substances 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
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- 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 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
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- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
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- 125000002947 alkylene group Chemical group 0.000 claims description 4
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 claims description 4
- NIHNNTQXNPWCJQ-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 claims description 4
- 150000002978 peroxides Chemical class 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 125000005913 (C3-C6) cycloalkyl group Chemical group 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 3
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- HGTUJZTUQFXBIH-UHFFFAOYSA-N (2,3-dimethyl-3-phenylbutan-2-yl)benzene Chemical group C=1C=CC=CC=1C(C)(C)C(C)(C)C1=CC=CC=C1 HGTUJZTUQFXBIH-UHFFFAOYSA-N 0.000 claims description 2
- KDGNCLDCOVTOCS-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy propan-2-yl carbonate Chemical compound CC(C)OC(=O)OOC(C)(C)C KDGNCLDCOVTOCS-UHFFFAOYSA-N 0.000 claims description 2
- XSZYESUNPWGWFQ-UHFFFAOYSA-N 1-(2-hydroperoxypropan-2-yl)-4-methylcyclohexane Chemical compound CC1CCC(C(C)(C)OO)CC1 XSZYESUNPWGWFQ-UHFFFAOYSA-N 0.000 claims description 2
- 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 2
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 2
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 claims description 2
- BWOITHKYQUJGSB-UHFFFAOYSA-N 2-methylbutan-2-ylperoxycyclohexane Chemical compound CCC(C)(C)OOC1CCCCC1 BWOITHKYQUJGSB-UHFFFAOYSA-N 0.000 claims description 2
- BIISIZOQPWZPPS-UHFFFAOYSA-N 2-tert-butylperoxypropan-2-ylbenzene Chemical compound CC(C)(C)OOC(C)(C)C1=CC=CC=C1 BIISIZOQPWZPPS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 claims description 2
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004641 Diallyl-phthalate Substances 0.000 claims description 2
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229940118662 aluminum carbonate Drugs 0.000 claims description 2
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 claims description 2
- 150000001491 aromatic compounds Chemical class 0.000 claims description 2
- 125000000732 arylene group Chemical group 0.000 claims description 2
- 125000000751 azo group Chemical group [*]N=N[*] 0.000 claims description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 2
- 229910002113 barium titanate Inorganic materials 0.000 claims description 2
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- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 claims description 2
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 239000000378 calcium silicate Substances 0.000 claims description 2
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 2
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 claims description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
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- SPTHWAJJMLCAQF-UHFFFAOYSA-M ctk4f8481 Chemical compound [O-]O.CC(C)C1=CC=CC=C1C(C)C SPTHWAJJMLCAQF-UHFFFAOYSA-M 0.000 claims description 2
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 2
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- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 2
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
本发明提供一种树脂组合物及包含其的粘结片、覆金属箔层压板,所述树脂组合物以重量份计包括如下组分:以硅芳炔树脂和多官能乙烯基芳香族聚合物的重量份之和为100份计,硅芳炔树脂5~95份,多官能乙烯基芳香族聚合物5~95份。所述树脂组合物通过特定聚合物的复配,显著提升了加工性,固化物具有高模量、优异的介电性能和耐热性,而且热膨胀比例低,阻燃性、尺寸稳定性和粘结性能好。包含所述树脂组合物的覆金属箔层压板板材表观平整均匀,具有优异的加工性、耐热性和尺寸稳定性,且剥离强度高、介电常数和介电损耗因数低,能够充分满足高频电路基板在加工和应用性能方面的要求。
Description
技术领域
本发明属于覆铜板技术领域,具体涉及一种树脂组合物及包含其的粘结片、覆金属箔层压板。
背景技术
随着电子设备向小型化、多功能化和高性能化方面的迅速发展,要求电子材料和电子元器件具有高精度、高密度、高性能、薄型化和多层化的性能。印制电路板(PrintedCircuit Board,PCB)是电子工业的重要部件之一,是实现电子设备中电气互连的不可或缺的基础材料。覆金属箔层压板是制备PCB的基层压料板,其在整个PCB中担负有导电、绝缘和支撑三个方面的功能。PCB的性能、品质、加工性、制造成本以及长期可靠性,在很大程度上取决于覆金属箔层压板的性能水平。
覆金属箔层压板是将玻璃纤维布等增强材料浸以树脂胶液,然后在一面或两面覆以金属箔并热压而成的板材。目前应用比较广泛的树脂胶液为环氧树脂体系,环氧树脂固化物的耐热性和绝缘性良好,且具有较好的加工性与成本优势。但是,环氧树脂本身的介电常数和介电损耗偏高,且固化后会产生大量的二次羟基,容易在使用过程中吸水,吸水率上升导致材料的介电性能和耐湿热性能下降,难以满足高性能PCB的使用要求。
聚烯烃树脂又称碳氢树脂,具有良好的介电性能,能够满足覆金属箔层压板在低介电常数和低介质损耗方面的要求,因此在层压板中的使用日益广泛;但是,烯烃聚合物以脂肪族碳链为主,其柔性和非极性碳链的结构导致聚烯烃树脂的固化物刚性不足,强度偏低,耐热性和粘接性能不理想,因此难以单独使用,通过需要将聚烯烃树脂与其他聚合物进行搭配使用。
CN111825943A公开了一种碳氢覆铜板用树脂组合物,包括以下重量份原料:聚丁二烯20~40份,腈基树脂和改性马来酰亚胺树脂的混合物10~20份,陶瓷粉和火山灰的混合物25~45份,聚二烯烃-苯乙烯-乙烯三元共聚物15~40份,交联剂8~12份,固化剂4~6份;该碳氢覆铜板用树脂组合物制成的覆铜板具有介电常数可控、低介电损耗、剥离强度高和耐热性好等优点。然而,腈基树脂和改性马来酰亚胺树脂与聚烯烃树脂的相容性不好,在胶水混制过程中容易发生分层或分相的问题,给实际加工过程带来阻碍,而且还会影响板材的表观均匀性。
CN108676209A公开了一种碳氢聚合物覆铜板组合物,该组合物以重量份计包括:聚丁二烯20~40重量份、苯乙烯-乙烯嵌段共聚物15~30重量份、聚苯醚15~25重量份、交联剂5~10重量份、固化剂3~5重量份和无机填料20~40重量份,用所述组合物制成的覆铜板具有较低的介电常数和介质损耗。CN106379006A公开了一种高频覆铜板,包括绝缘层和设置于绝缘层单面或双面的金属箔,绝缘层包括树脂组合物和增强材料(玻璃布或玻纤纸),树脂组合物包括丁苯树脂、聚丁二烯树脂、交联剂和引发剂;该高频覆铜板具有耐热性好、介电损耗小等性能,可满足高频板材的性能要求。但是,以上述树脂组合物为代表的聚烯烃体系中,引发剂或固化剂的分解温度一般都≤150℃,导致聚丁二烯树脂等烯烃聚合物都在较低的温度下即发生交联反应,树脂粘度过高,不利于层压粘合等加工,为粘结片和覆金属箔层压板的工艺制程带来了很大的难度。
因此,开发一种兼具优异的加工性、介电性能、耐热性和力学性能的树脂材料,以满足覆金属箔层压板的加工及性能要求,是本领域的研究重点。
发明内容
针对现有技术的不足,本发明的目的在于提供一种树脂组合物及包含其的粘结片、覆金属箔层压板,通过硅芳炔树脂和多官能乙烯基芳香族聚合物的组分复配,使所述树脂组合物的加工性显著提升,其固化物具有高模量、优异的介电性能、耐热性和尺寸稳定性,能够充分满足高频印制电路板在加工性和应用性能方面的需求。
为达此目的,本发明采用以下技术方案:
第一方面,本发明提供一种树脂组合物,所述树脂组合物以重量份计包括如下组分:以硅芳炔树脂和多官能乙烯基芳香族聚合物的重量份之和为100份计,硅芳炔树脂5~95份,多官能乙烯基芳香族聚合物5~95份;所述多官能乙烯基芳香族聚合物由二乙烯基芳香族化合物和其他乙烯基化合物共聚而成,且二乙烯基芳香族化合物在共聚物的重复单元中的摩尔占比大于等于15%。
本发明提供的树脂组合物包括硅芳炔树脂和多官能乙烯基芳香族聚合物的组合,所述硅芳炔树脂在固化反应前的熔融粘度很低,能够显著改善多官能乙烯基芳香族聚合物在固化过程中的加工性;二者以特定比例协同复配,使所述树脂组合物的加工性优异,且固化物具有高模量、优异的介电性能和耐热性,而且热膨胀比例低,阻燃性、尺寸稳定性和粘结性能好,充分满足了印制电路板对于树脂组合物的性能要求。
本发明提供的树脂组合物中,所述硅芳炔树脂为5~95份,例如6份、8份、10份、12份、15份、18份、20份、22份、25份、28份、30份、32份、35份、38份、40份、42份、45份、48份、50份、52份、55份、58份、60份、65份、70份、75份、80份、85份、90份或92份等。
所述多官能乙烯基芳香族聚合物为5~95份,例如8份、10份、15份、20份、25份、30份、35份、40份、42份、45份、48份、50份、52份、55份、58份、60份、62份、65份、68份、70份、72份、75份、78份、80份、82份、85份、88份、90份、92份或94份等。
本发明中,所述硅芳炔树脂具有如式I所示结构:
式I中,n选自1~50的整数,例如1、2、3、4、5、8、10、15、18、21、25、27、30、35、38、40、43、45、48或50等。
式I中,R1、R2各自独立地选自氢、C1~C6直链或支链烷基、C3~C6环烷基。
所述C1~C6直链或支链烷基可以为C1、C2、C3、C4、C5或C6的直链或支链烷基,示例性地包括但不限于:甲基、乙基、正丙基、异丙基、正丁基、异丁基、叔丁基、正戊基、新戊基、异戊基或正己基等。
所述C3~C6环烷基可以为C3、C4、C5或C6的环烷基,示例性地包括但不限于:环丙基、环丁基、环戊基或环己基等。
M选自单键、O、SO2、C1~C5直链或支链亚烷基;所述“M为单键”意指两个苯环通过单键直接相连形成联苯结构。
R3、R4各自独立地选自卤素(例如氟、氯、溴或碘)、C1~C5(例如C1、C2、C3、C4或C5)直链或支链烷基。
m1、m3各自独立地选自0~4的整数,例如0、1、2、3或4。
m2选自0~6的整数,例如0、1、2、3、4、5或6。
优选地,所述R1、R2各自独立地选自C1~C5(例如C1、C2、C3、C4或C5)直链或支链烷基,示例性地包括但不限于:甲基、乙基、正丙基、异丙基、正丁基、异丁基、叔丁基、正戊基、新戊基或异戊基等。
优选地,所述硅芳炔树脂的数均分子量为200~8000,例如300、500、800、1000、1200、1500、1800、2000、2200、2500、2800、3000、3200、3500、3800、4000、4500、5000、5500、6000、6500、7000、7500或7800等,进一步优选为400~4000,更进一步优选为500~3500。
本发明中,分子量(数均分子量、重均分子量等)的测试方法为GB/T21863-2008,以聚苯乙烯校准为基础通过凝胶渗透色谱法(GPC)测定得到。
本发明中,所述硅芳炔树脂可通过芳炔化合物HC≡C-Ar-C≡CH和硅烷化合物反应得到;其中,R1、R2、Ar具有与式I中相同的限定范围,X1、X2各自独立地选自卤素,优选为氯、溴或碘;所述反应在格氏试剂存在下进行。
所述多官能乙烯基芳香族聚合物由二乙烯基芳香族化合物和其他乙烯基化合物共聚而成,且二乙烯基芳香族化合物在共聚物的重复单元中的摩尔占比大于等于15%,例如可以为20%、25%、30%、35%、40%、45%、50%、55%、60%、65%、70%、75%、80%、85%或90%等,上限至90%。示例性地,多官能乙烯基芳香族聚合物市售商品可以选自新日铁的ODV。
优选地,所述二乙烯基芳香族化合物包括二乙烯基苯、二乙烯基联苯、二乙烯基萘、二异丙烯基苯、二异丙烯基萘和二异丙烯基联苯中的任意一种或至少两种的组合。本发明中,上述列举的二乙烯基芳香族化合物包括其所有的同分异构体。
其中,所述二乙烯基苯包括邻二乙烯基苯、间二乙烯基苯或对二乙烯基苯中的任意一种或至少两种的组合。
所述二乙烯基联苯包括4,4'-二乙烯基联苯、4,3'-二乙烯基联苯、4,2'-二乙烯基联苯、3,2'-二乙烯基联苯、3,3'-二乙烯基联苯、2,2'-二乙烯基联苯或2,4-二乙烯基联苯中的任意一种或至少两种的组合。
所述二乙烯基萘包括1,3-二乙烯基萘、1,4-二乙烯基萘、1,5-二乙烯基萘、1,8-二乙烯基萘、2,3-二乙烯基萘、2,6-二乙烯基萘或2,7-二乙烯基萘中的任意一种或至少两种的组合。
所述二异丙烯基苯包括1,2-二异丙烯基苯、1,3-二异丙烯基苯或1,4-二异丙烯基苯中的任意一种或至少两种的组合。
所述二异丙烯基萘包括1,3-二异丙烯基萘、1,4-二异丙烯基萘、1,5-二异丙烯基萘、1,8-二异丙烯基萘、2,3-二异丙烯基萘、2,6-二异丙烯基萘或2,7-二异丙烯基萘中的任意一种或至少两种的组合。
所述二异丙烯基联苯包括4,4'-二异丙烯基联苯、4,3'-二异丙烯基联苯、4,2'-二异丙烯基联苯、3,2'-二异丙烯基联苯、3,3'-二异丙烯基联苯、2,2'-二异丙烯基联苯或2,4-二异丙烯基联苯中的任意一种或至少两种的组合。
其中,R5和R6各自独立地碳原子数为6~30(例如6、9、10、12、14、16、18、20、22、24、26或28等)的亚芳香族烃基。
优选地,所述所述多官能乙烯基芳香族聚合物中重复单元a1的摩尔百分含量≥10%,例如可以为12%、15%、18%、20%、25%、28%、30%、35%、40%、45%、50%、55%、60%、65%、70%、75%、80%或85%等,进一步优选≥50%。
优选地,所述其他乙烯基化合物包括而不限于丁二烯、异戊二烯、双环戊二烯、马来酸酐化二烯、三烯丙基异氰脲酸酯树脂或单乙烯基芳香族化合物中的任意一种或至少两种的组合。
示例性地,所述其他乙烯基化合物可全部以单体的形式与二乙烯基芳香族化合物共聚,得到所述多官能乙烯基芳香族聚合物;或可将一部分其他乙烯基化合物先进行共聚,形成具有一定分子量的聚合物(例如形成苯乙烯-丁二烯-苯乙烯嵌段共聚物),再将其与二乙烯基芳香族化合物、剩余部分的乙烯基化合物(例如双环戊二烯)进行共聚,得到所述多官能乙烯基芳香族聚合物;或可将其他乙烯基化合物先进行共聚,形成具有一定分子量的聚合物(例如形成苯乙烯-丁二烯-苯乙烯嵌段共聚物),再将其与二乙烯基芳香族化合物共聚,得到所述多官能乙烯基芳香族聚合物。
优选地,所述单乙烯基芳香族化合物包括苯乙烯、含一个乙烯基的芴、含一个乙烯基的萘或含一个乙烯基的联苯中的任意一种或至少两种的组合。
优选地,所述多官能乙烯基芳香族聚合物的数均分子量为1000~500000,例如1500、2000、2500、3000、3500、4000、4500、5000、6000、8000、10000、20000、30000、40000、50000、70000、90000、100000、150000、200000、250000、300000、350000、400000或450000等。
优选地,所述多官能乙烯基芳香族聚合物包括低分子量聚合物和高分子量聚合物的组合;所述低分子量聚合物的数均分子量为1000~10000,所述高分子量聚合物的数均分子量为100000~500000。
优选地,所述多官能乙烯基芳香族聚合物中高分子量聚合物的质量百分含量为1~40%,例如3%、5%、8%、10%、12%、15%、18%、20%、22%、25%、28%、30%、32%、35%或38%等。
作为本发明的优选技术方案,所述多官能乙烯基芳香族聚合物包括低分子量聚合物和高分子量聚合物的组合;两种分子量范围的聚合物相互协同,使所述树脂组合物在反应活性、固化效率、介电性能、粘度、流动性和相容性方面取得良好的平衡。
硅芳炔树脂在常温下趋向于结晶,但在120~140℃熔融后的粘度很低,因此,当树脂组合物中含有过多的硅芳炔树脂时,树脂流动性会过大,不易于加工。而过少量的硅芳炔树脂难以在体系中形成稳定的网络,则难以发挥其高模量的优势。优选地,以硅芳炔树脂和多官能乙烯基芳香族聚合物重量份之和为100份计,所述硅芳炔树脂的质量为20~60份,例如22份、25份、28份、30份、32份、35份、38份、40份、42份、45份、48份、50份、52份、55份、57份或59份等。
优选地,所述树脂组合物以重量份计还包括5~85份含不饱和键的聚苯醚树脂,例如含不饱和键的聚苯醚树脂可以为6份、8份、10份、15份、20份、25份、30份、35份、40份、42份、45份、48份、50份、52份、55份、58份、60份、62份、65份、68份、70份、72份、75份、78份、80份或82份等。
所述含不饱和键的聚苯醚树脂中的不饱和键可以在聚苯醚树脂的端基或侧链上,所述含不饱和键的聚苯醚树脂的主链结构式为m是8-100。所述含不饱和键的聚苯醚树脂可以通过含有不饱和双键的化合物取代低分子化的聚苯醚树脂的端基或侧链上的氢原子制备得到。该类树脂的分子量大小影响其加工工艺和最终固化物的性能,其分子量越大,则树脂或溶液粘度越大,反应基团越少,与其他组份的相容性越差;分子量越小,则树脂或溶液的粘度越小,反应基团越多,而且与其他组份的相容性越好,但是分子量太小又会使固化物的介电性能和韧性损失。所述含不饱和键的聚苯醚可以采用市售材料,例如,沙伯基SA9000(甲基丙烯酰基封端的聚苯醚)、三菱化学株式会社的OPE-2st(末端含有乙烯基苄基的聚苯醚)等。
优选地,所述含不饱和键的聚苯醚树脂的数均分子量为1000~7000,例如1200、1500、1800、2000、2200、2500、2800、3000、3200、3500、3800、4000、4200、4500、4800、5000、5500、6000、6500或6800等,进一步优选为1000~4000。
优选地,所述树脂组合物以重量份计还包括0.01~10份引发剂,例如引发剂可以为0.03份、0.05份、0.08份、0.1份、0.3份、0.5份、0.8份、1份、1.5份、2份、2.5份、3份、3.5份、4份、4.5份、5份、6份、7份、8份或9份等。
优选地,所述引发剂包括过氧化物、偶氮类化合物、联枯或聚联枯中的任意一种或至少两种的组合。
优选地,所述过氧化物包括过氧化二异丙苯、叔丁基过氧化异丙苯、二叔丁基过氧化物、过氧化异丙基碳酸叔丁酯、2,5-二甲基-2,5-二叔丁基过氧基-3-己炔、2,5-二甲基-2,5-二(叔丁基过氧化)己烷、过氧化氢对孟烷,1,1-双(叔戊基过氧)环己烷、过氧化氢二异丙基苯、过氧化苯甲酰或过氧化苯甲酰衍生物中的任意一种或至少两种的组合。
优选地,所述偶氮类化合物包括偶氮二异丁腈。
优选地,所述树脂组合物以重量份计还包括5~60份交联剂,例如交联剂可以为6份、8份、10份、12份、15份、18份、20份、22份、25份、28份、30份、32份、35份、38份、40份、45份、50份、55份或58份等。
优选地,所述交联剂为分子结构中含有至少2个(例如2个、3个或4个等)不饱和键的化合物。
优选地,所述交联剂包括三烯丙基异氰脲酸酯、聚异氰脲酸三烯丙酯、三聚氰酸三烯丙酯、邻苯二甲酸二烯丙酯、在分子内具有2个以上甲基丙烯酰基的多官能甲基丙烯酸酯化合物、含有至少两个双键的联苯、双环戊二烯、含有至少两个双键的萘类化合物、p,p'-二乙烯基-1,2-二苯基乙烷或二乙烯基苯中的任意一种或至少两种的组合。
优选地,所述树脂组合物以重量份计还包括10~80份阻燃剂,例如阻燃剂可以为12份、15份、18份、20份、22份、25份、28份、30份、32份、35份、38份、40份、45份、50份、55份、60份、65份、70份、75份或78份等。
优选地,所述阻燃剂包括卤系阻燃剂、磷系阻燃剂或氮系阻燃剂中的任意一种或至少两种的组合。
本发明对于阻燃剂没有特别限定,具有阻燃效果的阻燃剂均可应用于所述树脂组合物中。示例性地,所述阻燃剂包括十溴二苯乙烷、十溴二苯乙撑、苯基膦酸二乙烯酯、苯基膦酸二烯丙酯、苯基膦酸二(1-丁烯基)酯、二苯基膦酸苯酯、二苯基膦酸甲酯、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物及其衍生物、双(2-烯丙基苯氧基)磷腈、二甲酚磷腈、磷酸三聚氰胺、焦磷酸三聚氰胺或聚磷酸三聚氰胺中的任意一种或至少两种的组合。
优选地,所述树脂组合物以重量份计还包括5~120份无机填料,例如无机填料可以为10份、15份、20份、25份、30份、35份、40份、50份、60份、70份、80份、90份、100份、110份、120份、130份、140份或145份等。
优选地,所述无机填料包括二氧化硅、硅微粉、氧化铝、二氧化钛、云母、氧化铍、钛酸钡、钛酸钾、钛酸锶、钛酸钙、碳酸铝、氢氧化镁、氢氧化铝、硅酸铝、碳酸钙、硅酸钙、硅酸镁、氮化硅、氮化硼、粘土、滑石粉、硼酸铝或碳化硅中的任意一种或至少两种的组合。
所述无机填料的形状没有特别的限制,可以为球型、角形、片型或空心等,优选为球型。
优选地,所述无机填料的粒径为0.01~30μm,例如0.02μm、0.05μm、0.08μm、0.1μm、0.5μm、0.5μm、0.8μm、1μm、3μm、5μm、8μm、10μm、12μm、15μm、18μm、20μm、22μm、25μm或28μm等,进一步优选为0.1~15μm。粒径为采用马尔文2000激光粒度分析仪测试。
作为本发明的优选技术方案,所述无机填料的粒径为0.01~30μm,可以使树脂组合物具有良好的流动性、加工成型性、机械性能、粘接性能和可靠性。如果无机填料的粒径小于0.01μm,会导致树脂组合物的流动性下降,使其在制作粘结片及覆金属箔层压板时的成型性变差,容易产生空隙;如果无机填料的粒径大于30μm,无机填料的表面积变大,使金属箔与树脂的粘接面积减小,进而导致印制电路板的剥离强度下降,配线间或绝缘层的绝缘可靠性下降。
优选地,所述树脂组合物以重量份计还包括0.01~7份硅烷偶联剂,例如硅烷偶联剂可以为0.03份、0.05份、0.08份、0.1份、0.3份、0.5份、0.8份、1份、1.2份、1.5份、1.8份、2份、2.5份、3份、3.5份、4份、4.5份、5份、5.5份、6份或6.5份等。
本发明对于硅烷偶联剂的种类没有特别限定,优选为乙烯基硅烷和/或烯丙基硅烷,主要用于促进无机填料和/或无机阻燃剂的分散。
示例性地,所述树脂组合物的制备方法可以为:将树脂组合物中的各组分与溶剂混合均匀,得到所述树脂组合物;优选地,可以先将固形物放入,然后加入溶剂,搅拌至固形物完全溶解后,再加入液态树脂和固化促进剂,继续搅拌均匀即可。
所述溶剂没有特别限定,包括醇类溶剂、醚类溶剂、芳香烃类溶剂、酯类溶剂、酮类溶剂或含氮类溶剂中的任意一种或至少两种的组合。其中,所述醇类溶剂包括甲醇、乙醇或丁醇中的任意一种或至少两种的组合;所述醚类溶剂包括乙基溶纤剂、丁基溶纤剂、乙二醇单甲醚、卡必醇或丁基卡必醇中的任意一种或至少两种的组合;所述芳香烃类溶剂包括苯、甲苯、二甲苯或均三甲苯中的任意一种或至少两种的组合;所述酯类溶剂包括乙酸乙酯、乙酸丁酯、甲氧基乙基乙酸酯、乙氧基乙基乙酸酯或丁氧基乙基乙酸酯中的任意一种或至少两种的组合;所述酮类溶剂包括丙酮、丁酮、甲基异丁酮、甲基乙基酮或环己酮中的任意一种或至少两种的组合;所述含氮类溶剂包括N,N-二甲基甲酰胺、N,N-二甲基乙酰胺或N-甲基-2-吡咯烷酮中的任意一种或至少两种的组合。
优选地,所述溶剂包括芳香烃类溶剂,所述芳香烃类溶剂在溶剂中的质量百分含量≥50%,例如52%、55%、58%、60%、62%、65%、68%、70%、72%、75%、78%、80%、82%、85%、88%、90%、92%、95%、98%或100%等。
所述溶剂的用量可以根据实际加工和应用需求进行调节。
本发明还涉及固化物,所述固化物为将如第一方面所述的树脂组合物固化而制备得到的。
另一方面,本发明提供一种树脂薄膜,所述树脂薄膜的原料包括如第一方面所述的树脂组合物;所述树脂膜是将如第一方面所述的树脂组合物涂覆在离型材料上经过干燥和/或半固化制得。
示例性地,所述树脂膜的制备方法为:将如第一方面所述的树脂组合物涂覆于离型材料(例如离型膜)上,干燥和/或半固化,得到所述树脂膜。
优选地,所述干燥的温度为180~220℃,例如185℃、190℃、195℃、200℃、205℃、210℃或215℃等。
优选地,所述干燥的时间为3~120min,例如5min、10min、15min、20min、25min、30min、35min、40min、50min、60min、70min、80min、90min、100min、105min、110min或115min等。
另一方面,本发明提供一种粘结片,所述粘结片包括增强材料,以及附着于所述增强材料上的如第一方面所述的树脂组合物。
优选地,所述增强材料包括石英布、石英玻璃纤维混纺布、玻纤布、玻纤纸或无纺布中的任意一种。
示例性地,所述粘结片的制备方法为:采用所述树脂组合物的树脂胶液浸润增强材料,然后干燥,得到所述粘结片。
优选地,所述树脂胶液中的溶剂没有特限定,进一步优选具有与上述相同的选择范围。
优选地,所述干燥的温度为130~180℃,例如135℃、140℃、145℃、150℃、155℃、160℃、165℃、170℃或175℃等。
优选地,所述干燥的时间为1~10min,例如2min、3min、4min、5min、6min、7min、8min或9min等。
本发明还涉及一种绝缘板,所述绝缘板包括至少一张如上所述的粘结片。
另一方面,本发明提供一种覆金属箔层压板,所述覆金属箔层压板包括至少一张如上所述的粘结片,以及设置于所述粘结片的一侧或两侧的金属箔。
优选地,所述金属箔为铜箔,所述覆金属箔层压板为覆铜板。
示例性地,所述覆金属箔层压板的制备方法为:在一张粘结片的一侧或两侧压合金属箔,固化,得到所述覆金属箔层压板;或,将至少两张粘结片粘合制成绝缘板,然后在所述绝缘板的一侧或两侧压合金属箔,固化,得到所述覆金属箔层压板。
优选地,所述固化在热压机中进行。
优选地,所述固化的温度为100~250℃,例如110℃、120℃、130℃、140℃、150℃、160℃、170℃、180℃、190℃、200℃、210℃、220℃、230℃、240℃或245℃等。
优选地,所述固化的压力为0.5~6MPa,例如0.8MPa、1MPa、1.2MPa、1.5MPa、1.8MPa、2MPa、2.2MPa、2.5MPa、2.8MPa、3MPa、3.2MPa、3.5MPa、3.8MPa、4MPa、4.2MPa、4.5MPa、4.8MPa、5MPa、5.2MPa、5.5MPa或5.8MPa等。
优选地,所述固化的时间为30~150min,例如40min、50min、60min、70min、80min、90min、100min、110min、120min、130min、140min或145min等。
另一方面,本发明提供一种印制电路板,所述印制电路板包括至少一张如上所述的粘结片或如上所述的覆金属箔层压板。
相对于现有技术,本发明具有以下有益效果:
本发明提供的树脂组合物包括硅芳炔树脂和多官能乙烯基芳香族聚合物的组合,通过特定聚合物的复配,使所述树脂组合物的加工性优异,固化物具有高模量、优异的介电性能和耐热性,而且热膨胀比例低,阻燃性、尺寸稳定性和粘结性能好。通过对树脂组合物中各组分的进一步优化和复配,使包含所述树脂组合物的覆金属箔层压板的玻璃化转变温度为210~270℃,热分解温度达到400~460℃,剥离强度为0.7~0.9N/mm,介电常数≤3.9(10GHz),介电损耗因数≤0.0045(10GHz),热膨胀比例低至1.2~2.2%,阻燃性达到V-0级,板材表观平整均匀,热应力(288℃浸锡)>10min,具有优异的加工性、粘接性、耐热性、介电性能和尺寸稳定性,能够充分满足高频电路基板在加工和应用性能方面的要求。
具体实施方式
下面通过具体实施方式来进一步说明本发明的技术方案。本领域技术人员应该明了,所述实施例仅仅是帮助理解本发明,不应视为对本发明的具体限制。
制备例1
一种硅芳炔树脂,具体为硅苯炔树脂,结构式如下:
制备方法包括如下步骤:
在充满氮气的反应釜中加入3.5份镁粉(化学纯,上海国药集团化学试剂有限公司)和40份四氢呋喃THF溶剂,在室温下搅拌并滴加13.5份溴乙烷(化学纯,上海国药集团化学试剂有限公司)和40份THF的混合溶液,滴加完成后于50℃保温1h;然后在冰水冷浴条件下,滴加7.5份1,3-二乙炔基苯(山东胶州市精细化工有限公司)和40份THF溶剂的混合物,滴加完毕后,65℃保温1h;再次冷却,在冰水冷浴条件下滴加5.5份二氯二甲基硅烷(化学纯,浙江新安化工集团有限公司,蒸馏后使用)和40份THF的混合物,滴加完毕后分别于40℃和70℃保温1h。反应完成后,蒸除反应物中的THF,并于冰水冷浴条件下滴加7.2份冰醋酸和50份甲苯溶剂的混合物,充分搅拌后再滴加140份2.0%稀盐酸水溶液,充分搅拌后分离出上层有机相。将有机相充分水洗至中性,然后干燥,过滤,蒸除甲苯,得到所述硅芳炔树脂。
通过凝胶色谱法(GPC,流动相为THF)对所述硅芳炔树脂进行测试,得到数均分子量为1200,以下实施例中简称为PSA1200。
制备例2
一种硅芳炔树脂,具体为硅苯炔树脂,结构式与制备例1中相同。
制备方法包括如下步骤:
在充满氮气的反应釜中加入3.5份镁粉(化学纯,上海国药集团化学试剂有限公司)和40份THF溶剂,在室温下搅拌并滴加13.5份溴乙烷(化学纯,上海国药集团化学试剂有限公司)和40份THF的混合溶液,滴加完成后于50℃保温1h;然后在冰水冷浴条件下,滴加7.5份1,3-二乙炔基苯(山东胶州市精细化工有限公司)和40份THF溶剂的混合物,滴加完毕后,于65℃保温1h;再次冷却,在冰水冷浴条件下滴加5.5份二氯二甲基硅烷(化学纯,浙江新安化工集团有限公司,蒸馏后使用)和40份THF的混合物,滴加完毕后分别于40℃和70℃保温2h。反应完成后,蒸除反应物中的THF,并于冰水冷浴条件下滴加7.2份冰醋酸和50份甲苯的混合物,充分搅拌后再滴加140份2.0%稀盐酸水溶液,充分搅拌后分离出上层有机相。将有机相充分水洗至中性,然后干燥,过滤,蒸除甲苯,得到所述硅芳炔树脂。
通过凝胶色谱法(GPC,流动相为THF)对所述硅芳炔树脂进行测试,得到数均分子量为3000,以下实施例中简称为PSA3000。
制备例3
一种硅芳炔树脂,具体为硅联苯炔树脂,结构式如下:
制备方法包括如下步骤:
在充满氮气的反应釜中加入3.5份镁粉(化学纯,上海国药集团化学试剂有限公司)和40份THF溶剂,在室温下搅拌并滴加13.5份溴乙烷(化学纯,上海国药集团化学试剂有限公司)和40份THF的混合溶液,滴加完成后于50℃保温1h;然后在冰水冷浴条件下,滴加12份对二乙炔基联苯(试剂,梯希爱(上海)提供)和40份THF溶剂的混合物,滴加完毕后,于65℃保温1h;再次冷却,在冰水冷浴条件下滴加5.5份二氯二甲基硅烷(化学纯,浙江新安化工集团有限公司,蒸馏后使用)和40份THF的混合物,滴加完毕后分别于40℃和70℃保温2h。反应完成后,蒸除反应物中的THF,并于冰水冷浴条件下滴加7.2份冰醋酸和50份甲苯的混合物,充分搅拌后再滴加140份2.0%稀盐酸水溶液,充分搅拌后分离出上层有机相。将有机相充分水洗至中性,然后干燥,过滤,蒸除甲苯,得到所述硅芳炔树脂。
通过凝胶色谱法(GPC,流动相为THF)对所述硅芳炔树脂进行测试,得到数均分子量为3500,以下实施例中简称为PSA3500。
制备例4
一种多官能乙烯基芳香族聚合物,制备方法如下:
将65份对二乙烯基苯(DVB)和5份A1536(苯乙烯-丁二烯-苯乙烯嵌段共聚物,数均分子量Mn为8.8万,购自科腾)在甲苯溶剂中混合均匀,然后加入0.14份引发剂过氧化二异丙苯(DCP),升温至100℃搅拌反应6h,冷却至室温,得到所述多官能乙烯基芳香族聚合物,以下实施例中简称为B-1。
制备例5
一种多官能乙烯基芳香族聚合物,制备方法如下:
将30份对二乙烯基苯(DVB)、5份A1535(苯乙烯-丁二烯-苯乙烯嵌段共聚物,Mn为20万,购自科腾)和5份双环戊二烯在甲苯中混合均匀,然后加入0.08份引发剂DCP,升温至120℃搅拌反应6h,冷却至室温,得到所述多官能乙烯基芳香族聚合物,以下实施例中简称为B-2。
制备例6
一种多官能乙烯基芳香族聚合物,制备方法如下:
将42份对二乙烯基苯(DVB)、5份A1536(苯乙烯-丁二烯-苯乙烯嵌段共聚物,Mn为8.8万,购自科腾)和3份双环戊二烯在甲苯中混合均匀,然后加入0.1份引发剂DCP,升温至120℃搅拌反应7h,冷却至室温,得到所述多官能乙烯基芳香族聚合物,以下实施例中简称为B-3。
本发明以下实施例及对比例中所涉及的实验材料包括:
(1)硅芳炔树脂
PSA1200,制备例1
PSA3000,制备例2
PSA3500,制备例3
(2)多官能乙烯基芳香族聚合物
B-1,制备例4
B-2,制备例5
B-3,制备例6
B-4,RICON257,丁二烯-苯乙烯-二乙烯基苯枝化三元共聚物,购自克雷威利;
B-5,ODV-XET,多官能乙烯基芳香族聚合物,Mn为2400,购自日本新日铁
聚烯烃树脂:A1536,苯乙烯-丁二烯-苯乙烯嵌段共聚物,数均分子量Mn为8.8万,购自科腾
(3)含不饱和键的聚苯醚树脂
SA9000,购自沙伯基础化学
OPE-2st,购自三菱化学
(4)交联剂
TAICROS,三烯丙基异三聚氰酸酯,购自赢创
4,4'-二乙烯基联苯,购自临川化工;
BVPE,p,p'-二乙烯基-1,2-二苯基乙烷,购自临川化工;
(5)引发剂
Perkadox BC-FF,过氧化二异丙苯,购自诺力昂
(6)无机填料
DQ1028L,球型硅微粉,中值粒径D50约3.0μm,购自江苏联瑞
(7)阻燃剂
BT-93w,添加型溴化阻燃剂,购自雅宝
XP7866,添加型含磷阻燃剂,购自雅宝
实施例1
本实施例提供一种树脂组合物,以重量份计包括如下组分:30份硅芳炔树脂PSA3000和70份多官能乙烯基芳香族聚合物B-1。
本实施例还提供一种覆金属箔层压板,具体制备方法如下:
(1)将本实施例提供的树脂组合物与50份甲苯混合、分散均匀,得到树脂胶液;
(2)取平整光洁、型号为2116的E型玻璃纤维布均匀浸渍步骤(1)得到的树脂胶液,在鼓风烘箱中于150℃烘烤5min,制得粘结片;
(3)将6张步骤(2)得到的粘结片叠合,在其上下两面覆上35μm铜箔,于真空热压机中在3MPa压力和220℃温度下压制90min,得到所述覆金属箔层压板。
实施例2
本实施例提供一种树脂组合物,以重量份计包括如下组分:60份硅芳炔树脂PSA1200,40份多官能乙烯基芳香族聚合物B-2,0.1份引发剂Perkadox BC-FF,110份无机填料DQ1028L。
本实施例还提供一种覆金属箔层压板,具体制备方法如下:
(1)将本实施例提供的树脂组合物与50份甲苯混合、分散均匀,得到树脂胶液;
(2)取平整光洁、型号为2116的E型玻璃纤维布均匀浸渍步骤(1)得到的树脂胶液,在鼓风烘箱中于150℃烘烤5min,制得粘结片;
(3)将6张步骤(2)得到的粘结片叠合,在其上下两面覆上35μm铜箔,于真空热压机中在3MPa压力和220℃温度下压制90min,得到所述覆金属箔层压板。
实施例3
本实施例提供一种树脂组合物,以重量份计包括如下组分:50份硅芳炔树脂PSA3000、50份多官能乙烯基芳香族聚合物B-3、80份含不饱和键的聚苯醚树脂SA9000,20份交联剂BVPE,0.4份引发剂Perkadox BC-FF,110份无机填料DQ1028L,50份阻燃剂BT-93w。
本实施例还提供一种覆金属箔层压板,具体制备方法如下:
(1)将本实施例提供的树脂组合物中的聚合物和引发剂、50份丁酮和100份甲苯混合后充分分散,然后加入无机填料和阻燃剂,经过高速剪切乳化后得到树脂胶液;
(2)取平整光洁、型号为2116的E型玻璃纤维布均匀浸渍步骤(1)得到的树脂胶液,在鼓风烘箱中于150℃烘烤5min,制得粘结片;
(3)将6张步骤(2)得到的粘结片叠合,在其上下两面覆上35μm铜箔,于真空热压机中在3MPa压力和220℃温度下压制90min,得到所述覆金属箔层压板。
实施例4~9,对比例1~3
一种树脂组合物,其组分及其含量如表1所示;表1中的各组分的用量单位均为“份”。
表1
将上述树脂组合物按照实施例3中的方法制成覆金属箔层压板,并对其性能进行测试,测试方法如下:
(1)玻璃化转变温度Tg:使用动态热机械分析仪(DMA),按照标准IPC-TM-6502.4.24中规定的DMA测试方法进行测定;
(2)热分解温度Td:使用热失重分析TGA,按照标准IPC-TM-650 2.4.24.6中规定的方法进行测试;
(3)剥离强度PS:在室温下将每毫米铜箔剥离覆金属箔层压板(覆铜板)所需的拉力,按照标准IPC-TM-650 2.4.8中规定的“接收态”实验条件,测试金属盖层的剥离强度;
(4)介电常数Dk和介电损耗因数Df:10GHz使用谐振腔法(SPDR)法测定,按照标准IPC-TM-650 2.5.5.5中规定的方法进行;
(5)阻燃性:按照UL94“50W(20mm)垂直燃烧试验:V-0、V-1和V-2”测试方法测试,认定V-0为阻燃;
(6)热膨胀比例CTE:采用静态热分析仪TMA进行测试,按照标准IPC-TM-6502.4.24中规定的方法进行;50~260℃热膨胀比例是在层压板样品的长度方向上测量得到的值;
(7)热应力:将5cm×5cm的覆铜板在288℃中浸锡,观察分层或起泡时间,小于10min则记为fail;
(8)样品板表观:目测板材平整度、是否有沟壑,流胶不良等,并测试板材厚度均匀性;
(9)加工性:根据常规的覆铜板层压程序(1.5~2℃/min升温速率,90℃加压,200℃保温90min)进行加工,可以直接加工成型,则认为易于加工;需调整程序,则认为难加工;经过多次程序调整依旧难以加工,则认为是极难加工。
测试结果如表2所示:
表2
根据表2的性能测试数据可知,相较于不含硅芳炔树脂的对比例1和不含多官能乙烯基芳香族聚合物的对比例2,本发明实施例提供的树脂组合物通过组分的协同复配,使包含其的覆金属箔层压板的玻璃化转变温度为210~270℃,热分解温度达到400~460℃,剥离强度为0.7~0.9N/mm,热膨胀比例低至1.2~2.2%,介电常数≤3.90(10GHz),介电损耗因数≤0.0045(10GHz),阻燃性达到V-0级,板材表观平整均匀,热应力(288℃浸锡时间)>10min,具有优异的加工性、粘接性、耐热性、介电性能和尺寸稳定性,能够充分满足高频电路基板在加工性和应用性能方面的要求。
进一步地,本发明通过对硅芳炔树脂和多官能乙烯基芳香族聚合物的组分和用量的调节,能够实现覆金属箔层压板性能的优化和改善。根据实施例4的测试结果可知,多官能乙烯基芳香族聚合物中多官能乙烯基芳香族单体(二乙烯基苯)用量过低时,体系的固化交联密度较低,样品的Tg明显降低,且CTE升高。实施例7中硅芳炔树脂的含量很高,板材样品的Tg明显较高,但因硅芳炔树脂的流动性过大,板材加工时难度较大,极易导致板材厚度不均。实施例8中硅芳炔树脂的含量较低,板材样品的Tg明显较低,且由于多官能乙烯基芳香族聚合物中多官能乙烯基芳香族单体(二乙烯基苯)用量较多,树脂固化速度较快,板材加工过程中流胶偏低,流动不良,较难加工。实施例9中所用硅芳炔树脂中的芳香基团为联苯基,板材的Tg相对实施例5略高,且在CTE方面有较好表现。
对比例1未添加硅芳炔,与实施例5相比,耐热性及CTE都变差;对比例2未添加多官能乙烯基芳香族聚合物,与实施例2相比,剥离强度、介电性能、表观及加工性都变差;对比例3中采用普通的丁二烯-苯乙烯-丁二烯嵌段聚合物替代多官能乙烯基芳香族聚合物,其固化反应难度较大,不易完全交联反应,板材样品Tg偏低,且在热应力测试时易于分层起泡,在耐热性和加工性方面都无法满足高频电路基板的使用要求。
申请人声明,本发明通过上述实施例来说明本发明的一种树脂组合物及包含其的粘结片、覆金属箔层压板,但本发明并不局限于上述实施例,即不意味着本发明必须依赖上述实施例才能实施。所属技术领域的技术人员应该明了,对本发明的任何改进,对本发明产品各原料的等效替换及辅助成分的添加、具体方式的选择等,均落在本发明的保护范围和公开范围之内。
Claims (10)
1.一种树脂组合物,其特征在于,所述树脂组合物以重量份计包括如下组分:以硅芳炔树脂和多官能乙烯基芳香族聚合物的重量份之和为100份计,硅芳炔树脂5~95份,多官能乙烯基芳香族聚合物5~95份;所述多官能乙烯基芳香族聚合物由二乙烯基芳香族化合物和其他乙烯基化合物共聚而成,且二乙烯基芳香族化合物在共聚物的重复单元中的摩尔占比大于等于15%。
3.根据权利要求1或2所述的树脂组合物,其特征在于,所述多官能乙烯基芳香族聚合物包含重复单元a1和/或重复单元a2;
其中,R5和R6各自独立地为碳原子数为6~30的亚芳香族烃基;
优选地,所述多官能乙烯基芳香族聚合物中重复单元a1的摩尔百分含量≥10%,进一步优选≥50%;
优选地,所述其他乙烯基化合物包括丁二烯、异戊二烯、双环戊二烯、马来酸酐化二烯、三烯丙基异氰脲酸酯树脂或单乙烯基芳香族化合物中的任意一种或至少两种的组合;
优选地,所述单乙烯基芳香族化合物包括苯乙烯、含一个乙烯基的芴、含一个乙烯基的萘或含一个乙烯基的联苯中的任意一种或至少两种的组合;
优选地,所述多官能乙烯基芳香族聚合物的数均分子量为1000~500000;
优选地,所述多官能乙烯基芳香族聚合物包括低分子量聚合物和高分子量聚合物的组合;所述低分子量聚合物的数均分子量为1000~10000,所述高分子量聚合物的数均分子量为100000~500000;
优选地,所述多官能乙烯基芳香族聚合物中高分子量聚合物的质量百分含量为1~40%;
优选地,以硅芳炔树脂和多官能乙烯基芳香族聚合物的重量份之和为100份计,所述硅芳炔树脂的质量为20~60份。
4.根据权利要求1~3任一项所述的树脂组合物,其特征在于,所述树脂组合物以重量份计还包括5~85份含不饱和键的聚苯醚树脂;
优选地,所述含不饱和键的聚苯醚树脂的数均分子量为1000~7000,进一步优选为1000~4000。
5.根据权利要求1~4任一项所述的树脂组合物,其特征在于,所述树脂组合物以重量份计还包括0.01~10份引发剂;
优选地,所述引发剂包括过氧化物、偶氮类化合物、联枯或聚联枯中的任意一种或至少两种的组合;
优选地,所述过氧化物包括过氧化二异丙苯、叔丁基过氧化异丙苯、二叔丁基过氧化物、过氧化异丙基碳酸叔丁酯、2,5-二甲基-2,5-二叔丁基过氧基-3-己炔、2,5-二甲基-2,5-二(叔丁基过氧化)己烷、过氧化氢对孟烷,1,1-双(叔戊基过氧)环己烷、过氧化氢二异丙基苯、过氧化苯甲酰或过氧化苯甲酰衍生物中的任意一种或至少两种的组合;
优选地,所述树脂组合物以重量份计还包括5~60份交联剂;
优选地,所述交联剂为分子结构中含有至少2个不饱和键的化合物;
优选地,所述交联剂包括三烯丙基异氰脲酸酯、聚异氰脲酸三烯丙酯、三聚氰酸三烯丙酯、邻苯二甲酸二烯丙酯、在分子内具有2个以上甲基丙烯酰基的多官能甲基丙烯酸酯化合物、含有至少两个双键的联苯、双环戊二烯、含有至少两个双键的萘类化合物、p,p'-二乙烯基-1,2-二苯基乙烷或二乙烯基苯中的任意一种或至少两种的组合;
优选地,所述树脂组合物以重量份计还包括10~80份阻燃剂;
优选地,所述阻燃剂包括卤系阻燃剂、磷系阻燃剂或氮系阻燃剂中的任意一种或至少两种的组合。
6.根据权利要求1~5任一项所述的树脂组合物,其特征在于,所述树脂组合物以重量份计还包括5~120份无机填料;
优选地,所述无机填料包括二氧化硅、硅微粉、氧化铝、二氧化钛、云母、氧化铍、钛酸钡、钛酸钾、钛酸锶、钛酸钙、碳酸铝、氢氧化镁、氢氧化铝、硅酸铝、碳酸钙、硅酸钙、硅酸镁、氮化硅、氮化硼、粘土、滑石粉、硼酸铝或碳化硅中的任意一种或至少两种的组合;
优选地,所述无机填料的粒径为0.01~30μm,进一步优选为0.1~15μm;
优选地,所述树脂组合物以重量份计还包括0.01~7份硅烷偶联剂。
7.一种树脂膜,其特征在于,所述树脂膜是将如权利要求1~6任一项所述的树脂组合物涂覆在离型材料上经过干燥和/或半固化制得。
8.一种粘结片,其特征在于,所述粘结片包括增强材料,以及附着于所述增强材料上的如权利要求1~6任一项所述的树脂组合物;
优选地,所述增强材料包括石英布、石英玻璃混纺布、玻纤布、玻纤纸或无纺布中的任意一种。
9.一种覆金属箔层压板,其特征在于,所述覆金属箔层压板包括至少一张如权利要求8所述的粘结片,以及设置于所述粘结片的一侧或两侧的金属箔;
优选地,所述金属箔为铜箔。
10.一种印制电路板,其特征在于,所述印制电路板包括至少一张如权利要求8所述的粘结片或如权利要求9所述的覆金属箔层压板。
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