JP2022047422A - Hardening body - Google Patents
Hardening body Download PDFInfo
- Publication number
- JP2022047422A JP2022047422A JP2020153335A JP2020153335A JP2022047422A JP 2022047422 A JP2022047422 A JP 2022047422A JP 2020153335 A JP2020153335 A JP 2020153335A JP 2020153335 A JP2020153335 A JP 2020153335A JP 2022047422 A JP2022047422 A JP 2022047422A
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- Prior art keywords
- cured product
- resin
- mass
- epoxy resin
- manufactured
- 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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- 239000011342 resin composition Substances 0.000 claims abstract description 95
- 239000011256 inorganic filler Substances 0.000 claims abstract description 84
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 84
- 239000000758 substrate Substances 0.000 claims abstract description 75
- 239000001023 inorganic pigment Substances 0.000 claims abstract description 58
- 239000004020 conductor Substances 0.000 claims abstract description 18
- 239000004065 semiconductor Substances 0.000 claims abstract description 9
- 239000003822 epoxy resin Substances 0.000 claims description 138
- 229920000647 polyepoxide Polymers 0.000 claims description 138
- 229920005989 resin Polymers 0.000 claims description 117
- 239000011347 resin Substances 0.000 claims description 117
- 239000010410 layer Substances 0.000 claims description 78
- 229920001187 thermosetting polymer Polymers 0.000 claims description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 16
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 12
- 229910000679 solder Inorganic materials 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011229 interlayer Substances 0.000 claims description 6
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 4
- 229910002113 barium titanate Inorganic materials 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
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- 230000001747 exhibiting effect Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 115
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- 239000007787 solid Substances 0.000 description 20
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- 235000010290 biphenyl Nutrition 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 10
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- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 9
- 125000003700 epoxy group Chemical group 0.000 description 9
- PARWUHTVGZSQPD-UHFFFAOYSA-N phenylsilane Chemical compound [SiH3]C1=CC=CC=C1 PARWUHTVGZSQPD-UHFFFAOYSA-N 0.000 description 9
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- ZFVMWEVVKGLCIJ-UHFFFAOYSA-N bisphenol AF Chemical compound C1=CC(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C=C1 ZFVMWEVVKGLCIJ-UHFFFAOYSA-N 0.000 description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
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- 239000010969 white metal Substances 0.000 description 8
- 239000004925 Acrylic resin Substances 0.000 description 7
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- 239000004642 Polyimide Substances 0.000 description 7
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 7
- 239000002270 dispersing agent Substances 0.000 description 7
- 239000011888 foil Substances 0.000 description 7
- 239000000178 monomer Substances 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- 239000011574 phosphorus Substances 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 239000003381 stabilizer Substances 0.000 description 7
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 6
- 239000000654 additive Substances 0.000 description 6
- 150000001718 carbodiimides Chemical class 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 229930003836 cresol Natural products 0.000 description 6
- 238000002788 crimping Methods 0.000 description 6
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- 229910052731 fluorine Inorganic materials 0.000 description 6
- 125000004433 nitrogen atom Chemical group N* 0.000 description 6
- 229920001955 polyphenylene ether Polymers 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 6
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 5
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- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 5
- 239000002518 antifoaming agent Substances 0.000 description 5
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- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 5
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- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 4
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- XDKMXYYPKSWJNR-UHFFFAOYSA-N thiocyanic acid;triphenylphosphane Chemical compound SC#N.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 XDKMXYYPKSWJNR-UHFFFAOYSA-N 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- JUWGUJSXVOBPHP-UHFFFAOYSA-B titanium(4+);tetraphosphate Chemical compound [Ti+4].[Ti+4].[Ti+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JUWGUJSXVOBPHP-UHFFFAOYSA-B 0.000 description 1
- PJANXHGTPQOBST-VAWYXSNFSA-N trans-stilbene Chemical class C=1C=CC=CC=1/C=C/C1=CC=CC=C1 PJANXHGTPQOBST-VAWYXSNFSA-N 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
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- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- TUQOTMZNTHZOKS-UHFFFAOYSA-N tributylphosphine Chemical compound CCCCP(CCCC)CCCC TUQOTMZNTHZOKS-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- GFKCWAROGHMSTC-UHFFFAOYSA-N trimethoxy(6-trimethoxysilylhexyl)silane Chemical compound CO[Si](OC)(OC)CCCCCC[Si](OC)(OC)OC GFKCWAROGHMSTC-UHFFFAOYSA-N 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 description 1
- XMQSELBBYSAURN-UHFFFAOYSA-M triphenyl(propyl)phosphanium;bromide Chemical compound [Br-].C=1C=CC=CC=1[P+](C=1C=CC=CC=1)(CCC)C1=CC=CC=C1 XMQSELBBYSAURN-UHFFFAOYSA-M 0.000 description 1
- MXSVLWZRHLXFKH-UHFFFAOYSA-N triphenylborane Chemical compound C1=CC=CC=C1B(C=1C=CC=CC=1)C1=CC=CC=C1 MXSVLWZRHLXFKH-UHFFFAOYSA-N 0.000 description 1
- IDXDWPWXHTXJMZ-UHFFFAOYSA-N tris(2,4,6-trimethylphenyl)phosphane Chemical compound CC1=CC(C)=CC(C)=C1P(C=1C(=CC(C)=CC=1C)C)C1=C(C)C=C(C)C=C1C IDXDWPWXHTXJMZ-UHFFFAOYSA-N 0.000 description 1
- XDHRVAHAGMMFMC-UHFFFAOYSA-N tris(2,4-dimethylphenyl)phosphane Chemical compound CC1=CC(C)=CC=C1P(C=1C(=CC(C)=CC=1)C)C1=CC=C(C)C=C1C XDHRVAHAGMMFMC-UHFFFAOYSA-N 0.000 description 1
- KAAYGTMPJQOOGY-UHFFFAOYSA-N tris(2,5-dimethylphenyl)phosphane Chemical compound CC1=CC=C(C)C(P(C=2C(=CC=C(C)C=2)C)C=2C(=CC=C(C)C=2)C)=C1 KAAYGTMPJQOOGY-UHFFFAOYSA-N 0.000 description 1
- RERMPCBBVZEPBS-UHFFFAOYSA-N tris(2,6-dimethylphenyl)phosphane Chemical compound CC1=CC=CC(C)=C1P(C=1C(=CC=CC=1C)C)C1=C(C)C=CC=C1C RERMPCBBVZEPBS-UHFFFAOYSA-N 0.000 description 1
- IIOSDXGZLBPOHD-UHFFFAOYSA-N tris(2-methoxyphenyl)phosphane Chemical compound COC1=CC=CC=C1P(C=1C(=CC=CC=1)OC)C1=CC=CC=C1OC IIOSDXGZLBPOHD-UHFFFAOYSA-N 0.000 description 1
- COIOYMYWGDAQPM-UHFFFAOYSA-N tris(2-methylphenyl)phosphane Chemical compound CC1=CC=CC=C1P(C=1C(=CC=CC=1)C)C1=CC=CC=C1C COIOYMYWGDAQPM-UHFFFAOYSA-N 0.000 description 1
- XRALRSQLQXKXKP-UHFFFAOYSA-N tris(3,5-dimethylphenyl)phosphane Chemical compound CC1=CC(C)=CC(P(C=2C=C(C)C=C(C)C=2)C=2C=C(C)C=C(C)C=2)=C1 XRALRSQLQXKXKP-UHFFFAOYSA-N 0.000 description 1
- RYXYUARTMQUYKV-UHFFFAOYSA-N tris(4-butylphenyl)phosphane Chemical compound C1=CC(CCCC)=CC=C1P(C=1C=CC(CCCC)=CC=1)C1=CC=C(CCCC)C=C1 RYXYUARTMQUYKV-UHFFFAOYSA-N 0.000 description 1
- SPNVODOGUAUMCA-UHFFFAOYSA-N tris(4-ethoxy-2,6-dimethylphenyl)phosphane Chemical compound CC1=CC(OCC)=CC(C)=C1P(C=1C(=CC(OCC)=CC=1C)C)C1=C(C)C=C(OCC)C=C1C SPNVODOGUAUMCA-UHFFFAOYSA-N 0.000 description 1
- PCCAGZSOGFNURV-UHFFFAOYSA-N tris(4-ethylphenyl)phosphane Chemical compound C1=CC(CC)=CC=C1P(C=1C=CC(CC)=CC=1)C1=CC=C(CC)C=C1 PCCAGZSOGFNURV-UHFFFAOYSA-N 0.000 description 1
- UYUUAUOYLFIRJG-UHFFFAOYSA-N tris(4-methoxyphenyl)phosphane Chemical compound C1=CC(OC)=CC=C1P(C=1C=CC(OC)=CC=1)C1=CC=C(OC)C=C1 UYUUAUOYLFIRJG-UHFFFAOYSA-N 0.000 description 1
- NTUMNRFLAZXNBW-UHFFFAOYSA-N tris(4-propan-2-ylphenyl)phosphane Chemical compound C1=CC(C(C)C)=CC=C1P(C=1C=CC(=CC=1)C(C)C)C1=CC=C(C(C)C)C=C1 NTUMNRFLAZXNBW-UHFFFAOYSA-N 0.000 description 1
- JTOQWGJGVSYTTN-UHFFFAOYSA-N tris(4-propylphenyl)phosphane Chemical compound C1=CC(CCC)=CC=C1P(C=1C=CC(CCC)=CC=1)C1=CC=C(CCC)C=C1 JTOQWGJGVSYTTN-UHFFFAOYSA-N 0.000 description 1
- UGNAOCDIZFIEQK-UHFFFAOYSA-N tris[4-[(2-methylpropan-2-yl)oxy]phenyl]phosphane Chemical compound C1=CC(OC(C)(C)C)=CC=C1P(C=1C=CC(OC(C)(C)C)=CC=1)C1=CC=C(OC(C)(C)C)C=C1 UGNAOCDIZFIEQK-UHFFFAOYSA-N 0.000 description 1
- 229920001862 ultra low molecular weight polyethylene Polymers 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
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Abstract
Description
本発明は、硬化体に関する。さらには、当該硬化体を用いて得られる、積層構造体、反射シート、プリント配線板及び半導体装置に関する。 The present invention relates to a cured product. Further, the present invention relates to a laminated structure, a reflective sheet, a printed wiring board and a semiconductor device obtained by using the cured product.
プリント配線板においては、携帯端末、コンピューター、テレビ等の液晶ディスプレイのバックライト;照明器具の光源など、低電力で発光する発光ダイオード(LED)を直接実装して用いられる用途が増えてきている。LEDは、近年、小型化が進行し、ミニLEDやマイクロLEDと称されるLEDがある。 In printed wiring boards, there are an increasing number of applications in which light emitting diodes (LEDs) that emit light with low power are directly mounted and used, such as backlights for liquid crystal displays of mobile terminals, computers, televisions, etc.; light sources for lighting equipment. In recent years, LEDs have been miniaturized, and there are LEDs called mini LEDs and micro LEDs.
このようなプリント配線板の最外層には、光源から発せられる光の取り出し効率を高めるため、光を反射させるための反射シートが形成されている。 A reflective sheet for reflecting light is formed on the outermost layer of such a printed wiring board in order to increase the efficiency of extracting light emitted from a light source.
このような反射シートの材料として、例えば、特許文献1には、バインダーポリマー、白色無機顔料を含有する架橋ポリマー粒子を含有する樹脂組成物が開示されている。 As a material for such a reflective sheet, for example, Patent Document 1 discloses a resin composition containing crosslinked polymer particles containing a binder polymer and a white inorganic pigment.
ところで、本発明者らが検討したところ、高い光反射率を達成すべく白色無機顔料の含有量の高い樹脂組成物を用いると、得られる硬化体と下地基板の導体層との密着性(以下、単に「下地密着性」ともいう。)が劣る場合があることを見出した。白色無機顔料の含有量を抑えることにより下地密着性は幾分改善されるものの、その場合は、光反射率が低下してしまう。 By the way, as a result of studies by the present inventors, when a resin composition having a high content of white inorganic pigment is used in order to achieve high light reflectance, the adhesion between the obtained cured product and the conductor layer of the base substrate (hereinafter referred to as “adhesion”). , Simply referred to as "base adhesion") was found to be inferior. By suppressing the content of the white inorganic pigment, the adhesion to the substrate is somewhat improved, but in that case, the light reflectance is lowered.
本発明は、高い光反射率を呈すると共に良好な下地密着性を呈する硬化体を提供することを課題とする。 An object of the present invention is to provide a cured product which exhibits high light reflectance and good substrate adhesion.
本発明者らは、上記課題を解決すべく鋭意検討した結果、下地基板の上に設けた際に、下地基板とは接していない側の表面近傍の領域において樹脂成分と白色無機顔料等の無機充填材成分との量比(無機充填材成分/樹脂成分)に勾配(すなわち、硬化体表面から深さ方向に向かって一定値以上の負の勾配)を有する硬化体が、高い光反射率を呈すると共に良好な下地密着性を呈することを見出し、本発明を完成するに至った。 As a result of diligent studies to solve the above problems, the present inventors have made a resin component and an inorganic substance such as a white inorganic pigment in a region near the surface on the side not in contact with the underlying substrate when the substrate is provided. A cured product having a gradient (that is, a negative gradient of a certain value or more in the depth direction from the surface of the cured product) in the amount ratio (inorganic filler component / resin component) with the filler component has high light reflectance. It has been found that the present invention exhibits good adhesion to the substrate as well as the present invention, and has completed the present invention.
すなわち、本発明は以下の内容を含む。
[1] 表面の少なくとも一部に導体層を備える基板上に設けられた、少なくとも白色無機顔料を含む無機充填材成分を含有した樹脂組成物の硬化体であって、
該硬化体中の不揮発成分を100質量%としたとき、白色無機顔料の含有量が20質量%以上であり、
該硬化体の、基板と接していない側の表面を第1の主面としたとき、
該硬化体の第1の主面に垂直な方向における硬化体の断面において、硬化体の第1の主面からの距離が0μmから5μmまでの領域における単位面積当たりの無機充填材成分の面積A0-5と、第1の主面からの距離が5μmから10μmまでの領域における単位面積当たりの無機充填材成分の面積A5-10とが、A0-5/A5-10>1.1を満たす、硬化体。
[2] 熱硬化性樹脂をさらに含む、[1]に記載の硬化体。
[3] 硬化体中の不揮発成分を100質量%としたとき、白色無機顔料の含有量が20~60質量%である、[1]又は[2]に記載の硬化体。
[4] 熱硬化性樹脂がエポキシ樹脂を含む、[2]又は[3]に記載の硬化体。
[5] 硬化体中の不揮発成分を100質量%としたとき、エポキシ樹脂の含有量が10~50質量%である、[4]に記載の硬化体。
[6] 白色無機顔料が、酸化アルミニウム、酸化チタン、酸化ジルコニウム、酸化マグネシウム、チタン酸バリウム、酸化亜鉛、酸化セリウム、及び炭酸カルシウムから選ばれる1種以上である、[1]~[5]の何れかに記載の硬化体。
[7] プリント配線板の絶縁層用又はソルダーレジスト層用である、[1]~[6]の何れかに記載の硬化体。
[8] 光反射用である、[1]~[7]の何れかに記載の硬化体。
[9] 波長460nmの光に対する反射率が80%以上である、[1]~[8]の何れかに記載の硬化体。
[10] 表面の少なくとも一部に導体層を備える基板と、該基板の上に設けられた[1]~[9]の何れかに記載の硬化体とを含む、積層構造体。
[11] [1]~[9]の何れかに記載の硬化体を含む、反射シート。
[12] [11]に記載の反射シートを層間絶縁層又はソルダーレジストとして含む、プリント配線板。
[13] [1]~[9]の何れかに記載の硬化体を含む、プリント配線板。
[14] [12]又は[13]に記載のプリント配線板を含む、半導体装置。
That is, the present invention includes the following contents.
[1] A cured product of a resin composition containing an inorganic filler component containing at least a white inorganic pigment, which is provided on a substrate having a conductor layer on at least a part of the surface thereof.
When the non-volatile component in the cured product is 100% by mass, the content of the white inorganic pigment is 20% by mass or more.
When the surface of the cured product on the side not in contact with the substrate is used as the first main surface,
Area A of the inorganic filler component per unit area in the region where the distance from the first main surface of the cured body is from 0 μm to 5 μm in the cross section of the cured body in the direction perpendicular to the first main surface of the cured body. 0-5 and the area A 5-10 of the inorganic filler component per unit area in the region where the distance from the first main surface is from 5 μm to 10 μm are A 0-5 / A 5-10 > 1. A cured product that satisfies 1.
[2] The cured product according to [1], further containing a thermosetting resin.
[3] The cured product according to [1] or [2], wherein the content of the white inorganic pigment is 20 to 60% by mass when the non-volatile component in the cured product is 100% by mass.
[4] The cured product according to [2] or [3], wherein the thermosetting resin contains an epoxy resin.
[5] The cured product according to [4], wherein the content of the epoxy resin is 10 to 50% by mass when the non-volatile component in the cured product is 100% by mass.
[6] The white inorganic pigment is one or more selected from aluminum oxide, titanium oxide, zirconium oxide, magnesium oxide, barium titanate, zinc oxide, cerium oxide, and calcium carbonate, [1] to [5]. The cured product described in any of them.
[7] The cured product according to any one of [1] to [6], which is used for an insulating layer of a printed wiring board or a solder resist layer.
[8] The cured product according to any one of [1] to [7], which is for light reflection.
[9] The cured product according to any one of [1] to [8], which has a reflectance of 80% or more with respect to light having a wavelength of 460 nm.
[10] A laminated structure including a substrate having a conductor layer on at least a part of the surface thereof and a cured product according to any one of [1] to [9] provided on the substrate.
[11] A reflective sheet containing the cured product according to any one of [1] to [9].
[12] A printed wiring board containing the reflective sheet according to [11] as an interlayer insulating layer or a solder resist.
[13] A printed wiring board containing the cured product according to any one of [1] to [9].
[14] A semiconductor device including the printed wiring board according to [12] or [13].
本発明によれば、高い光反射率を呈すると共に良好な下地密着性を呈する硬化体を提供することができる。 According to the present invention, it is possible to provide a cured product which exhibits high light reflectance and good substrate adhesion.
以下、本発明をその好適な実施形態に即して詳細に説明する。ただし、本発明は、下記実施形態及び例示物に限定されるものではなく、本発明の特許請求の範囲及びその均等の範囲を逸脱しない範囲において任意に変更して実施され得る。 Hereinafter, the present invention will be described in detail according to the preferred embodiment thereof. However, the present invention is not limited to the following embodiments and examples, and may be arbitrarily modified and implemented without departing from the scope of claims of the present invention and the equivalent scope thereof.
[硬化体]
本発明の硬化体は、表面の少なくとも一部に導体層を備える基板(以下、単に「下地基板」ともいう。)上に設けられた、少なくとも白色無機顔料を含む無機充填材成分を含有した樹脂組成物の硬化体であって、下地基板とは接していない側の表面近傍の領域において樹脂成分と無機充填材成分との量比(無機充填材成分/樹脂成分)に勾配(すなわち、硬化体表面から深さ方向に向かって一定値以上の負の勾配)を有することを特徴とする。
[Hardened body]
The cured product of the present invention is a resin containing an inorganic filler component containing at least a white inorganic pigment, which is provided on a substrate having a conductor layer on at least a part of the surface (hereinafter, also simply referred to as a “base substrate”). A cured product of the composition having a gradient (that is, a cured product) in the amount ratio (inorganic filler component / resin component) of the resin component and the inorganic filler component in the region near the surface on the side not in contact with the underlying substrate. It is characterized by having a negative gradient of a certain value or more from the surface toward the depth direction).
以下の説明においては、硬化体の2つの主面(表面)のうち、下地基板と接していない側の主面を「第1の主面」、下地基板と接している主面を「第2の主面」という場合がある。 In the following description, of the two main surfaces (surfaces) of the cured body, the main surface on the side not in contact with the base substrate is the "first main surface", and the main surface in contact with the base substrate is the "second main surface". It may be called "the main surface of".
本発明の硬化体においては、下地基板と接してない側の表面(第1の主面)には無機充填材成分リッチな相が存在するが、該表面から厚さ方向に向かって一定の距離位置において、無機充填材成分の割合が減少する。ここで、「厚さ方向」とは、硬化体の厚さ方向をいい、硬化体の第1の主面に垂直な方向を表す。 In the cured product of the present invention, a phase rich in the inorganic filler component exists on the surface (first main surface) on the side not in contact with the underlying substrate, but a certain distance from the surface in the thickness direction. At the position, the proportion of the inorganic filler component is reduced. Here, the "thickness direction" refers to the thickness direction of the cured body, and represents the direction perpendicular to the first main surface of the cured body.
第1の主面近傍の限られた領域に無機充填材成分リッチな相が存在する本発明の硬化体によれば、斯かる無機充填材成分リッチな相によって、バルクの無機充填材濃度から期待されるよりも顕著に高い光反射率を実現すると共に、下地基板と接している主面(第2の主面)近傍の領域に樹脂成分リッチな相が存在することとなり、下地基板に対して優れた密着性を呈することができるものと推察される。 According to the cured product of the present invention in which an inorganic filler component-rich phase exists in a limited region near the first main surface, such an inorganic filler component-rich phase is expected from the bulk inorganic filler concentration. In addition to achieving a significantly higher light reflectance than that of the base substrate, a resin-rich phase exists in the region near the main surface (second main surface) in contact with the base substrate. It is presumed that it can exhibit excellent adhesion.
本発明において、第1の主面近傍の領域における無機充填材成分と樹脂成分との量比の勾配を表すにあたっては、該第1の主面に垂直な方向における硬化体の断面における、該第1の主面からの距離がd1(μm)からd2(μm)までの領域の無機充填材成分面積Ad1-d2と、前記第1の主面からの距離がd2(μm)からd3(μm)までの領域の無機充填材成分面積Ad2-d3との比(kAd1-d2/Ad2-d3)を用いることとする。ここで、d1、d2及びd3は、0≦d1<d2<d3≦Dを満たす数であり、kは、k=|d2-d3|/|d1-d2|を満たす係数であり、Dは硬化体の厚さ(μm)である。 In the present invention, in expressing the gradient of the quantitative ratio of the inorganic filler component and the resin component in the region near the first main surface, the first aspect of the cured product in the direction perpendicular to the first main surface. The inorganic filler component area A d1-d2 in the region where the distance from the main surface of 1 is from d1 (μm) to d2 (μm), and the distance from the first main surface is d2 (μm) to d3 (μm). The ratio (kA d1-d2 / A d2-d3 ) to the inorganic filler component area A d2-d3 in the region up to) is used. Here, d1, d2 and d3 are numbers satisfying 0 ≦ d1 <d2 <d3 ≦ D, k is a coefficient satisfying k = | d2-d3 | / | d1-d2 |, and D is curing. Body thickness (μm).
本発明において、「無機充填材成分面積」とは、無機充填材成分が占める面積をいい、「無機充填材成分」とは、白色無機顔料のほか、シリカ等の他の無機充填材を包含する。また本発明において、「白色無機顔料」とは、一実施形態において、波長500nmの光に対する反射率が90%以上である無機化合物、無機充填材のことをいう。 In the present invention, the "inorganic filler component area" refers to the area occupied by the inorganic filler component, and the "inorganic filler component" includes other inorganic fillers such as silica in addition to the white inorganic pigment. .. Further, in the present invention, the "white inorganic pigment" refers to an inorganic compound or an inorganic filler having a reflectance of 90% or more with respect to light having a wavelength of 500 nm in one embodiment.
無機充填材成分面積の比(kAd1-d2/Ad2-d3)は、後述の<無機充填材成分面積比の測定>に記載の方法により測定することができる。具体的には、(1)硬化体の第1の主面に垂直な断面が露出するように断面出しを行い、断面試料を作製すること、(2)断面試料をSEM観察し、得られたSEM像について画像解析してAd1-d2値及びAd2-d3値を求めること、及び(3)得られたAd1-d2値及びAd2-d3値から比(kAd1-d2/Ad2-d3)を算出すること、を含む方法により、測定することができる。画像解析では、樹脂成分部分と無機充填材成分部分を2値化し、無機充填材成分部分のピクセル数を無機充填材成分面積として扱う。また、Ad1-d2値及びAd2-d3値の測定にあたっては、測定領域の幅(硬化体表面に平行な方向における測定距離)を等しく設定する。これにより、上記の比(kAd1-d2/Ad2-d3)は、表面からの距離がd1(μm)からd2(μm)までの領域における単位面積当たりの無機充填材成分面積と、表面からの距離がd2(μm)からd3(μm)までの領域における単位面積当たりの無機充填材成分面積との比を表す。例えば、無機充填材成分面積比A0-5/A5-10の測定においては、d1=0μm、d2=5μm、d3=10μm、k=1である。 The ratio of the inorganic filler component area (kA d1-d2 / A d2-d3 ) can be measured by the method described in <Measurement of Inorganic Filler Component Area Ratio> described later. Specifically, it was obtained by (1) making a cross section so that the cross section perpendicular to the first main surface of the cured product was exposed to prepare a cross section sample, and (2) observing the cross section sample by SEM. Image analysis of the SEM image is performed to obtain the A d1-d2 value and the A d2-d3 value, and (3) the ratio (kA d1-d2 / A d2 ) from the obtained A d1-d2 value and the A d2-d3 value. -D3 ) can be measured by a method including the calculation. In the image analysis, the resin component portion and the inorganic filler component portion are binarized, and the number of pixels of the inorganic filler component portion is treated as the inorganic filler component area. Further, when measuring the A d1-d2 value and the A d2-d3 value, the width of the measurement region (measurement distance in the direction parallel to the surface of the cured product) is set to be equal. As a result, the above ratio (kA d1-d2 / A d2-d3 ) is the area of the inorganic filler component per unit area in the region where the distance from the surface is from d1 (μm) to d2 (μm), and from the surface. Represents the ratio to the area of the inorganic filler component per unit area in the region where the distance is from d2 (μm) to d3 (μm). For example, in the measurement of the inorganic filler component area ratio A 0-5 / A 5-10 , d1 = 0 μm, d2 = 5 μm, d3 = 10 μm, and k = 1.
当然のことではあるが、無機充填材成分面積の比の測定に際しては、画像解析の精度を担保させるべく、条件の校正を行う。斯かる校正は、(無機充填材成分部分のピクセル数)/(断面試料の断面の全ピクセル数)×100の値が、断面試料の無機充填材成分の体積%値と実質的に一致するように2値化閾値を設定することで実施し得る。 As a matter of course, when measuring the ratio of the component areas of the inorganic filler, the conditions are calibrated in order to ensure the accuracy of the image analysis. In such a calibration, the value of (the number of pixels of the inorganic filler component portion) / (the total number of pixels of the cross section of the cross-sectional sample) × 100 substantially matches the volume% value of the inorganic filler component of the cross-sectional sample. It can be carried out by setting a binarization threshold value.
好適な一実施形態において、本発明の硬化体は、
表面の少なくとも一部に導体層を備える基板(「下地基板」)上に設けられた、少なくとも白色無機顔料を含む無機充填材成分を含有した樹脂組成物の硬化体であって、
該硬化体中の不揮発成分を100質量%としたとき、白色無機顔料の含有量が20質量%以上であり、
該硬化体の第1の主面に垂直な方向における硬化体の断面において、硬化体の第1の主面からの距離が0μmから5μmまでの領域における単位面積当たりの無機充填材成分の面積A0-5と、第1の主面からの距離が5μmから10μmまでの領域における単位面積当たりの無機充填材成分の面積A5-10とが、A0-5/A5-10>1.1を満たす。先述のとおり、「第1の主面」とは、該硬化体の、下地基板と接していない側の表面を意味する。
In one preferred embodiment, the cured product of the present invention is:
A cured body of a resin composition containing an inorganic filler component containing at least a white inorganic pigment, which is provided on a substrate (“underlying substrate”) having a conductor layer on at least a part of the surface thereof.
When the non-volatile component in the cured product is 100% by mass, the content of the white inorganic pigment is 20% by mass or more.
Area A of the inorganic filler component per unit area in the region where the distance from the first main surface of the cured body is from 0 μm to 5 μm in the cross section of the cured body in the direction perpendicular to the first main surface of the cured body. 0-5 and the area A 5-10 of the inorganic filler component per unit area in the region where the distance from the first main surface is from 5 μm to 10 μm are A 0-5 / A 5-10 > 1. Satisfy 1. As described above, the "first main surface" means the surface of the cured product on the side not in contact with the base substrate.
より一層優れた光反射率と下地密着性を実現する観点から、本発明の硬化体は、好ましくはA0-5/A5-10≧1.15、より好ましくはA0-5/A5-10≧1.2、さらに好ましくはA0-5/A5-10≧1.22、A0-5/A5-10≧1.24、又はA0-5/A5-10≧1.25を満たす。 From the viewpoint of achieving even better light reflectance and substrate adhesion, the cured product of the present invention is preferably A 0-5 / A 5-10 ≧ 1.15, more preferably A 0-5 / A 5 . -10 ≧ 1.2, more preferably A 0-5 / A 5-10 ≧ 1.22, A 0-5 / A 5-10 ≧ 1.24, or A 0-5 / A 5-10 ≧ 1 Satisfy .25.
A0-5/A5-10比の上限は特に限定されないが、通常、10以下であり、好ましくは8以下、6以下又は5以下である。 The upper limit of the A 0-5 / A 5-10 ratio is not particularly limited, but is usually 10 or less, preferably 8 or less, 6 or less, or 5 or less.
なお、無機充填材成分面積の比を測定するにあたって、硬化体の第1の主面に凹凸が存在する場合、該硬化体(断面試料)の厚さ方向における凹凸の中心線(中心線から下の谷の部分の面積の和をS1、中心線から上の山の部分の面積の和をS2としたとき、S1=S2になるような近似直線)を「第1の主面」の基準位置として扱う。 When measuring the ratio of the component areas of the inorganic filler, if the first main surface of the cured product has irregularities, the center line of the irregularities (below the center line) in the thickness direction of the cured product (cross-sectional sample). When the sum of the areas of the valleys is S1 and the sum of the areas of the mountains above the center line is S2, an approximate straight line such that S1 = S2) is treated as the reference position of the "first main surface". ..
本発明の硬化体の厚さは、プリント配線板の薄型化の観点から、また、本発明の硬化体は薄膜であっても光反射率に優れることから、好ましくは200μm以下、より好ましくは150μm以下又は100μm以下、さらに好ましくは80μm以下、60μm以下又は50μm以下である。硬化体の厚さの下限は、特に限定されないが、通常、10μm以上、15μm以上、20μm以上等とし得る。 The thickness of the cured product of the present invention is preferably 200 μm or less, more preferably 150 μm, from the viewpoint of reducing the thickness of the printed wiring board and because the cured product of the present invention is excellent in light reflectance even if it is a thin film. It is less than or equal to 100 μm or less, more preferably 80 μm or less, 60 μm or less, or 50 μm or less. The lower limit of the thickness of the cured product is not particularly limited, but may be usually 10 μm or more, 15 μm or more, 20 μm or more, and the like.
本発明の硬化体は、高い光反射率を呈すると共に良好な下地密着性を呈する。したがって、本発明の硬化体は、光源からの光を反射させるための光反射用途の硬化体(光反射用硬化体)として好適に使用することができる。具体的には、プリント配線板の最外層上に形成される反射シート用途の硬化体として好適に使用することができる。光源としては、発光ダイオード(LED)、ミニLED、マイクロLED等が挙げられる。また、本発明の硬化体は、プリント配線板のソルダーレジスト層用途の硬化体(ソルダーレジスト層用硬化体)としても好適に使用することができる。したがって、本発明の硬化体は、ソルダーレジスト層及び反射シートの両方を兼ねる層として好適に使用することができる。さらには、本発明の硬化体は、プリント配線板の絶縁層用途の硬化体(絶縁層用硬化体)、特には層間絶縁用途の硬化体(層間絶縁層用硬化体)としても好適に使用することができる。 The cured product of the present invention exhibits high light reflectance and good substrate adhesion. Therefore, the cured product of the present invention can be suitably used as a cured product for light reflection (cured body for light reflection) for reflecting light from a light source. Specifically, it can be suitably used as a cured body for a reflective sheet formed on the outermost layer of a printed wiring board. Examples of the light source include a light emitting diode (LED), a mini LED, a micro LED, and the like. Further, the cured product of the present invention can also be suitably used as a cured product for a solder resist layer of a printed wiring board (cured product for a solder resist layer). Therefore, the cured product of the present invention can be suitably used as a layer that also serves as both a solder resist layer and a reflective sheet. Further, the cured product of the present invention is also suitably used as a cured product for an insulating layer of a printed wiring board (cured product for an insulating layer), particularly as a cured product for an interlayer insulating material (cured product for an interlayer insulating layer). be able to.
本発明の硬化体は、第1の主面近傍の領域に無機充填材成分リッチな相を有するため高い光反射率を呈し、例えば、波長460nmの光に対し、好ましくは80%以上、より好ましくは85%以上、さらに好ましくは90%以上、92%以上、94%以上又は95%以上の反射率を呈する。斯かる光反射率の上限値は100%以下等とし得る。したがって好適な一実施形態において、本発明の硬化体は、波長460nmの光に対する反射率が80%以上である。硬化体の光反射率は、例えば、マルチチャンネル分光器(大塚電子社製、MCPD-7700)を用いて測定することができる。 The cured product of the present invention exhibits high light reflectance because it has a phase rich in the inorganic filler component in the region near the first main surface, and is preferably 80% or more, more preferably 80% or more, for example, with respect to light having a wavelength of 460 nm. Has a reflectance of 85% or more, more preferably 90% or more, 92% or more, 94% or more, or 95% or more. The upper limit of such light reflectance may be 100% or less. Therefore, in one preferred embodiment, the cured product of the present invention has a reflectance of 80% or more with respect to light having a wavelength of 460 nm. The light reflectance of the cured product can be measured using, for example, a multi-channel spectroscope (MCPD-7700, manufactured by Otsuka Electronics Co., Ltd.).
本発明の硬化体は、斯かる高い光反射率を、下地密着性の低下なしに達成し得る。例えば、本発明の硬化体は、下地基板の導体層に対し、好ましくは0.4kgf/cm以上、より好ましくは0.42kgf/cm以上、0.44kgf/cm以上、0.45kgf/cm以上、0.46kgf/cm以上、0.48kgf/cm以上又は0.5kgf/cm以上の密着強度を呈する。斯かる密着強度の上限値は、1kgf/cm以下、0.9kgf/cm以下等とし得る。 The cured product of the present invention can achieve such a high light reflectance without deterioration of the adhesion to the substrate. For example, the cured product of the present invention preferably has 0.4 kgf / cm or more, more preferably 0.42 kgf / cm or more, 0.44 kgf / cm or more, 0.45 kgf / cm or more, with respect to the conductor layer of the underlying substrate. It exhibits adhesion strength of 0.46 kgf / cm or more, 0.48 kgf / cm or more, or 0.5 kgf / cm or more. The upper limit of such adhesion strength may be 1 kgf / cm or less, 0.9 kgf / cm or less, or the like.
本発明の硬化体は、少なくとも白色無機顔料を含む無機充填材成分を含有した樹脂組成物を硬化させてなる。以下、本発明の硬化体を形成する際に用いる樹脂組成物について説明するが、本発明の硬化体中の各成分の含有量は、以下の説明中、樹脂組成物中の各成分の含有量に関連して「樹脂組成物中の不揮発成分を100質量%としたとき」とあるのを、「硬化体中の不揮発成分を100質量%としたとき」と読み替えて適用すればよい。 The cured product of the present invention is obtained by curing a resin composition containing an inorganic filler component containing at least a white inorganic pigment. Hereinafter, the resin composition used for forming the cured product of the present invention will be described, but the content of each component in the cured product of the present invention is the content of each component in the resin composition in the following description. In relation to the above, "when the non-volatile component in the resin composition is 100% by mass" may be read as "when the non-volatile component in the cured product is 100% by mass" and applied.
<樹脂組成物>
本発明の硬化体は、少なくとも白色無機顔料を含む無機充填材成分を含有した樹脂組成物を硬化させて得られる。
<Resin composition>
The cured product of the present invention is obtained by curing a resin composition containing an inorganic filler component containing at least a white inorganic pigment.
-白色無機顔料-
先述のとおり、白色無機顔料は、一実施形態において、波長500nmの光に対する反射率が90%以上である無機化合物、無機充填材のことをいう。
-White inorganic pigment-
As described above, the white inorganic pigment refers to an inorganic compound or an inorganic filler having a reflectance of 90% or more with respect to light having a wavelength of 500 nm in one embodiment.
高い光反射率を呈する硬化体を実現する観点から、樹脂組成物中の白色無機顔料の含有量は、樹脂組成物中の不揮発成分を100質量%としたとき、20質量%以上であり、好ましくは22質量%以上、より好ましくは24質量%以上又は25質量%以上である。 From the viewpoint of realizing a cured product exhibiting high light reflectance, the content of the white inorganic pigment in the resin composition is preferably 20% by mass or more, preferably 20% by mass or more, when the non-volatile component in the resin composition is 100% by mass. Is 22% by mass or more, more preferably 24% by mass or more or 25% by mass or more.
無機充填材成分面積の比(A0-5/A5-10)が特定範囲にある本発明の硬化体においては、下地密着性を低下させることなく、白色無機顔料の含有量を更に高めることができる。例えば、樹脂組成物中の白色無機顔料の含有量は、26質量%以上、28質量%以上、30質量%以上、32質量%以上、34質量%以上、36質量%以上、38質量%以上又は40質量%以上にまで高めてよい。 In the cured product of the present invention in which the ratio of the component areas of the inorganic filler (A 0-5 / A 5-10 ) is in a specific range, the content of the white inorganic pigment is further increased without lowering the adhesion to the substrate. Can be done. For example, the content of the white inorganic pigment in the resin composition is 26% by mass or more, 28% by mass or more, 30% by mass or more, 32% by mass or more, 34% by mass or more, 36% by mass or more, 38% by mass or more, or It may be increased to 40% by mass or more.
樹脂組成物中の白色無機顔料の含有量の上限は、良好な下地密着性を実現する観点から、好ましくは70質量%以下、より好ましくは65質量%以下、さらに好ましくは60質量%以下又は55質量%以下である。 The upper limit of the content of the white inorganic pigment in the resin composition is preferably 70% by mass or less, more preferably 65% by mass or less, still more preferably 60% by mass or less, or 55 from the viewpoint of achieving good substrate adhesion. It is less than mass%.
好適な一実施形態において、樹脂組成物中の不揮発成分を100質量%としたとき、白色無機顔料の含有量は20~60質量%である。 In one preferred embodiment, when the non-volatile component in the resin composition is 100% by mass, the content of the white inorganic pigment is 20 to 60% by mass.
白色無機顔料の材料の例としては、酸化アルミニウム(アルミナ)、酸化チタン、酸化ジルコニウム、酸化マグネシウム、酸化亜鉛、酸化セリウム、酸化アンチモン、酸化スズ、チタン酸バリウム、チタン酸ストロンチウム、チタン酸カルシウム、チタン酸マグネシウム、チタン酸ビスマス、チタン酸ジルコン酸バリウム、ジルコン酸バリウム、ジルコン酸カルシウム等の白色金属酸化物;硫化亜鉛、硫化ストロンチウム等の白色金属硫化物;水酸化アルミニウム、水酸化マグネシウム、水酸化カルシウム等の白色金属水酸化物;窒化ホウ素、窒化アルミニウム、窒化マンガン等の白色金属窒化物;炭酸カルシウム、炭酸バリウム、炭酸マグネシウム、炭酸ストロンチウム、炭酸鉛等の白色金属炭酸塩;硫酸バリウム、硫酸カルシウム、硫酸鉛等の白色金属硫酸塩;リン酸亜鉛、リン酸チタン、リン酸ジルコニウム、リン酸タングステン酸ジルコニウム等の白色金属リン酸塩;ホウ酸アルミニウム等の白色金属ホウ酸塩;コーディエライト、タルク、クレー、雲母、ハイドロタルサイト、ベーマイト等の白色鉱物類等が挙げられる。 Examples of materials for white inorganic pigments are aluminum oxide (alumina), titanium oxide, zirconium oxide, magnesium oxide, zinc oxide, cerium oxide, antimony oxide, tin oxide, barium titanate, strontium titanate, calcium titanate, and titanium. White metal oxides such as magnesium acid, bismuth titanate, barium zirconate titanate, barium zirconate, calcium zirconate; white metal sulfides such as zinc sulfide and strontium sulfide; aluminum hydroxide, magnesium hydroxide, calcium hydroxide White metal hydroxides such as; white metal nitrides such as boron nitride, aluminum nitride, manganese nitride; white metal carbonates such as calcium carbonate, barium carbonate, magnesium carbonate, strontium carbonate, lead carbonate; barium sulfate, calcium sulfate, etc. White metal sulfates such as lead sulfate; white metal phosphates such as zinc phosphate, titanium phosphate, zirconium phosphate, zirconium tungstate phosphate; white metal borates such as aluminum borate; cordierite, talc , Clay, mica, hydrotalcite, white minerals such as boehmite and the like.
これらの中でも、白色無機顔料は、酸化アルミニウム、酸化チタン、酸化ジルコニウム、酸化マグネシウム、チタン酸バリウム、酸化亜鉛、酸化セリウム、及び炭酸カルシウムから選ばれることが好ましく、酸化チタンが特に好適である。酸化チタンとしては、ルチル型、アナタース型、及びブルカイト型のいずれを用いてもよいが、反射率をより向上させる観点から、ルチル型が好ましい。酸化チタンは、硫酸法、塩素法などの方法により得られたものを用いることができる。白色無機顔料の材料は、1種類単独であってもよく、2種類以上の混合物であってもよい。白色無機顔料の形状は、例えば、不定形状、破砕状、鱗片状又は球状の何れであってもよい。 Among these, the white inorganic pigment is preferably selected from aluminum oxide, titanium oxide, zirconium oxide, magnesium oxide, barium titanate, zinc oxide, cerium oxide, and calcium carbonate, and titanium oxide is particularly preferable. As the titanium oxide, any of a rutile type, anatase type, and brookite type may be used, but the rutile type is preferable from the viewpoint of further improving the reflectance. As the titanium oxide, those obtained by a method such as a sulfuric acid method or a chlorine method can be used. The material of the white inorganic pigment may be one kind alone or a mixture of two or more kinds. The shape of the white inorganic pigment may be, for example, an indefinite shape, a crushed shape, a scaly shape, or a spherical shape.
白色無機顔料の市販品としては、例えば、堺化学工業社製の「PX3788」;石原産業社製のタイペーク「CR-50」、「CR-57」、「CR-80」、「CR-90」、「CR-93」、「CR-95」、「CR-97」、「CR-60」、「CR-63」、「CR-67」、「CR-58」、「CR-85」、「UT771」;デュポン社製のタイピュア「R-100」、「R-101」、「R-102」、「R-103」、「R-104」、「R-105」、「R-108」、「R-900」、「R-902」、「R-960」、「R-706」、「R-931」;日本軽金属社製「AHP300」;昭和電工社製アルナビーズ「CB-P05」、「CB-A30S」などが挙げられる。 Commercially available white inorganic pigments include, for example, "PX3788" manufactured by Sakai Chemical Industry Co., Ltd .; Typake "CR-50", "CR-57", "CR-80", "CR-90" manufactured by Ishihara Sangyo Co., Ltd. , "CR-93", "CR-95", "CR-97", "CR-60", "CR-63", "CR-67", "CR-58", "CR-85", " UT771 "; Typure" R-100 "," R-101 "," R-102 "," R-103 "," R-104 "," R-105 "," R-108 ", manufactured by DuPont. "R-900", "R-902", "R-960", "R-706", "R-931"; Nippon Light Metal Co., Ltd. "AHP300"; Showa Denko Co., Ltd. Arna beads "CB-P05", " CB-A30S "and the like.
白色無機顔料の比表面積としては、好ましくは0.5m2/g以上、より好ましくは1m2/g以上、特に好ましくは2m2/g以上である。上限に特段の制限は無いが、好ましくは80m2/g以下、70m2/g以下又は60m2/g以下である。比表面積は、BET法に従って、比表面積測定装置(マウンテック社製Macsorb HM-1210)を使用して試料表面に窒素ガスを吸着させ、BET多点法を用いて比表面積を算出することで得られる。 The specific surface area of the white inorganic pigment is preferably 0.5 m 2 / g or more, more preferably 1 m 2 / g or more, and particularly preferably 2 m 2 / g or more. The upper limit is not particularly limited, but is preferably 80 m 2 / g or less, 70 m 2 / g or less, or 60 m 2 / g or less. The specific surface area is obtained by adsorbing nitrogen gas on the sample surface using a specific surface area measuring device (Macsorb HM-1210 manufactured by Mountech) according to the BET method and calculating the specific surface area using the BET multipoint method. ..
白色無機顔料の平均粒径は、本発明の所望の効果を顕著に得る観点から、好ましくは0.01μm以上、より好ましくは0.05μm以上、さらに好ましくは0.1μm以上であり、好ましくは10μm以下、より好ましくは5μm以下、さらに好ましくは2μm以下又は1μm以下である。 The average particle size of the white inorganic pigment is preferably 0.01 μm or more, more preferably 0.05 μm or more, still more preferably 0.1 μm or more, and preferably 10 μm from the viewpoint of remarkably obtaining the desired effect of the present invention. Below, it is more preferably 5 μm or less, still more preferably 2 μm or less or 1 μm or less.
白色無機顔料の平均粒径は、ミー(Mie)散乱理論に基づくレーザー回折・散乱法により測定することができる。具体的には、レーザー回折散乱式粒径分布測定装置により、白色無機顔料の粒径分布を体積基準で作成し、そのメディアン径を平均粒径とすることで測定することができる。測定サンプルは、白色無機顔料100mg、メチルエチルケトン10gをバイアル瓶に秤取り、超音波にて10分間分散させたものを使用することができる。測定サンプルを、レーザー回折式粒径分布測定装置を使用して、使用光源波長を青色及び赤色とし、フローセル方式で白色無機顔料の体積基準の粒径分布を測定し、得られた粒径分布からメディアン径として平均粒径を算出できる。レーザー回折式粒径分布測定装置としては、例えば堀場製作所社製「LA-960」等が挙げられる。 The average particle size of the white inorganic pigment can be measured by a laser diffraction / scattering method based on the Mie scattering theory. Specifically, it can be measured by creating a particle size distribution of a white inorganic pigment on a volume basis using a laser diffraction / scattering type particle size distribution measuring device and using the median diameter as the average particle size. As the measurement sample, 100 mg of a white inorganic pigment and 10 g of methyl ethyl ketone can be weighed in a vial and dispersed by ultrasonic waves for 10 minutes. The measurement sample was measured using a laser diffraction type particle size distribution measuring device, the light source wavelengths used were blue and red, and the volume-based particle size distribution of the white inorganic pigment was measured by the flow cell method. The average particle size can be calculated as the median diameter. Examples of the laser diffraction type particle size distribution measuring device include "LA-960" manufactured by HORIBA, Ltd.
白色無機顔料は、耐湿性及び分散性を高める観点から、表面処理剤で処理されていることが好ましい。表面処理剤は、1種類単独で用いてもよく、2種類以上を任意に組み合わせて用いてもよい。表面処理剤としては、例えば、ビニル系シランカップリング剤、エポキシ系シランカップリング剤、スチリル系シランカップリング剤、(メタ)アクリル系シランカップリング剤、アミノ系シランカップリング剤、イソシアヌレート系シランカップリング剤、ウレイド系シランカップリング剤、メルカプト系シランカップリング剤、イソシアネート系シランカップリング剤、酸無水物系シランカップリング剤、アルキルシランカップリング剤、フェニルシランカップリング剤等のシランカップリング剤が挙げられる。反射率を向上させる観点、無機充填材成分面積の比(A0-5/A5-10)が特定範囲にある硬化体を実現し易い観点から、表面処理剤は、窒素原子を含まない(窒素原子不含の)表面処理剤であることが好ましく、より好ましくは、窒素原子を含まない(窒素原子不含の)シランカップリング剤であることが好ましい。窒素原子を含まない(窒素原子不含の)シランカップリング剤としては、フェニルシランカップリング剤、アルキルシランカップリング剤、エポキシ系シランカップリング剤、ビニル系シランカップリング剤、(メタ)アクリル系シランカップリング剤及びスチリル系シランカップリング剤から選ばれるシランカップリング剤が挙げられる。 The white inorganic pigment is preferably treated with a surface treatment agent from the viewpoint of enhancing moisture resistance and dispersibility. One type of surface treatment agent may be used alone, or two or more types may be used in any combination. Examples of the surface treatment agent include vinyl-based silane coupling agents, epoxy-based silane coupling agents, styryl-based silane coupling agents, (meth) acrylic-based silane coupling agents, amino-based silane coupling agents, and isocyanurate-based silanes. Silane couplings such as coupling agents, ureido-based silane coupling agents, mercapto-based silane coupling agents, isocyanate-based silane coupling agents, acid anhydride-based silane coupling agents, alkylsilane coupling agents, and phenylsilane coupling agents. Agents are mentioned. The surface treatment agent does not contain nitrogen atoms from the viewpoint of improving the reflectance and from the viewpoint of easily realizing a cured product in which the ratio of the component areas of the inorganic filler (A 0-5 / A 5-10 ) is in a specific range (A 0-5 / A 5-10). It is preferably a surface treatment agent (free of nitrogen atoms), and more preferably a silane coupling agent containing no nitrogen atoms (free of nitrogen atoms). Examples of the silane coupling agent containing no nitrogen atom (without nitrogen atom) include a phenylsilane coupling agent, an alkylsilane coupling agent, an epoxy-based silane coupling agent, a vinyl-based silane coupling agent, and a (meth) acrylic-based agent. Examples thereof include a silane coupling agent selected from a silane coupling agent and a styryl-based silane coupling agent.
フェニルシランカップリング剤としては、例えば、フェニルトリメトキシシラン、フェニルトリエトキシシラン等が挙げられる。アルキルシランカップリング剤としては、例えば、メチルトリメトキシシラン、ジメチルジメトキシシラン、メチルトリエトキシシラン、ジメチルジエトキシシラン、n-プロピルトリメトキシシラン、n-プロピルトリエトキシシラン、ヘキシルトリメトキシシラン、ヘキシルトリエトキシシラン、オクチルトリエトキシシラン、デシルトリメトキシシラン、1,6-ビス(トリメトキシシリル)ヘキサン等が挙げられる。エポキシ系シランカップリング剤としては、例えば、2-(3,4-エポキシシクロヘキシル)エチルトリメトキシシラン、3-グリシドキシプロピルメチルジメトキシシラン、3-グリシドキシプロピルトリメトキシシラン、3-グリシドキシプロピルメチルジエトキシシラン、3-グリシドキシプロピルトリエトキシシラン等が挙げられる。 Examples of the phenylsilane coupling agent include phenyltrimethoxysilane and phenyltriethoxysilane. Examples of the alkylsilane coupling agent include methyltrimethoxysilane, dimethyldimethoxysilane, methyltriethoxysilane, dimethyldiethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, hexyltrimethoxysilane, and hexyltri. Examples thereof include ethoxysilane, octyltriethoxysilane, decyltrimethoxysilane, and 1,6-bis (trimethoxysilyl) hexane. Examples of the epoxy-based silane coupling agent include 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, 3-glycidoxypropylmethyldimethoxysilane, 3-glycidoxypropyltrimethoxysilane, and 3-glycid. Examples thereof include xypropylmethyldiethoxysilane and 3-glycidoxypropyltriethoxysilane.
ビニル系シランカップリング剤としては、例えば、ビニルトリメトキシシラン、ビニルトリエトキシシラン等が挙げられる。(メタ)アクリル系シランカップリング剤としては、例えば、3-メタクリロキシプロピルメチルジメトキシシラン、3-メタクリロキシプロピルトリメトキシシラン、3-メタクリロキシプロピルメチルジエトキシシラン、3-メタクリロキシプロピルトリエトキシシラン、3-アクリロキシプロピルトリメトキシシラン等が挙げられる。スチリル系シランカップリング剤としては、例えば、p-スチリルトリメトキシシラン等が挙げられる。 Examples of the vinyl-based silane coupling agent include vinyltrimethoxysilane and vinyltriethoxysilane. Examples of the (meth) acrylic silane coupling agent include 3-methacryloxypropylmethyldimethoxysilane, 3-methacryloxypropyltrimethoxysilane, 3-methacryloxypropylmethyldiethoxysilane, and 3-methacryloxypropyltriethoxysilane. , 3-Acryloxypropyltrimethoxysilane and the like. Examples of the styryl-based silane coupling agent include p-styryltrimethoxysilane.
表面処理剤の市販品としては、例えば、信越化学工業社製の「KBM-103」、「KBE-103」(フェニルシランカップリング剤);「KBM-13」、「KBM-22」、「KBE-13」、「KBE-22」、「KBM-3033」、「KBE-3033」、「KBM-3063」、「KBE-3063」、「KBE-3083」、「KBM-3103C」、「KBM-3066」、「KBM-7103」(アルキルシランカップリング剤);「KBM-1003」、「KBE-1003」(ビニル系シランカップリング剤);「KBM-303」、「KBM-402」、「KBM-403」、「KBE-402」、「KBE-403」(エポキシ系シランカップリング剤);「KBM-1403」(スチリル系シランカップリング剤);「KBM-502」、「KBM-503」、「KBE-502」、「KBE-503」、「KBM-5103」((メタ)アクリル系シランカップリング剤)等が挙げられる。 Commercially available surface treatment agents include, for example, "KBM-103" and "KBE-103" (phenylsilane coupling agent) manufactured by Shin-Etsu Chemical Co., Ltd .; "KBM-13", "KBM-22", and "KBE". -13, "KBE-22", "KBM-3033", "KBE-3033", "KBM-3063", "KBE-3063", "KBE-3083", "KBM-3103C", "KBM-3066" , "KBM-7103" (alkylsilane coupling agent); "KBM-1003", "KBE-1003" (vinyl-based silane coupling agent); "KBM-303", "KBM-402", "KBM-" 403 "," KBE-402 "," KBE-403 "(epoxy-based silane coupling agent);" KBM-1403 "(styryl-based silane coupling agent);" KBM-502 "," KBM-503 "," Examples thereof include "KBE-502", "KBE-503", and "KBM-5103" ((meth) acrylic silane coupling agent).
表面処理剤による表面処理の程度は、白色無機顔料の分散性向上の観点から、所定の範囲に収まることが好ましい。具体的には、白色無機顔料100質量部は、0.2質量部~5質量部の表面処理剤で表面処理されていることが好ましく、0.2質量部~3質量部で表面処理されていることが好ましく、0.3質量部~2質量部で表面処理されていることが好ましい。 The degree of surface treatment with the surface treatment agent is preferably within a predetermined range from the viewpoint of improving the dispersibility of the white inorganic pigment. Specifically, 100 parts by mass of the white inorganic pigment is preferably surface-treated with 0.2 parts by mass to 5 parts by mass of a surface treatment agent, and is surface-treated with 0.2 parts by mass to 3 parts by mass. It is preferable that the surface is treated with 0.3 parts by mass to 2 parts by mass.
表面処理剤による表面処理の程度は、白色無機顔料の単位表面積当たりのカーボン量によって評価することができる。白色無機顔料の単位表面積当たりのカーボン量は、白色無機顔料の分散性向上の観点から、0.02mg/m2以上が好ましく、0.1mg/m2以上がより好ましく、0.2mg/m2以上が更に好ましい。一方、樹脂ワニスの溶融粘度及びシート形態での溶融粘度の上昇を抑制する観点から、1mg/m2以下が好ましく、0.8mg/m2以下がより好ましく、0.5mg/m2以下が更に好ましい。 The degree of surface treatment with the surface treatment agent can be evaluated by the amount of carbon per unit surface area of the white inorganic pigment. The amount of carbon per unit surface area of the white inorganic pigment is preferably 0.02 mg / m 2 or more, more preferably 0.1 mg / m 2 or more, and 0.2 mg / m 2 from the viewpoint of improving the dispersibility of the white inorganic pigment. The above is more preferable. On the other hand, from the viewpoint of suppressing an increase in the melt viscosity of the resin varnish and the melt viscosity in the sheet form, 1 mg / m 2 or less is preferable, 0.8 mg / m 2 or less is more preferable, and 0.5 mg / m 2 or less is further preferable. preferable.
白色無機顔料の単位表面積当たりのカーボン量は、表面処理後の白色無機顔料を溶剤(例えば、メチルエチルケトン(MEK))により洗浄処理した後に測定することができる。具体的には、溶剤として十分な量のMEKを表面処理剤で表面処理された白色無機顔料に加えて、25℃で5分間超音波洗浄する。上澄液を除去し、固形分を乾燥させた後、カーボン分析計を用いて白色無機顔料の単位表面積当たりのカーボン量を測定することができる。カーボン分析計としては、堀場製作所社製「EMIA-320V」等を使用することができる。 The amount of carbon per unit surface area of the white inorganic pigment can be measured after the surface-treated white inorganic pigment is washed with a solvent (for example, methyl ethyl ketone (MEK)). Specifically, a sufficient amount of MEK as a solvent is added to the white inorganic pigment surface-treated with a surface treatment agent, and ultrasonic cleaning is performed at 25 ° C. for 5 minutes. After removing the supernatant and drying the solid content, the amount of carbon per unit surface area of the white inorganic pigment can be measured using a carbon analyzer. As the carbon analyzer, "EMIA-320V" manufactured by HORIBA, Ltd. or the like can be used.
-他の無機充填材-
樹脂組成物は、少なくとも白色無機顔料を含む限りにおいて、他の無機充填材を含有してもよい。斯かる他の無機充填材としては、白色無機顔料とは異なる無機充填材である限り特に限定されず、例えば、波長500nmの光に対する反射率が90%未満である無機充填材を用いてよい。
-Other inorganic fillers-
The resin composition may contain other inorganic fillers as long as it contains at least a white inorganic pigment. The other inorganic filler is not particularly limited as long as it is an inorganic filler different from the white inorganic pigment, and for example, an inorganic filler having a reflectance of less than 90% for light having a wavelength of 500 nm may be used.
中でも、無機充填材成分面積の比(A0-5/A5-10)が特定範囲にある硬化体を実現し易い観点から、他の無機充填材としては、シリカが好適である。シリカとしては、例えば、無定形シリカ、溶融シリカ、結晶シリカ、合成シリカ、中空シリカ等が挙げられる。また、シリカとしては、球状シリカが好ましい。シリカの比表面積及び平均粒径は、白色無機顔料と同様である。シリカは、1種類単独で用いてもよく、2種類以上を組み合わせて用いてもよい。 Among them, silica is preferable as another inorganic filler from the viewpoint that it is easy to realize a cured product in which the ratio of the component areas of the inorganic filler (A 0-5 / A 5-10 ) is in a specific range. Examples of silica include amorphous silica, fused silica, crystalline silica, synthetic silica, hollow silica and the like. Further, as silica, spherical silica is preferable. The specific surface area and average particle size of silica are the same as those of the white inorganic pigment. One type of silica may be used alone, or two or more types may be used in combination.
シリカの市販品としては、例えば、デンカ社製の「UFP-30」;日鉄ケミカル&マテリアル社製の「SP60-05」、「SP507-05」;アドマテックス社製の「YC100C」、「YA050C」、「YA050C-MJE」、「YA010C」;トクヤマ社製の「シルフィルNSS-3N」、「シルフィルNSS-4N」、「シルフィルNSS-5N」;アドマテックス社製の「SC2500SQ」、「SO-C4」、「SO-C2」、「SO-C1」;などが挙げられる。 Examples of commercially available silica products include "UFP-30" manufactured by Denka Co., Ltd .; "SP60-05" and "SP507-05" manufactured by Nittetsu Chemical & Materials Co., Ltd .; "YC100C" and "YA050C" manufactured by Admatex Co., Ltd. , "YA050C-MJE", "YA010C"; "Silfil NSS-3N", "Silfil NSS-4N", "Silfil NSS-5N" manufactured by Tokuyama; "SC2500SQ", "SO-C4" manufactured by Admatex. , "SO-C2", "SO-C1"; and the like.
シリカ等の他の無機充填材は、耐湿性及び分散性を高める観点から、表面処理剤で処理されていることが好ましい。表面処理剤としては、白色無機顔料における表面処理剤と同様のものが挙げられる。他の無機充填材の表面処理剤による表面処理の程度は、白色無機顔料と同様である。 Other inorganic fillers such as silica are preferably treated with a surface treatment agent from the viewpoint of enhancing moisture resistance and dispersibility. Examples of the surface treatment agent include those similar to the surface treatment agent in the white inorganic pigment. The degree of surface treatment of other inorganic fillers with the surface treatment agent is the same as that of the white inorganic pigment.
樹脂組成物中の他の無機充填材の含有量は、本発明の効果を顕著に得る観点から、樹脂組成物中の不揮発成分を100質量%としたとき、好ましくは1質量%以上、より好ましくは5質量%以上、さらに好ましくは10質量%以上、特に好ましくは15質量%以上である。他の無機充填材の含有量の上限は、好ましくは70質量%以下、より好ましくは50質量%以下、さらに好ましくは40質量%以下、特に好ましくは35質量%以下である。 The content of the other inorganic filler in the resin composition is preferably 1% by mass or more, more preferably 1% by mass or more, when the non-volatile component in the resin composition is 100% by mass from the viewpoint of remarkably obtaining the effect of the present invention. Is 5% by mass or more, more preferably 10% by mass or more, and particularly preferably 15% by mass or more. The upper limit of the content of the other inorganic filler is preferably 70% by mass or less, more preferably 50% by mass or less, still more preferably 40% by mass or less, and particularly preferably 35% by mass or less.
白色無機顔料と他の無機充填材の合計の含有量、すなわち、無機充填材成分の合計の含有量は、高い光反射率を呈すると共に良好な下地密着性を呈する硬化体を実現する観点から、樹脂組成物中の不揮発成分を100質量%としたとき、好ましくは20質量%以上、より好ましくは30質量%以上、さらに好ましくは40質量%以上、特に好ましくは50質量%以上であり、好ましくは90質量%以下、より好ましくは80質量%以下、さらに好ましくは75質量%以下、特に好ましくは70質量%以下である。 The total content of the white inorganic pigment and other inorganic fillers, that is, the total content of the inorganic filler components, is from the viewpoint of realizing a cured product having high light reflectance and good substrate adhesion. When the non-volatile component in the resin composition is 100% by mass, it is preferably 20% by mass or more, more preferably 30% by mass or more, further preferably 40% by mass or more, and particularly preferably 50% by mass or more, preferably 50% by mass or more. It is 90% by mass or less, more preferably 80% by mass or less, still more preferably 75% by mass or less, and particularly preferably 70% by mass or less.
白色無機顔料に対するシリカ等の他の無機充填材の質量比(他の無機充填材の質量/白色無機顔料の質量)は、高い光反射率を呈すると共に良好な下地密着性を呈する硬化体を実現する観点から、好ましくは0.1以上、より好ましくは0.2以上、さらに好ましくは0.5以上、特に好ましくは0.8以上であり、好ましくは4以下、より好ましくは4以下、さらに好ましくは2以下、特に好ましくは1.5以下である。 The mass ratio of other inorganic fillers such as silica to the white inorganic pigment (mass of other inorganic fillers / mass of white inorganic pigments) realizes a cured product that exhibits high light reflectance and good substrate adhesion. From the viewpoint, it is preferably 0.1 or more, more preferably 0.2 or more, still more preferably 0.5 or more, particularly preferably 0.8 or more, preferably 4 or less, more preferably 4 or less, still more preferable. Is 2 or less, particularly preferably 1.5 or less.
本発明の硬化体を形成するために用いる樹脂組成物は、樹脂として、熱硬化性樹脂を含む。熱硬化性樹脂としては、プリント配線板の絶縁層を形成する際に使用される従来公知の熱硬化性樹脂を用いることができ、中でも、無機充填材成分面積の比(A0-5/A5-10)が特定範囲にある硬化体を実現し易い観点から、エポキシ樹脂が好ましい。したがって、一実施形態において樹脂組成物は熱硬化性樹脂を含み、好適な一実施形態において熱硬化性樹脂はエポキシ樹脂を含む。 The resin composition used for forming the cured product of the present invention contains a thermosetting resin as the resin. As the thermosetting resin, a conventionally known thermosetting resin used for forming the insulating layer of the printed wiring board can be used, and among them, the ratio of the component area of the inorganic filler (A 0-5 / A). Epoxy resin is preferable from the viewpoint that it is easy to realize a cured product in which 5-10 ) is in a specific range. Therefore, in one embodiment the resin composition comprises a thermosetting resin and in one preferred embodiment the thermosetting resin comprises an epoxy resin.
-エポキシ樹脂-
エポキシ樹脂とは、エポキシ基を有する硬化性樹脂を意味する。エポキシ樹脂は、1種類単独で用いてもよく、2種類以上を組み合わせて用いてもよい。
-Epoxy resin-
The epoxy resin means a curable resin having an epoxy group. One type of epoxy resin may be used alone, or two or more types may be used in combination.
エポキシ樹脂としては、例えば、ビキシレノール型エポキシ樹脂、ビスフェノールA型エポキシ樹脂、ビスフェノールF型エポキシ樹脂、ビスフェノールS型エポキシ樹脂、ビスフェノールAF型エポキシ樹脂、水添ビスフェノールA型エポキシ樹脂、ジシクロペンタジエン型エポキシ樹脂、トリスフェノール型エポキシ樹脂、ナフトールノボラック型エポキシ樹脂、フェノールノボラック型エポキシ樹脂、tert-ブチル-カテコール型エポキシ樹脂、ナフタレン型エポキシ樹脂、ナフトール型エポキシ樹脂、アントラセン型エポキシ樹脂、グリシジルアミン型エポキシ樹脂、グリシジルエステル型エポキシ樹脂、クレゾールノボラック型エポキシ樹脂、フェノールアラルキル型エポキシ樹脂、ビフェニル型エポキシ樹脂、線状脂肪族エポキシ樹脂、ブタジエン構造を有するエポキシ樹脂、脂環式エポキシ樹脂、複素環式エポキシ樹脂、スピロ環含有エポキシ樹脂、シクロヘキサン型エポキシ樹脂、シクロヘキサンジメタノール型エポキシ樹脂、ナフチレンエーテル型エポキシ樹脂、トリメチロール型エポキシ樹脂、テトラフェニルエタン型エポキシ樹脂、イソシアヌラート型エポキシ樹脂、フェノールフタルイミジン型エポキシ樹脂、フェノールフタレイン型エポキシ樹脂等が挙げられる。 Examples of the epoxy resin include bixilenol type epoxy resin, bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin, bisphenol AF type epoxy resin, hydrogenated bisphenol A type epoxy resin, and dicyclopentadiene type epoxy. Resin, Trisphenol type epoxy resin, naphthol novolac type epoxy resin, phenol novolac type epoxy resin, tert-butyl-catechol type epoxy resin, naphthalene type epoxy resin, naphthol type epoxy resin, anthracene type epoxy resin, glycidylamine type epoxy resin, Glycidyl ester type epoxy resin, cresol novolac type epoxy resin, phenol aralkyl type epoxy resin, biphenyl type epoxy resin, linear aliphatic epoxy resin, epoxy resin having a butadiene structure, alicyclic epoxy resin, heterocyclic epoxy resin, spiro Ring-containing epoxy resin, cyclohexane type epoxy resin, cyclohexanedimethanol type epoxy resin, naphthylene ether type epoxy resin, trimethylol type epoxy resin, tetraphenylethane type epoxy resin, isocyanurate type epoxy resin, phenolphthalimidine type epoxy Examples thereof include resins and phenolphthaline type epoxy resins.
樹脂組成物は、エポキシ樹脂として、1分子中に2個以上のエポキシ基を有するエポキシ樹脂を含むことが好ましい。エポキシ樹脂の不揮発成分100質量%に対して、1分子中に2個以上のエポキシ基を有するエポキシ樹脂の割合は、好ましくは50質量%以上、より好ましくは60質量%以上、特に好ましくは70質量%以上である。 The resin composition preferably contains, as the epoxy resin, an epoxy resin having two or more epoxy groups in one molecule. The ratio of the epoxy resin having two or more epoxy groups in one molecule is preferably 50% by mass or more, more preferably 60% by mass or more, and particularly preferably 70% by mass with respect to 100% by mass of the non-volatile component of the epoxy resin. % Or more.
エポキシ樹脂には、温度25℃で固体状のエポキシ樹脂(以下、「固体状エポキシ樹脂」ともいう。)と、温度25℃で液状のエポキシ樹脂(以下、「液状エポキシ樹脂」ともいう。)とがある。本発明の硬化体を形成するために用いる樹脂組成物は、エポキシ樹脂として、固体状エポキシ樹脂のみを含んでいてもよく、或いは液状エポキシ樹脂のみを含んでいてもよく、或いは固体状エポキシ樹脂と液状エポキシ樹脂とを組み合わせて含んでいてもよい。 The epoxy resin includes a solid epoxy resin at a temperature of 25 ° C. (hereinafter, also referred to as “solid epoxy resin”) and a liquid epoxy resin at a temperature of 25 ° C. (hereinafter, also referred to as “liquid epoxy resin”). There is. The resin composition used for forming the cured product of the present invention may contain only a solid epoxy resin, may contain only a liquid epoxy resin, or may contain only a liquid epoxy resin, or may be a solid epoxy resin. It may be contained in combination with a liquid epoxy resin.
固体状エポキシ樹脂としては、1分子中に3個以上のエポキシ基を有する固体状エポキシ樹脂が好ましく、1分子中に3個以上のエポキシ基を有する芳香族系の固体状エポキシ樹脂がより好ましい。 As the solid epoxy resin, a solid epoxy resin having three or more epoxy groups in one molecule is preferable, and an aromatic solid epoxy resin having three or more epoxy groups in one molecule is more preferable.
固体状エポキシ樹脂としては、ビキシレノール型エポキシ樹脂、ナフタレン型エポキシ樹脂、ナフタレン型4官能エポキシ樹脂、ナフトールノボラック型エポキシ樹脂、クレゾールノボラック型エポキシ樹脂、ジシクロペンタジエン型エポキシ樹脂、トリスフェノール型エポキシ樹脂、ナフトール型エポキシ樹脂、ビフェニル型エポキシ樹脂、ナフチレンエーテル型エポキシ樹脂、アントラセン型エポキシ樹脂、ビスフェノールA型エポキシ樹脂、ビスフェノールAF型エポキシ樹脂、フェノールアラルキル型エポキシ樹脂、テトラフェニルエタン型エポキシ樹脂、フェノールフタルイミジン型エポキシ樹脂、フェノールフタレイン型エポキシ樹脂が好ましい。 Examples of the solid epoxy resin include bixilenol type epoxy resin, naphthalene type epoxy resin, naphthalene type tetrafunctional epoxy resin, naphthol novolac type epoxy resin, cresol novolac type epoxy resin, dicyclopentadiene type epoxy resin, and trisphenol type epoxy resin. Naftor type epoxy resin, biphenyl type epoxy resin, naphthylene ether type epoxy resin, anthracene type epoxy resin, bisphenol A type epoxy resin, bisphenol AF type epoxy resin, phenol aralkyl type epoxy resin, tetraphenylethane type epoxy resin, phenol phthali Midin type epoxy resin and phenol phthalein type epoxy resin are preferable.
固体状エポキシ樹脂の具体例としては、DIC社製の「HP4032H」(ナフタレン型エポキシ樹脂);DIC社製の「HP-4700」、「HP-4710」(ナフタレン型4官能エポキシ樹脂);DIC社製の「N-690」(クレゾールノボラック型エポキシ樹脂);DIC社製の「N-695」(クレゾールノボラック型エポキシ樹脂);DIC社製の「HP-7200」、「HP-7200HH」、「HP-7200H」、「HP-7200L」(ジシクロペンタジエン型エポキシ樹脂);DIC社製の「EXA-7311」、「EXA-7311-G3」、「EXA-7311-G4」、「EXA-7311-G4S」、「HP6000」(ナフチレンエーテル型エポキシ樹脂);日本化薬社製の「EPPN-502H」(トリスフェノール型エポキシ樹脂);日本化薬社製の「NC7000L」(ナフトールノボラック型エポキシ樹脂);日本化薬社製の「NC3000H」、「NC3000」、「NC3000L」、「NC3000FH」、「NC3100」(ビフェニル型エポキシ樹脂);日鉄ケミカル&マテリアル社製の「ESN475V」(ナフタレン型エポキシ樹脂);日鉄ケミカル&マテリアル社製の「ESN485」(ナフトール型エポキシ樹脂);日鉄ケミカル&マテリアル社製の「ESN375」(ジヒドロキシナフタレン型エポキシ樹脂);三菱ケミカル社製の「YX4000H」、「YX4000」、「YX4000HK」、「YL7890」(ビキシレノール型エポキシ樹脂);三菱ケミカル社製の「YL6121」(ビフェニル型エポキシ樹脂);三菱ケミカル社製の「YX8800」(アントラセン型エポキシ樹脂);三菱ケミカル社製の「YX7700」(フェノールアラルキル型エポキシ樹脂);大阪ガスケミカル社製の「PG-100」、「CG-500」;三菱ケミカル社製の「YX7760」(ビスフェノールAF型エポキシ樹脂);三菱ケミカル社製の「YL7800」(フルオレン型エポキシ樹脂);三菱ケミカル社製の「jER1010」(ビスフェノールA型エポキシ樹脂);三菱ケミカル社製の「jER1031S」(テトラフェニルエタン型エポキシ樹脂);日本化薬社製の「WHR991S」(フェノールフタルイミジン型エポキシ樹脂)等が挙げられる。これらは、1種類単独で用いてもよく、2種類以上を組み合わせて用いてもよい。 Specific examples of the solid epoxy resin include "HP4032H" (naphthalene type epoxy resin) manufactured by DIC; "HP-4700" and "HP-4710" (naphthalen type tetrafunctional epoxy resin) manufactured by DIC; DIC. "N-690" (cresol novolac type epoxy resin); DIC "N-695" (cresol novolac type epoxy resin); DIC "HP-7200", "HP-7200HH", "HP" -7200H "," HP-7200L "(dicyclopentadiene type epoxy resin);" EXA-7311 "," EXA-7311-G3 "," EXA-7311-G4 "," EXA-7311-G4S "manufactured by DIC. , "HP6000" (naphthylene ether type epoxy resin); "EPPN-502H" (trisphenol type epoxy resin) manufactured by Nippon Kayaku Co., Ltd .; "NC7000L" (naphthol novolac type epoxy resin) manufactured by Nihon Kayaku Co., Ltd.; "NC3000H", "NC3000", "NC3000L", "NC3000FH", "NC3100" (biphenyl type epoxy resin) manufactured by Nippon Kayaku Co., Ltd .; "ESN475V" (naphthalene type epoxy resin) manufactured by Nittetsu Chemical & Materials Co., Ltd.; "ESN485" (naphthol type epoxy resin) manufactured by Nittetsu Chemical &Materials; "ESN375" (dihydroxynaphthalene type epoxy resin) manufactured by Nittetsu Chemical &Materials; "YX4000H", "YX4000", manufactured by Mitsubishi Chemical Co., Ltd. "YX4000HK", "YL7890" (bixilenol type epoxy resin); "YL6121" (biphenyl type epoxy resin) manufactured by Mitsubishi Chemical Co., Ltd .; "YX8800" (anthracen type epoxy resin) manufactured by Mitsubishi Chemical Co., Ltd. "YX7700" (phenol aralkyl type epoxy resin); "PG-100" and "CG-500" manufactured by Osaka Gas Chemical Co., Ltd .; "YX7760" (bisphenol AF type epoxy resin) manufactured by Mitsubishi Chemical Co., Ltd .; "YL7800" (fluorene type epoxy resin); "jER1010" manufactured by Mitsubishi Chemical Co., Ltd. (bisphenol A type epoxy resin); "jER1031S" manufactured by Mitsubishi Chemical Co., Ltd. (tetraphenylethane type epoxy resin); WHR991S ”(phenol phthalimidine type epoxy resin) and the like can be mentioned. These may be used individually by 1 type, or may be used in combination of 2 or more types.
液状エポキシ樹脂としては、1分子中に2個以上のエポキシ基を有する液状エポキシ樹脂が好ましい。 As the liquid epoxy resin, a liquid epoxy resin having two or more epoxy groups in one molecule is preferable.
液状エポキシ樹脂としては、ビスフェノールA型エポキシ樹脂、ビスフェノールF型エポキシ樹脂、ビスフェノールAF型エポキシ樹脂、水添ビスフェノールA型エポキシ樹脂、ナフタレン型エポキシ樹脂、グリシジルエステル型エポキシ樹脂、グリシジルアミン型エポキシ樹脂、フェノールノボラック型エポキシ樹脂、エステル骨格を有する脂環式エポキシ樹脂、シクロヘキサン型エポキシ樹脂、シクロヘキサンジメタノール型エポキシ樹脂、及びブタジエン構造を有するエポキシ樹脂が好ましい。 Examples of the liquid epoxy resin include bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol AF type epoxy resin, hydrogenated bisphenol A type epoxy resin, naphthalene type epoxy resin, glycidyl ester type epoxy resin, glycidylamine type epoxy resin, and phenol. A novolak type epoxy resin, an alicyclic epoxy resin having an ester skeleton, a cyclohexane type epoxy resin, a cyclohexanedimethanol type epoxy resin, and an epoxy resin having a butadiene structure are preferable.
液状エポキシ樹脂の具体例としては、DIC社製の「HP4032」、「HP4032D」、「HP4032SS」(ナフタレン型エポキシ樹脂);三菱ケミカル社製の「828US」、「828EL」、「jER828EL」、「825」、(ビスフェノールA型エポキシ樹脂);三菱ケミカル社製の「jER807」、「1750」(ビスフェノールF型エポキシ樹脂);三菱ケミカル社製の「jER152」(フェノールノボラック型エポキシ樹脂);三菱ケミカル社製の「630」、「630LSD」、「604」(グリシジルアミン型エポキシ樹脂);ADEKA社製の「ED-523T」(グリシロール型エポキシ樹脂);ADEKA社製の「EP-3950L」、「EP-3980S」(グリシジルアミン型エポキシ樹脂);ADEKA社製の「EP-4088S」(ジシクロペンタジエン型エポキシ樹脂);日鉄ケミカル&マテリアル社製の「ZX1059」(ビスフェノールA型エポキシ樹脂とビスフェノールF型エポキシ樹脂の混合品);ナガセケムテックス社製の「EX-721」(グリシジルエステル型エポキシ樹脂);ダイセル社製の「セロキサイド2021P」(エステル骨格を有する脂環式エポキシ樹脂);ダイセル社製の「PB-3600」、日本曹達社製の「JP-100」、「JP-200」(ブタジエン構造を有するエポキシ樹脂);日鉄ケミカル&マテリアル社製の「ZX1658」、「ZX1658GS」(1,4-グリシジルシクロヘキサン型エポキシ樹脂)、三菱ケミカル社製の「YX8000」(水添ビスフェノールA型エポキシ樹脂)、信越化学社製「KF-101」(エポキシ変性シリコーン樹脂)等が挙げられる。これらは、1種類単独で用いてもよく、2種類以上を組み合わせて用いてもよい。 Specific examples of the liquid epoxy resin include "HP4032", "HP4032D", and "HP4032SS" (naphthalene type epoxy resin) manufactured by DIC; "828US", "828EL", "jER828EL", and "825" manufactured by Mitsubishi Chemical Co., Ltd. , (Bisphenol A type epoxy resin); "jER807", "1750" (bisphenol F type epoxy resin) manufactured by Mitsubishi Chemical Co., Ltd .; "jER152" (phenol novolak type epoxy resin) manufactured by Mitsubishi Chemical Co., Ltd.; "630", "630LSD", "604" (glycidylamine type epoxy resin); "ED-523T" (glycylol type epoxy resin) manufactured by ADEKA; "EP-3950L", "EP-3980S" manufactured by ADEKA. (Glysidylamine type epoxy resin); "EP-4088S" (dicyclopentadiene type epoxy resin) manufactured by ADEKA; "ZX1059" (bisphenol A type epoxy resin and bisphenol F type epoxy resin) manufactured by Nittetsu Chemical & Materials Co., Ltd. (Mixed product); "EX-721" (glycidyl ester type epoxy resin) manufactured by Nagase Chemtex Co., Ltd .; "Selokiside 2021P" (alicyclic epoxy resin having an ester skeleton) manufactured by Daicel Co., Ltd .; "PB" manufactured by Daisel Co., Ltd. -3600 "," JP-100 "," JP-200 "(epoxy resin having a butadiene structure) manufactured by Nippon Soda Co., Ltd .;" ZX1658 "," ZX1658GS "(1,4-glycidyl) manufactured by Nittetsu Chemical & Materials Co., Ltd. Cyclohexane type epoxy resin), "YX8000" manufactured by Mitsubishi Chemical Co., Ltd. (hydrogenated bisphenol A type epoxy resin), "KF-101" manufactured by Shinetsu Chemical Co., Ltd. (epoxy-modified silicone resin), and the like. These may be used individually by 1 type, or may be used in combination of 2 or more types.
エポキシ樹脂は、固体状エポキシ樹脂、液状エポキシ樹脂、又はそれらの組み合わせの何れであってもよいが、無機充填材成分面積の比(A0-5/A5-10)が特定範囲にある硬化体を実現し易い観点から、固体状エポキシ樹脂を含むことが好ましく、固体状エポキシ樹脂と液状エポキシ樹脂との組み合わせであることが特に好ましい。 The epoxy resin may be a solid epoxy resin, a liquid epoxy resin, or a combination thereof, but the curing is such that the ratio of the component areas of the inorganic filler (A 0-5 / A 5-10 ) is within a specific range. From the viewpoint of easy realization of the body, it is preferable to contain a solid epoxy resin, and a combination of the solid epoxy resin and the liquid epoxy resin is particularly preferable.
エポキシ樹脂として、固体状エポキシ樹脂と液状エポキシ樹脂とを組み合わせて用いる場合、それらの質量比(固体状エポキシ樹脂:液状エポキシ樹脂)は、好ましくは20:1~1:20、より好ましくは10:1~1:10、特に好ましくは3:1~1:3である。 When a solid epoxy resin and a liquid epoxy resin are used in combination as the epoxy resin, their mass ratio (solid epoxy resin: liquid epoxy resin) is preferably 20: 1 to 1:20, more preferably 10:20. It is 1 to 1:10, particularly preferably 3: 1 to 1: 3.
エポキシ樹脂のエポキシ当量は、好ましくは50g/eq.~5,000g/eq.、より好ましくは60g/eq.~1,000g/eq.、さらに好ましくは80g/eq.~500g/eq.、さらにより好ましくは100g/eq.~300g/eq.である。エポキシ当量は、エポキシ基1当量あたりの樹脂の質量である。このエポキシ当量は、JIS K7236に従って測定することができる。 The epoxy equivalent of the epoxy resin is preferably 50 g / eq. ~ 5,000 g / eq. , More preferably 60 g / eq. ~ 1,000 g / eq. , More preferably 80 g / eq. ~ 500 g / eq. , Even more preferably 100 g / eq. ~ 300 g / eq. Is. Epoxy equivalent is the mass of resin per equivalent of epoxy group. This epoxy equivalent can be measured according to JIS K7236.
エポキシ樹脂の重量平均分子量(Mw)は、好ましくは100~5,000、より好ましくは250~3,000、さらに好ましくは400~1,500である。樹脂の重量平均分子量は、ゲルパーミエーションクロマトグラフィー(GPC)法により、ポリスチレン換算の値として測定できる。 The weight average molecular weight (Mw) of the epoxy resin is preferably 100 to 5,000, more preferably 250 to 3,000, and even more preferably 400 to 1,500. The weight average molecular weight of the resin can be measured as a polystyrene-equivalent value by a gel permeation chromatography (GPC) method.
エポキシ樹脂の含有量は、本発明の効果を顕著に得る観点から、樹脂組成物中の不揮発成分を100質量%としたとき、好ましくは1質量%以上、より好ましくは5質量%以上、さらに好ましくは10質量%以上、特に好ましくは15質量%以上であり、好ましくは50質量%以下、より好ましくは40質量%以下、さらに好ましくは35質量%以下、特に好ましくは30質量%以下である。したがって、好適な一実施形態において、樹脂組成物中の不揮発成分を100質量%としたとき、エポキシ樹脂の含有量は10~50質量%である。 The content of the epoxy resin is preferably 1% by mass or more, more preferably 5% by mass or more, still more preferably, when the non-volatile component in the resin composition is 100% by mass, from the viewpoint of remarkably obtaining the effect of the present invention. Is 10% by mass or more, particularly preferably 15% by mass or more, preferably 50% by mass or less, more preferably 40% by mass or less, still more preferably 35% by mass or less, and particularly preferably 30% by mass or less. Therefore, in one preferred embodiment, the content of the epoxy resin is 10 to 50% by mass when the non-volatile component in the resin composition is 100% by mass.
本発明の硬化体を形成するために用いる樹脂組成物は、さらに他の成分を含有してもよい。斯かる他の成分としては、例えば、硬化剤、熱可塑性樹脂、硬化促進剤、その他の添加剤、及び有機溶剤等が挙げられる。以下、各成分について詳細に説明する。 The resin composition used for forming the cured product of the present invention may further contain other components. Examples of such other components include curing agents, thermoplastic resins, curing accelerators, other additives, organic solvents and the like. Hereinafter, each component will be described in detail.
-硬化剤-
樹脂組成物は、硬化剤を含有してよい。硬化剤は、エポキシ樹脂と反応して樹脂組成物を硬化させる機能を有する。硬化剤は1種単独で用いてもよく、2種以上を組み合わせて用いてもよい。
-Hardener-
The resin composition may contain a curing agent. The curing agent has a function of reacting with the epoxy resin to cure the resin composition. The curing agent may be used alone or in combination of two or more.
硬化剤としては、特に限定されるものではないが、例えば、フェノール系硬化剤、カルボジイミド系硬化剤、酸無水物系硬化剤、アミン系硬化剤、ベンゾオキサジン系硬化剤、シアネートエステル系硬化剤、チオール系硬化剤等が挙げられる。無機充填材成分面積の比(A0-5/A5-10)が特定範囲にある硬化体を実現し易い観点から、硬化剤は、フェノール系硬化剤を含むことが好ましい。 The curing agent is not particularly limited, but for example, a phenol-based curing agent, a carbodiimide-based curing agent, an acid anhydride-based curing agent, an amine-based curing agent, a benzoxazine-based curing agent, a cyanate ester-based curing agent, and the like. Examples include thiol-based curing agents. From the viewpoint of facilitating the realization of a cured product in which the ratio of the component areas of the inorganic filler (A 0-5 / A 5-10 ) is in a specific range, the curing agent preferably contains a phenolic curing agent.
フェノール系硬化剤は、1分子中に2個以上のフェノール性水酸基を有する硬化剤であり、例えば、ビスフェノール系硬化剤、ビフェニル型フェノール系硬化剤、ナフタレン型フェノール系硬化剤、フェノールノボラック型フェノール系硬化剤、ナフチレンエーテル型フェノール系硬化剤、トリアジン骨格含有フェノール系硬化剤、ポリフェニレンエーテル型フェノール系硬化剤、フェノールアラルキル型フェノール系硬化剤、クレゾールノボラック型フェノール系硬化剤、ビスフェノール型フェノール系硬化剤等が挙げられる。中でも、無機充填材成分面積の比(A0-5/A5-10)が特定範囲にある硬化体を実現し易い観点から、好ましくは、ビスフェノール系硬化剤であり、より好ましくは、フッ素原子を有するビスフェノール化合物、脂環構造を有するビスフェノール化合物、フルオレン骨格を有するビスフェノール化合物から選ばれるビスフェノール系硬化剤、さらに好ましくは、フッ素原子を有するビスフェノール化合物、特に好ましくは、ビスフェノールAFである。 The phenol-based curing agent is a curing agent having two or more phenolic hydroxyl groups in one molecule, and is, for example, a bisphenol-based curing agent, a biphenyl-type phenol-based curing agent, a naphthalene-type phenol-based curing agent, and a phenol novolac-type phenol-based. Hardener, naphthylene ether type phenolic hardener, triazine skeleton-containing phenolic hardener, polyphenylene ether type phenolic hardener, phenol aralkyl type phenolic hardener, cresol novolak type phenolic hardener, bisphenol type phenolic hardener And so on. Among them, a bisphenol-based curing agent is preferable, and a fluorine atom is more preferable, from the viewpoint of facilitating the realization of a cured product in which the ratio of the component areas of the inorganic filler (A 0-5 / A 5-10 ) is in a specific range. A bisphenol compound having an alicyclic structure, a bisphenol compound having a fluorene skeleton, a bisphenol-based curing agent selected from the above, more preferably a bisphenol compound having a fluorine atom, and particularly preferably a bisphenol AF.
フェノール系硬化剤の市販品としては、具体的に、セントラル硝子社製の「BIS-AF」、「BIS-Z」、本州化学工業社製「BisE」、「BisP-TMC」;三井化学ファイン社製「BisA」、「BisF」、「BisP-M」;本州化学工業社製「BisP-AP」、「BisP-MIBK」、「BisP-B」、「Bis-Z」、「BisP-CP」、「o,o’-BPF」、「BisP-IOTD」、「BisP-IBTD」、「BisP-DED」、「BisP-BA」;本州化学工業社製「Bis-C」、「Bis26X-A」、「BisOPP-A」、「BisOTBP-A」、「BisOCHP―A」、「BisOFP-A」、「BisOC-Z」、「BisOC-FL」、「BisOFP-A」、「BisOC-CP」、「BisOCHP-Z」、「メチレンビスP-CR」、「TM-BPF」、「BisOC-F」、「Bis3M6B-IBTD」、「BisOC-IST」、「BisP-IST」、「BisP-PRM」、「BisP-LV」等が挙げられる。 Specific examples of commercially available phenolic curing agents include "BIS-AF" and "BIS-Z" manufactured by Central Glass Co., Ltd., "BisE" and "BisP-TMC" manufactured by Honshu Chemical Industry Co., Ltd .; Mitsui Chemical Fine Co., Ltd. "BisA", "BisF", "BisP-M" manufactured by Honshu Chemical Industry Co., Ltd. "BisP-AP", "BisP-MIBK", "BisP-B", "Bis-Z", "BisP-CP", "O, o'-BPF", "BisP-IOTD", "BisP-IBTD", "BisP-DED", "BisP-BA"; "Bis-C", "Bis26X-A" manufactured by Honshu Chemical Industry Co., Ltd., "BisOPP-A", "BisOTBP-A", "BisOCHP-A", "BisOFP-A", "BisOC-Z", "BisOC-FL", "BisOFP-A", "BisOC-CP", "BisOCHP" -Z "," Methylenebis P-CR "," TM-BPF "," BisOC-F "," Bis3M6B-IBTD "," BisOC-IST "," BisP-IST "," BisP-PRM "," BisP- LV ”and the like.
カルボジイミド系硬化剤は、1分子中に2個以上のカルボジイミド構造を有する硬化剤であり、例えば、テトラメチレン-ビス(t-ブチルカルボジイミド)、シクロヘキサンビス(メチレン-t-ブチルカルボジイミド)等の脂肪族ビスカルボジイミド;フェニレン-ビス(キシリルカルボジイミド)等の芳香族ビスカルボジイミド等のビスカルボジイミド;ポリヘキサメチレンカルボジイミド、ポリトリメチルヘキサメチレンカルボジイミド、ポリシクロヘキシレンカルボジイミド、ポリ(メチレンビスシクロヘキシレンカルボジイミド)、ポリ(イソホロンカルボジイミド)等の脂肪族ポリカルボジイミド;ポリ(フェニレンカルボジイミド)、ポリ(ナフチレンカルボジイミド)、ポリ(トリレンカルボジイミド)、ポリ(メチルジイソプロピルフェニレンカルボジイミド)、ポリ(トリエチルフェニレンカルボジイミド)、ポリ(ジエチルフェニレンカルボジイミド)、ポリ(トリイソプロピルフェニレンカルボジイミド)、ポリ(ジイソプロピルフェニレンカルボジイミド)、ポリ(キシリレンカルボジイミド)、ポリ(テトラメチルキシリレンカルボジイミド)、ポリ(メチレンジフェニレンカルボジイミド)、ポリ[メチレンビス(メチルフェニレン)カルボジイミド]等の芳香族ポリカルボジイミド等のポリカルボジイミドが挙げられる。 The carbodiimide-based curing agent is a curing agent having two or more carbodiimide structures in one molecule, and is an aliphatic such as tetramethylene-bis (t-butylcarbodiimide) and cyclohexanebis (methylene-t-butylcarbodiimide). Biscarbodiimide; Fragrant biscarbodiimide such as phenylene-bis (kisilylcarbodiimide); Polyhexamethylenecarbodiimide, Polytrimethylhexamethylenecarbodiimide, Polycyclohexylenecarbodiimide, Poly (methylenebiscyclohexylenecarbodiimide), Poly (isophorone) Carbodiimide) and other aliphatic polycarbodiimides; poly (phenylene carbodiimide), poly (naphthylene carbodiimide), poly (trilen carbodiimide), poly (methyldiisopropylphenylene carbodiimide), poly (triethylphenylene carbodiimide), poly (diethylphenylene carbodiimide) , Poly (triisopropylphenylene carbodiimide), poly (diisopropylphenylene carbodiimide), poly (xylylene carbodiimide), poly (tetramethylxylylene carbodiimide), poly (methylenediphenylene carbodiimide), poly [methylenebis (methylphenylene) carbodiimide], etc. Examples thereof include polycarbodiimides such as aromatic polycarbodiimides.
カルボジイミド系硬化剤の市販品としては、例えば、日清紡ケミカル社製の「カルボジライトV-02B」、「カルボジライトV-03」、「カルボジライトV-04K」、「カルボジライトV-07」及び「カルボジライトV-09」;ラインケミー社製の「スタバクゾールP」、「スタバクゾールP400」、「ハイカジル510」等が挙げられる。 Commercially available products of carbodiimide-based curing agents include, for example, "carbodilite V-02B", "carbodilite V-03", "carbodilite V-04K", "carbodilite V-07" and "carbodilite V-09" manufactured by Nisshinbo Chemical Co., Ltd. "; Examples thereof include" Stavaxol P "," Stavaxol P400 ", and" High Kazil 510 "manufactured by Rheinchemy.
酸無水物系硬化剤は、1分子中に1個以上のカルボン酸無水物基(-CO-O-CO-)を有する硬化剤であり、例えば、無水フタル酸、ピロメリット酸二無水物、1,4,5,8-ナフタレンテトラカルボン酸二無水物、2,3,6,7-ナフタレンテトラカルボン酸二無水物、3,3’,4,4’-ベンソフェノンテトラカルボン酸二無水物、オキシジフタル酸二無水物、3,3’,4,4’-ジフェニルスルホンテトラカルボン酸二無水物、3,3’,4,4’-ジフェニルエーテルテトラカルボン酸二無水物、3,3’,4,4’-ビフェニルテトラカルボン酸二無水物、メチレン-4,4’-ジフタル酸二無水物等の芳香族酸無水物系硬化剤;テトラヒドロ無水フタル酸、ヘキサヒドロ無水フタル酸、メチルテトラヒドロ無水フタル酸、メチルヘキサヒドロ無水フタル酸、メチルナジック酸無水物、水素化メチルナジック酸無水物、トリアルキルテトラヒドロ無水フタル酸、ドデセニル無水コハク酸、シクロペンタンテトラカルボン酸二無水物、シクロヘキサン-1,2,4,5-テトラカルボン酸二無水物等の脂肪族酸無水物系硬化剤;スチレン/無水マレイン酸共重合体、(メタ)アクリル酸アルキル/スチレン/無水マレイン酸共重合体等の重合体無水物系硬化剤などが挙げられる。酸無水物系硬化剤の市販品としては、新日本理化社製の「HNA-100」、「MH-700」、「MTA-15」、「DDSA」、「OSA」、三菱ケミカル社製の「YH-306」、「YH-307」、日立化成社製の「HN-2200」、「HN-5500」等が挙げられる。 The acid anhydride-based curing agent is a curing agent having one or more carboxylic acid anhydride groups (-CO-O-CO-) in one molecule, and is, for example, phthalic anhydride, pyromellitic dianhydride, and the like. 1,4,5,8-naphthalenetetracarboxylic acid dianhydride, 2,3,6,7-naphthalenetetracarboxylic acid dianhydride, 3,3', 4,4'-benzophenonetetracarboxylic acid dianhydride , Oxydiphthalic acid dianhydride, 3,3', 4,4'-diphenylsulfone tetracarboxylic acid dianhydride, 3,3', 4,4'-diphenyl ether tetracarboxylic acid dianhydride, 3,3', Aromatic acid anhydride-based curing agents such as 4,4'-biphenyltetracarboxylic acid dianhydride, methylene-4,4'-diphthalic acid dianhydride; tetrahydroanhydride, hexahydroanhydride, methyltetrahydrohydride. Acid, Methylhexahydroanhydride, Methylnagic acid anhydride, Hydrogenated methylnagic acid anhydride, Trialkyltetrahydroanhydride, Dodecenylhydride succinic acid, Cyclopentanetetracarboxylic acid dianhydride, Cyclohexane-1,2, Alipid acid anhydride-based curing agent such as 4,5-tetracarboxylic dianhydride; polymer anhydride such as styrene / maleic anhydride copolymer, alkyl (meth) acrylate / styrene / maleic anhydride copolymer Examples include physical hardeners. Commercially available acid anhydride curing agents include "HNA-100", "MH-700", "MTA-15", "DDSA", "OSA" manufactured by Shin Nihon Rika Co., Ltd., and "OSA" manufactured by Mitsubishi Chemical Corporation. Examples thereof include "YH-306" and "YH-307", "HN-2200" and "HN-5500" manufactured by Hitachi Chemical Co., Ltd.
アミン系硬化剤は、2個以上のアミノ基を有する硬化剤であり、例えば、脂肪族アミン類、ポリエーテルアミン類、脂環式アミン類、芳香族アミン類等が挙げられ、中でも、本発明の所望の効果を奏する観点から、芳香族アミン類が好ましい。アミン系硬化剤は、第1級アミン又は第2級アミンが好ましく、第1級アミンがより好ましい。アミン系硬化剤の具体例としては、4,4’-メチレンビス(2,6-ジメチルアニリン)、4,4’-ジアミノジフェニルメタン、4,4’-ジアミノジフェニルスルホン、3,3’-ジアミノジフェニルスルホン、m-フェニレンジアミン、m-キシリレンジアミン、ジエチルトルエンジアミン、4,4’-ジアミノジフェニルエーテル、3,3’-ジメチル-4,4’-ジアミノビフェニル、2,2’-ジメチル-4,4’-ジアミノビフェニル、3,3’-ジヒドロキシベンジジン、2,2-ビス(3-アミノ-4-ヒドロキシフェニル)プロパン、3,3-ジメチル-5,5-ジエチル-4,4-ジフェニルメタンジアミン、2,2-ビス(4-アミノフェニル)プロパン、2,2-ビス(4-(4-アミノフェノキシ)フェニル)プロパン、1,3-ビス(3-アミノフェノキシ)ベンゼン、1,3-ビス(4-アミノフェノキシ)ベンゼン、1,4-ビス(4-アミノフェノキシ)ベンゼン、4,4’-ビス(4-アミノフェノキシ)ビフェニル、ビス(4-(4-アミノフェノキシ)フェニル)スルホン、ビス(4-(3-アミノフェノキシ)フェニル)スルホン、等が挙げられる。アミン系硬化剤は市販品を用いてもよく、例えば、セイカ社製「SEIKACURE-S」、日本化薬社製の「KAYABOND C-200S」、「KAYABOND C-100」、「カヤハードA-A」、「カヤハードA-B」、「カヤハードA-S」、三菱ケミカル社製の「エピキュアW」等が挙げられる。 The amine-based curing agent is a curing agent having two or more amino groups, and examples thereof include aliphatic amines, polyether amines, alicyclic amines, aromatic amines, and the like. Among them, the present invention. Aromatic amines are preferable from the viewpoint of exhibiting the desired effect of. The amine-based curing agent is preferably a primary amine or a secondary amine, more preferably a primary amine. Specific examples of the amine-based curing agent include 4,4'-methylenebis (2,6-dimethylaniline), 4,4'-diaminodiphenylmethane, 4,4'-diaminodiphenylsulfone, and 3,3'-diaminodiphenylsulfone. , M-phenylenediamine, m-xylylene diamine, diethyltoluenediamine, 4,4'-diaminodiphenyl ether, 3,3'-dimethyl-4,4'-diaminobiphenyl, 2,2'-dimethyl-4,4' -Diaminobiphenyl, 3,3'-dihydroxybenzidine, 2,2-bis (3-amino-4-hydroxyphenyl) propane, 3,3-dimethyl-5,5-diethyl-4,4-diphenylmethanediamine, 2, 2-Bis (4-aminophenyl) propane, 2,2-bis (4- (4-aminophenoxy) phenyl) propane, 1,3-bis (3-aminophenoxy) benzene, 1,3-bis (4-) Aminophenoxy) benzene, 1,4-bis (4-aminophenoxy) benzene, 4,4'-bis (4-aminophenoxy) biphenyl, bis (4- (4-aminophenoxy) phenyl) sulfone, bis (4-) (3-Aminophenoxy) phenyl) sulfone, etc. may be mentioned. Commercially available products may be used as the amine-based curing agent, for example, "SEIKACURE-S" manufactured by Seika, "KAYABOND C-200S", "KAYABOND C-100", and "Kayahard A-A" manufactured by Nippon Kayaku. , "Kayahard AB", "Kayahard AS", "Epicure W" manufactured by Mitsubishi Chemical Corporation, and the like.
ベンゾオキサジン系硬化剤の具体例としては、JFEケミカル社製の「JBZ-OP100D」、「ODA-BOZ」;昭和高分子社製の「HFB2006M」;四国化成工業社製の「P-d」、「F-a」などが挙げられる。 Specific examples of the benzoxazine-based curing agent include "JBZ-OP100D" and "ODA-BOZ" manufactured by JFE Chemical Co., Ltd .; "HFB2006M" manufactured by Showa High Polymer Co., Ltd .; "Pd" manufactured by Shikoku Chemicals Corporation. Examples include "FA".
シアネートエステル系硬化剤としては、例えば、ビスフェノールAジシアネート、ポリフェノールシアネート(オリゴ(3-メチレン-1,5-フェニレンシアネート))、4,4’-メチレンビス(2,6-ジメチルフェニルシアネート)、4,4’-エチリデンジフェニルジシアネート、ヘキサフルオロビスフェノールAジシアネート、2,2-ビス(4-シアネート)フェニルプロパン、1,1-ビス(4-シアネートフェニルメタン)、ビス(4-シアネート-3,5-ジメチルフェニル)メタン、1,3-ビス(4-シアネートフェニル-1-(メチルエチリデン))ベンゼン、ビス(4-シアネートフェニル)チオエーテル、及びビス(4-シアネートフェニル)エーテル等の2官能シアネート樹脂、フェノールノボラック及びクレゾールノボラック等から誘導される多官能シアネート樹脂、これらシアネート樹脂が一部トリアジン化したプレポリマーなどが挙げられる。シアネートエステル系硬化剤の具体例としては、ロンザジャパン社製の「PT30」及び「PT60」(いずれもフェノールノボラック型多官能シアネートエステル樹脂)、「BA230」、「BA230S75」(ビスフェノールAジシアネートの一部又は全部がトリアジン化され三量体となったプレポリマー)等が挙げられる。 Examples of the cyanate ester-based curing agent include bisphenol A dicyanate, polyphenol cyanate (oligo (3-methylene-1,5-phenylencianate)), 4,4'-methylenebis (2,6-dimethylphenylcyanate), and 4, 4'-Etilidene diphenyl disyanate, hexafluorobisphenol A disyanate, 2,2-bis (4-cyanate) phenylpropane, 1,1-bis (4-cyanate phenylmethane), bis (4-cyanate-3,5-) Bifunctional cyanate resins such as dimethylphenyl) methane, 1,3-bis (4-cyanatephenyl-1- (methylethylidene)) benzene, bis (4-cyanatephenyl) thioether, and bis (4-cyanatephenyl) ether, Examples thereof include polyfunctional cyanate resins derived from phenol novolak and cresol novolak, and prepolymers in which these cyanate resins are partially triazined. Specific examples of the cyanate ester-based curing agent include "PT30" and "PT60" (both are phenol novolac type polyfunctional cyanate ester resins), "BA230", and "BA230S75" (part of bisphenol A dicyanate) manufactured by Lonza Japan. Alternatively, a prepolymer in which the whole is triazined to become a trimer) and the like can be mentioned.
チオール系硬化剤は、2個以上のメルカプト基を有する硬化剤であり、例えば、トリメチロールプロパントリス(3-メルカプトプロピオネート)、ペンタエリスリトールテトラキス(3-メルカプトブチレート)、トリス(3-メルカプトプロピル)イソシアヌレート等が挙げられる。 Thiol-based curing agents are curing agents having two or more mercapto groups, and are, for example, trimethylolpropanetris (3-mercaptopropionate), pentaerythritol tetrakis (3-mercaptobutyrate), and tris (3-mercapto). Propyl) isocyanurate and the like.
硬化剤の反応基当量は、好ましくは50g/eq.~3000g/eq.、より好ましくは100g/eq.~1000g/eq.、さらに好ましくは100g/eq.~500g/eq.、特に好ましくは100g/eq.~300g/eq.である。反応基当量は、反応基1当量あたりの硬化剤の質量である。反応基は、例えば、フェノール系硬化剤であればフェノール性水酸基である。酸無水物系硬化剤の場合はカルボン酸無水物基(-CO-O-CO-)1当量で反応基2当量に相当する。 The reaction group equivalent of the curing agent is preferably 50 g / eq. ~ 3000 g / eq. , More preferably 100 g / eq. ~ 1000 g / eq. , More preferably 100 g / eq. ~ 500 g / eq. , Particularly preferably 100 g / eq. ~ 300 g / eq. Is. The reaction group equivalent is the mass of the curing agent per reaction group equivalent. The reactive group is, for example, a phenolic hydroxyl group in the case of a phenolic curing agent. In the case of an acid anhydride-based curing agent, 1 equivalent of a carboxylic acid anhydride group (-CO-O-CO-) corresponds to 2 equivalents of a reactive group.
硬化剤の含有量は、本発明の効果を顕著に得る観点から、樹脂組成物中の不揮発成分を100質量%としたとき、好ましくは30質量%以下、より好ましくは20質量%以下、さらに好ましくは15質量%以下、特に好ましくは10質量%以下であり、例えば0質量%以上、0.001質量%以上、好ましくは0.01質量%以上、より好ましくは0.1質量%以上、さらに好ましくは1質量%以上、特に好ましくは3質量%以上である。 The content of the curing agent is preferably 30% by mass or less, more preferably 20% by mass or less, still more preferably, when the non-volatile component in the resin composition is 100% by mass, from the viewpoint of remarkably obtaining the effect of the present invention. Is 15% by mass or less, particularly preferably 10% by mass or less, for example, 0% by mass or more, 0.001% by mass or more, preferably 0.01% by mass or more, more preferably 0.1% by mass or more, still more preferable. Is 1% by mass or more, particularly preferably 3% by mass or more.
-熱可塑性樹脂-
樹脂組成物は、熱可塑性樹脂を含有してもよい。熱可塑性樹脂は、1種単独で用いてもよく、又は2種以上を組み合わせて用いてもよい。
-Thermoplastic resin-
The resin composition may contain a thermoplastic resin. The thermoplastic resin may be used alone or in combination of two or more.
熱可塑性樹脂としては、例えば、フェノキシ樹脂、ポリビニルアセタール樹脂、アクリル樹脂、ポリオレフィン樹脂、ポリブタジエン樹脂、ポリイミド樹脂、ポリアミドイミド樹脂、ポリスルホン樹脂、ポリエーテルスルホン樹脂、ポリフェニレンエーテル樹脂、ポリエーテルイミド樹脂、ポリカーボネート樹脂、ポリエーテルエーテルケトン樹脂、ポリエステル樹脂が挙げられ、中でも、フェノキシ樹脂、アクリル樹脂及びポリフェニレンエーテル樹脂から選ばれる樹脂が好ましい。 Examples of the thermoplastic resin include phenoxy resin, polyvinyl acetal resin, acrylic resin, polyolefin resin, polybutadiene resin, polyimide resin, polyamideimide resin, polysulfone resin, polyethersulfone resin, polyphenylene ether resin, polyetherimide resin, and polycarbonate resin. , Polyether ether ketone resin, polyester resin, and among them, a resin selected from a phenoxy resin, an acrylic resin and a polyphenylene ether resin is preferable.
フェノキシ樹脂としては、例えば、ビスフェノールA骨格、ビスフェノールF骨格、ビスフェノールS骨格、ビスフェノールアセトフェノン骨格、ノボラック骨格、ビフェニル骨格、フルオレン骨格、ジシクロペンタジエン骨格、ノルボルネン骨格、ナフタレン骨格、アントラセン骨格、アダマンタン骨格、テルペン骨格、及びトリメチルシクロヘキサン骨格からなる群から選択される1種以上の骨格を有するフェノキシ樹脂が挙げられる。フェノキシ樹脂の末端は、フェノール性水酸基、エポキシ基等のいずれの官能基でもよい。フェノキシ樹脂は1種単独で用いてもよく、2種以上を組み合わせて用いてもよい。フェノキシ樹脂の具体例としては、三菱ケミカル社製の「1256」及び「4250」(いずれもビスフェノールA骨格含有フェノキシ樹脂)、「YX8100」(ビスフェノールS骨格含有フェノキシ樹脂)、及び「YX6954」(ビスフェノールアセトフェノン骨格含有フェノキシ樹脂)、日鉄ケミカル&マテリアル社製の「FX280」及び「FX293」、三菱ケミカル社製の「YX7200B35」、「YL7500BH30」、「YX6954BH30」、「YX7553」、「YX7553BH30」、「YL7769BH30」、「YL6794」、「YL7213」、「YL7290」及び「YL7482」等が挙げられる。 Examples of the phenoxy resin include bisphenol A skeleton, bisphenol F skeleton, bisphenol S skeleton, bisphenol acetophenone skeleton, novolak skeleton, biphenyl skeleton, fluorene skeleton, dicyclopentadiene skeleton, norbornene skeleton, naphthalene skeleton, anthracene skeleton, adamantan skeleton, and terpene. Examples thereof include phenoxy resins having one or more skeletons selected from the group consisting of skeletons and trimethylcyclohexane skeletons. The terminal of the phenoxy resin may be any functional group such as a phenolic hydroxyl group or an epoxy group. The phenoxy resin may be used alone or in combination of two or more. Specific examples of the phenoxy resin include "1256" and "4250" (both bisphenol A skeleton-containing phenoxy resin), "YX8100" (bisphenol S skeleton-containing phenoxy resin), and "YX6954" (bisphenol acetophenone) manufactured by Mitsubishi Chemical Corporation. (Skeletal-containing phenoxy resin), "FX280" and "FX293" manufactured by Nittetsu Chemical & Materials, "YX7200B35", "YL7500BH30", "YX6954BH30", "YX7553", "YX7553BH30", "YL7769BH30" manufactured by Mitsubishi Chemical Co., Ltd. , "YL6794", "YL7213", "YL7290", "YL7482" and the like.
ポリビニルアセタール樹脂としては、例えば、ポリビニルホルマール樹脂、ポリビニルブチラール樹脂が挙げられ、ポリビニルブチラール樹脂が好ましい。ポリビニルアセタール樹脂の具体例としては、例えば、電気化学工業社製の「電化ブチラール4000-2」、「電化ブチラール5000-A」、「電化ブチラール6000-C」、「電化ブチラール6000-EP」、積水化学工業社製のエスレックBHシリーズ、BXシリーズ(例えばBX-5Z)、KSシリーズ(例えばKS-1)、BLシリーズ、BMシリーズ等が挙げられる。 Examples of the polyvinyl acetal resin include polyvinyl formal resin and polyvinyl butyral resin, and polyvinyl butyral resin is preferable. Specific examples of the polyvinyl acetal resin include, for example, "Electrified Butyral 4000-2", "Electrified Butyral 5000-A", "Electrified Butyral 6000-C", "Electrified Butyral 6000-EP", Sekisui Chemical Co., Ltd. Examples thereof include Eslek BH series, BX series (for example, BX-5Z), KS series (for example, KS-1), BL series, and BM series manufactured by Chemical Industry Co., Ltd.
アクリル樹脂とは、(メタ)アクリル酸エステル系モノマーを含むモノマー成分を重合してなる重合体を意味する。アクリル樹脂を構成するモノマー成分には、(メタ)アクリル酸エステル系モノマーに加えて、(メタ)アクリルアミド系モノマー、スチレン系モノマー、官能基含有モノマー等が共重合成分として含まれていてもよい。アクリル樹脂の具体例としては、東亜合成社製の「ARUFON UP-1000」、「ARUFON UP-1010」、「ARUFON UP-1020」、「ARUFON UP-1021」、「ARUFON UP-1061」、「ARUFON UP-1080」、「ARUFON UP-1110」、「ARUFON UP-1170」、「ARUFON UP-1190」、「ARUFON UP-1500」、「ARUFON UH-2000」、「ARUFON UH-2041」、「ARUFON UH-2190」、「ARUFON UHE-2012」、「ARUFON UC-3510」、「ARUFON UG-4010」、「ARUFON US-6100」、「ARUFON US-6170」などが挙げられる。これらは、1種類単独で用いてもよく、2種類以上を組み合わせて用いてもよい。 The acrylic resin means a polymer obtained by polymerizing a monomer component containing a (meth) acrylic acid ester-based monomer. In addition to the (meth) acrylic acid ester-based monomer, the monomer component constituting the acrylic resin may contain a (meth) acrylamide-based monomer, a styrene-based monomer, a functional group-containing monomer and the like as a copolymerization component. Specific examples of the acrylic resin include "ARUFON UP-1000", "ARUFON UP-1010", "ARUFON UP-1020", "ARUFON UP-1021", "ARUFON UP-1061", and "ARUFON" manufactured by Toagosei Corporation. UP-1080, "ARUFON UP-1110", "ARUFON UP-1170", "ARUFON UP-1190", "ARUFON UP-1500", "ARUFON UH-2000", "ARUFON UH-2041", "ARUFON UH" -2190, "ARUFON UHE-2012", "ARUFON UC-3510", "ARUFON UG-4010", "ARUFON US-6100", "ARUFON US-6170" and the like. These may be used individually by 1 type, or may be used in combination of 2 or more types.
ポリオレフィン樹脂としては、例えば、低密度ポリエチレン、超低密度ポリエチレン、高密度ポリエチレン、エチレン-酢酸ビニル共重合体、エチレン-アクリル酸エチル共重合体、エチレン-アクリル酸メチル共重合体等のエチレン系共重合樹脂;ポリプロピレン、エチレン-プロピレンブロック共重合体等のポリオレフィン系エラストマー等が挙げられる。 Examples of the polyolefin resin include ethylene-based copolymers such as low-density polyethylene, ultra-low-density polyethylene, high-density polyethylene, ethylene-vinyl acetate copolymer, ethylene-ethyl acrylate copolymer, and ethylene-methyl acrylate copolymer. Polymerized resin; examples thereof include polyolefin-based elastomers such as polypropylene and ethylene-propylene block copolymers.
ポリブタジエン樹脂としては、例えば、水素化ポリブタジエン骨格含有樹脂、ヒドロキシ基含有ポリブタジエン樹脂、フェノール性水酸基含有ポリブタジエン樹脂、カルボキシ基含有ポリブタジエン樹脂、酸無水物基含有ポリブタジエン樹脂、エポキシ基含有ポリブタジエン樹脂、イソシアネート基含有ポリブタジエン樹脂、ウレタン基含有ポリブタジエン樹脂、ポリフェニレンエーテル-ポリブタジエン樹脂等が挙げられる。 Examples of the polybutadiene resin include hydride polybutadiene skeleton-containing resin, hydroxy group-containing polybutadiene resin, phenolic hydroxyl group-containing polybutadiene resin, carboxy group-containing polybutadiene resin, acid anhydride group-containing polybutadiene resin, epoxy group-containing polybutadiene resin, and isocyanate group-containing. Examples thereof include polybutadiene resin, urethane group-containing polybutadiene resin, and polyphenylene ether-polybutadiene resin.
ポリイミド樹脂の具体例としては、新日本理化社製の「リカコートSN20」及び「リカコートPN20」が挙げられる。ポリイミド樹脂の具体例としてはまた、2官能性ヒドロキシル基末端ポリブタジエン、ジイソシアネート化合物及び四塩基酸無水物を反応させて得られる線状ポリイミド(特開2006-37083号公報記載のポリイミド)、ポリシロキサン骨格含有ポリイミド(特開2002-12667号公報及び特開2000-319386号公報等に記載のポリイミド)等の変性ポリイミドが挙げられる。 Specific examples of the polyimide resin include "Ricacoat SN20" and "Ricacoat PN20" manufactured by NEW JAPAN CHEMICAL CO., LTD. Specific examples of the polyimide resin include a linear polyimide obtained by reacting a bifunctional hydroxyl group-terminated polybutadiene, a diisocyanate compound and a tetrabasic acid anhydride (polyimide described in JP-A-2006-37083), and a polysiloxane skeleton. Examples thereof include modified polyimides such as contained polyimides (polyimides described in JP-A-2002-12667 and JP-A-2000-31386).
ポリアミドイミド樹脂の具体例としては、東洋紡績社製の「バイロマックスHR11NN」及び「バイロマックスHR16NN」が挙げられる。ポリアミドイミド樹脂の具体例としてはまた、日立化成工業社製の「KS9100」、「KS9300」(ポリシロキサン骨格含有ポリアミドイミド)等の変性ポリアミドイミドが挙げられる。 Specific examples of the polyamide-imide resin include "Vilomax HR11NN" and "Vilomax HR16NN" manufactured by Toyobo Co., Ltd. Specific examples of the polyamide-imide resin include modified polyamide-imides such as "KS9100" and "KS9300" (polysiloxane skeleton-containing polyamide-imide) manufactured by Hitachi Chemical Industries, Ltd.
ポリエーテルスルホン樹脂の具体例としては、住友化学社製の「PES5003P」等が挙げられる。 Specific examples of the polyether sulfone resin include "PES5003P" manufactured by Sumitomo Chemical Co., Ltd.
ポリスルホン樹脂の具体例としては、ソルベイアドバンストポリマーズ社製のポリスルホン「P1700」、「P3500」等が挙げられる。 Specific examples of the polysulfone resin include polysulfones "P1700" and "P3500" manufactured by Solvay Advanced Polymers.
ポリフェニレンエーテル樹脂の具体例としては、三菱ガス化学社製のオリゴフェニレンエーテル・スチレン樹脂「OPE-2St1200」、「OPE-2St2200」、SABIC製「Noryl(登録商標)SA90」等が挙げられる。ポリエーテルイミド樹脂の具体例としては、GE社製の「ウルテム」等が挙げられる。 Specific examples of the polyphenylene ether resin include oligophenylene ether / styrene resin "OPE-2St1200" and "OPE-2St2200" manufactured by Mitsubishi Gas Chemical Company, Inc., and "Noryl (registered trademark) SA90" manufactured by SABIC. Specific examples of the polyetherimide resin include "Ultem" manufactured by GE.
ポリカーボネート樹脂としては、ヒドロキシ基含有カーボネート樹脂、フェノール性水酸基含有カーボネート樹脂、カルボキシ基含有カーボネート樹脂、酸無水物基含有カーボネート樹脂、イソシアネート基含有カーボネート樹脂、ウレタン基含有カーボネート樹脂等が挙げられる。ポリカーボネート樹脂の具体例としては、三菱瓦斯化学社製の「FPC0220」、旭化成ケミカルズ社製の「T6002」、「T6001」(ポリカーボネートジオール)、クラレ社製の「C-1090」、「C-2090」、「C-3090」(ポリカーボネートジオール)等が挙げられる。ポリエーテルエーテルケトン樹脂の具体例としては、住友化学社製の「スミプロイK」等が挙げられる。ポリエステル樹脂としては、例えばポリエチレンテレフタレート樹脂等が挙げられる。 Examples of the polycarbonate resin include a hydroxy group-containing carbonate resin, a phenolic hydroxyl group-containing carbonate resin, a carboxy group-containing carbonate resin, an acid anhydride group-containing carbonate resin, an isocyanate group-containing carbonate resin, and a urethane group-containing carbonate resin. Specific examples of the polycarbonate resin include "FPC0220" manufactured by Mitsubishi Gas Chemical Company, "T6002" and "T6001" (polycarbonate diol) manufactured by Asahi Kasei Chemicals, and "C-1090" and "C-2090" manufactured by Kuraray. , "C-3090" (polycarbonate diol) and the like. Specific examples of the polyetheretherketone resin include "Sumiproi K" manufactured by Sumitomo Chemical Co., Ltd. Examples of the polyester resin include polyethylene terephthalate resin and the like.
熱可塑性樹脂の重量平均分子量は、好ましくは8,000以上、より好ましくは10,000以上、さらに好ましくは20,000以上であり、好ましくは100,000以下、より好ましくは70,000以下、さらに好ましくは60,000以下である。樹脂の重量平均分子量は、ゲルパーミエーションクロマトグラフィー(GPC)法により、ポリスチレン換算の値として測定できる。 The weight average molecular weight of the thermoplastic resin is preferably 8,000 or more, more preferably 10,000 or more, still more preferably 20,000 or more, preferably 100,000 or less, more preferably 70,000 or less, and further. It is preferably 60,000 or less. The weight average molecular weight of the resin can be measured as a polystyrene-equivalent value by a gel permeation chromatography (GPC) method.
熱可塑性樹脂は、厚さ20μmに製膜した場合の膜面に対して垂直方向から入射した波長450nmの光の透過率が80%以上となる熱可塑性樹脂であることが好ましい。 The thermoplastic resin is preferably a thermoplastic resin having a transmittance of 80% or more of light having a wavelength of 450 nm incident on the film surface in a direction perpendicular to the film surface when the film is formed to a thickness of 20 μm.
熱可塑性樹脂の含有量は、樹脂組成物中の不揮発成分を100質量%としたとき、好ましくは50質量%以下、より好ましくは40質量%以下、さらに好ましくは30質量%以下、特に好ましくは25質量%以下であり、例えば、0質量%以上、0.1質量%以上であり、好ましくは1質量%以上、より好ましくは5質量%以上、特に好ましくは10質量%以上である。 The content of the thermoplastic resin is preferably 50% by mass or less, more preferably 40% by mass or less, still more preferably 30% by mass or less, and particularly preferably 25, when the non-volatile component in the resin composition is 100% by mass. It is 0% by mass or more, for example, 0% by mass or more, 0.1% by mass or more, preferably 1% by mass or more, more preferably 5% by mass or more, and particularly preferably 10% by mass or more.
-硬化促進剤-
樹脂組成物は、硬化促進剤を含有してもよい。硬化促進剤は、熱硬化性樹脂の硬化反応を促進させる機能を有する。硬化促進剤は、1種単独で用いてもよく、2種以上を組み合わせて用いてもよい。
-Curing accelerator-
The resin composition may contain a curing accelerator. The curing accelerator has a function of accelerating the curing reaction of the thermosetting resin. The curing accelerator may be used alone or in combination of two or more.
硬化促進剤としては、例えば、リン系硬化促進剤、イミダゾール系硬化促進剤、アミン系硬化促進剤、グアニジン系硬化促進剤、金属系硬化促進剤等が挙げられる。中でも、硬化促進剤としては、より高い光反射率を達成する観点から、リン系硬化促進剤、イミダゾール系硬化促進剤が好ましく、リン系硬化促進剤がより好ましい。 Examples of the curing accelerator include phosphorus-based curing accelerators, imidazole-based curing accelerators, amine-based curing accelerators, guanidine-based curing accelerators, metal-based curing accelerators, and the like. Among them, as the curing accelerator, a phosphorus-based curing accelerator and an imidazole-based curing accelerator are preferable, and a phosphorus-based curing accelerator is more preferable, from the viewpoint of achieving a higher light reflectance.
リン系硬化促進剤としては、より高い光反射率を達成する観点から、ホスホニウム塩及びホスフィンからなる群より選ばれる1以上を含むことが好ましい。 The phosphorus-based curing accelerator preferably contains one or more selected from the group consisting of phosphonium salts and phosphines from the viewpoint of achieving higher light reflectance.
ホスホニウム塩としては、例えば、テトラブチルホスホニウムブロマイド、テトラブチルホスホニウムクロライド、テトラブチルホスホニウムアセテート、テトラブチルホスホニウムデカノエート、テトラブチルホスホニウムラウレート、ビス(テトラブチルホスホニウム)ピロメリテート、テトラブチルホスホニウムハイドロジェンヘキサヒドロフタレート、テトラブチルホスホニウム2,6-ビス[(2-ヒドロキシ-5-メチルフェニル)メチル]-4-メチルフェノラート、ジ-tert-ブチルメチルホスホニウムテトラフェニルボレート等の脂肪族ホスホニウム塩;メチルトリフェニルホスホニウムブロマイド、エチルトリフェニルホスホニウムブロマイド、プロピルトリフェニルホスホニウムブロマイド、ブチルトリフェニルホスホニウムブロマイド、ベンジルトリフェニルホスホニウムクロライド、テトラフェニルホスホニウムブロマイド、p-トリルトリフェニルホスホニウムテトラ-p-トリルボレート、テトラフェニルホスホニウムテトラフェニルボレート、テトラフェニルホスホニウムテトラp-トリルボレート、トリフェニルエチルホスホニウムテトラフェニルボレート、トリス(3-メチルフェニル)エチルホスホニウムテトラフェニルボレート、トリス(2-メトキシフェニル)エチルホスホニウムテトラフェニルボレート、(4-メチルフェニル)トリフェニルホスホニウムチオシアネート、テトラフェニルホスホニウムチオシアネート、ブチルトリフェニルホスホニウムチオシアネート等の芳香族ホスホニウム塩等が挙げられる。
Examples of the phosphonium salt include tetrabutylphosphonium bromide, tetrabutylphosphonium chloride, tetrabutylphosphonium acetate, tetrabutylphosphonium decanoate, tetrabutylphosphonium laurate, bis (tetrabutylphosphonium) pyromeritate, and tetrabutylphosphonium hydroxyhexahydro. Fat group phosphonium salts such as phthalate,
ホスフィンとしては、例えば、トリブチルホスフィン、トリ-tert-ブチルホスフィン、トリオクチルホスフィン、ジ-tert-ブチル(2-ブテニル)ホスフィン、ジ-tert-ブチル(3-メチル-2-ブテニル)ホスフィン、トリシクロヘキシルホスフィン等の脂肪族ホスフィン;ジブチルフェニルホスフィン、ジ-tert-ブチルフェニルホスフィン、メチルジフェニルホスフィン、エチルジフェニルホスフィン、ブチルジフェニルホスフィン、ジフェニルシクロヘキシルホスフィン、トリフェニルホスフィン、トリ-o-トリルホスフィン、トリ-m-トリルホスフィン、トリ-p-トリルホスフィン、トリス(4-エチルフェニル)ホスフィン、トリス(4-プロピルフェニル)ホスフィン、トリス(4-イソプロピルフェニル)ホスフィン、トリス(4-ブチルフェニル)ホスフィン、トリス(4-tert-ブチルフェニル)ホスフィン、トリス(2,4-ジメチルフェニル)ホスフィン、トリス(2,5-ジメチルフェニル)ホスフィン、トリス(2,6-ジメチルフェニル)ホスフィン、トリス(3,5-ジメチルフェニル)ホスフィン、トリス(2,4,6-トリメチルフェニル)ホスフィン、トリス(2,6-ジメチル-4-エトキシフェニル)ホスフィン、トリス(2-メトキシフェニル)ホスフィン、トリス(4-メトキシフェニル)ホスフィン、トリス(4-エトキシフェニル)ホスフィン、トリス(4-tert-ブトキシフェニル)ホスフィン、ジフェニル-2-ピリジルホスフィン、1,2-ビス(ジフェニルホスフィノ)エタン、1,3-ビス(ジフェニルホスフィノ)プロパン、1,4-ビス(ジフェニルホスフィノ)ブタン、1,2-ビス(ジフェニルホスフィノ)アセチレン、2,2’-ビス(ジフェニルホスフィノ)ジフェニルエーテル等の芳香族ホスフィン;トリフェニルホスフィン・トリフェニルボラン等の芳香族ホスフィン・ボラン複合体;トリフェニルホスフィン・p-ベンゾキノン付加反応物等の芳香族ホスフィン・キノン付加反応物等が挙げられる。 Examples of phosphine include tributylphosphine, tri-tert-butylphosphine, trioctylphosphine, di-tert-butyl (2-butenyl) phosphine, di-tert-butyl (3-methyl-2-butenyl) phosphine, and tricyclohexyl. Aliphatic phosphines such as phosphine; dibutylphenylphosphine, di-tert-butylphenylphosphine, methyldiphenylphosphine, ethyldiphenylphosphine, butyldiphenylphosphine, diphenylcyclohexylphosphine, triphenylphosphine, tri-o-tolylphosphine, tri-m- Trilylphosphine, tri-p-trilphosphine, tris (4-ethylphenyl) phosphine, tris (4-propylphenyl) phosphine, tris (4-isopropylphenyl) phosphine, tris (4-butylphenyl) phosphine, tris (4-butylphenyl) tert-butylphenyl) phosphine, tris (2,4-dimethylphenyl) phosphine, tris (2,5-dimethylphenyl) phosphine, tris (2,6-dimethylphenyl) phosphine, tris (3,5-dimethylphenyl) phosphine , Tris (2,4,6-trimethylphenyl) phosphine, tris (2,6-dimethyl-4-ethoxyphenyl) phosphine, tris (2-methoxyphenyl) phosphine, tris (4-methoxyphenyl) phosphine, tris (4) -Ethoxyphenyl) phosphine, tris (4-tert-butoxyphenyl) phosphine, diphenyl-2-pyridylphosphine, 1,2-bis (diphenylphosphine) ethane, 1,3-bis (diphenylphosphine) propane, 1, Aromatic phosphines such as 4-bis (diphenylphosphine) butane, 1,2-bis (diphenylphosphine) acetylene, 2,2'-bis (diphenylphosphine) diphenyl ether; fragrances such as triphenylphosphine and triphenylborane. Group phosphine-boran complex; aromatic phosphine / quinone addition reaction product such as triphenylphosphine / p-benzoquinone addition reaction product and the like can be mentioned.
リン系硬化促進剤としては、市販品を用いてもよく、例えば、北興化学工業社製の「TBP-DA」等が挙げられる。 As the phosphorus-based curing accelerator, a commercially available product may be used, and examples thereof include "TBP-DA" manufactured by Hokuko Chemical Industry Co., Ltd.
イミダゾール系硬化促進剤としては、例えば、2-メチルイミダゾール、2-ウンデシルイミダゾール、2-ヘプタデシルイミダゾール、1,2-ジメチルイミダゾール、2-エチル-4-メチルイミダゾール、1,2-ジメチルイミダゾール、2-エチル-4-メチルイミダゾール、2-フェニルイミダゾール、2-フェニル-4-メチルイミダゾール、1-ベンジル-2-メチルイミダゾール、1-ベンジル-2-フェニルイミダゾール、1-シアノエチル-2-メチルイミダゾール、1-シアノエチル-2-ウンデシルイミダゾール、1-シアノエチル-2-エチル-4-メチルイミダゾール、1-シアノエチル-2-フェニルイミダゾール、1-シアノエチル-2-ウンデシルイミダゾリウムトリメリテイト、1-シアノエチル-2-フェニルイミダゾリウムトリメリテイト、2,4-ジアミノ-6-[2’-メチルイミダゾリル-(1’)]-エチル-s-トリアジン、2,4-ジアミノ-6-[2’-ウンデシルイミダゾリル-(1’)]-エチル-s-トリアジン、2,4-ジアミノ-6-[2’-エチル-4’-メチルイミダゾリル-(1’)]-エチル-s-トリアジン、2,4-ジアミノ-6-[2’-メチルイミダゾリル-(1’)]-エチル-s-トリアジンイソシアヌル酸付加物、2-フェニルイミダゾールイソシアヌル酸付加物、2-フェニル-4,5-ジヒドロキシメチルイミダゾール、2-フェニル-4-メチル-5-ヒドロキシメチルイミダゾール、2,3-ジヒドロ-1H-ピロロ[1,2-a]ベンズイミダゾール、1-ドデシル-2-メチル-3-ベンジルイミダゾリウムクロライド、2-メチルイミダゾリン、2-フェニルイミダゾリン等のイミダゾール化合物及びイミダゾール化合物とエポキシ樹脂とのアダクト体が挙げられ、2-エチル-4-メチルイミダゾール、1-ベンジル-2-フェニルイミダゾールが好ましい。 Examples of the imidazole-based curing accelerator include 2-methylimidazole, 2-undecylimidazole, 2-heptadecylimidazole, 1,2-dimethylimidazole, 2-ethyl-4-methylimidazole, 1,2-dimethylimidazole, and the like. 2-Ethyl-4-methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole, 1-benzyl-2-methylimidazole, 1-benzyl-2-phenylimidazole, 1-cyanoethyl-2-methylimidazole, 1-Cyanoethyl-2-undecylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, 1-cyanoethyl-2-phenylimidazole, 1-cyanoethyl-2-undecylimidazolium trimellitate, 1-cyanoethyl- 2-Phenylimidazolium trimellitate, 2,4-diamino-6- [2'-methylimidazolyl- (1')]-ethyl-s-triazine, 2,4-diamino-6- [2'-undecyl Imidazolyl- (1')]-ethyl-s-triazine, 2,4-diamino-6- [2'-ethyl-4'-methylimidazolyl- (1')]-ethyl-s-triazine, 2,4- Diamino-6- [2'-methylimidazolyl- (1')]-ethyl-s-triazine isocyanuric acid adduct, 2-phenylimidazole isocyanuric acid adduct, 2-phenyl-4,5-dihydroxymethylimidazole, 2- Phenyl-4-methyl-5-hydroxymethylimidazole, 2,3-dihydro-1H-pyrrolo [1,2-a] benzimidazole, 1-dodecyl-2-methyl-3-benzylimidazolium chloride, 2-methylimidazoline Examples thereof include imidazole compounds such as 2-phenylimidazolin and adducts of the imidazole compound and an epoxy resin, and 2-ethyl-4-methylimidazole and 1-benzyl-2-phenylimidazole are preferable.
イミダゾール系硬化促進剤としては、市販品を用いてもよく、例えば、三菱ケミカル社製の「P200-H50」、四国化成社製の「1B2PZ-10M」等が挙げられる。 As the imidazole-based curing accelerator, a commercially available product may be used, and examples thereof include "P200-H50" manufactured by Mitsubishi Chemical Corporation and "1B2PZ-10M" manufactured by Shikoku Kasei Co., Ltd.
アミン系硬化促進剤としては、例えば、トリエチルアミン、トリブチルアミン等のトリアルキルアミン、4-ジメチルアミノピリジン、ベンジルジメチルアミン、2,4,6,-トリス(ジメチルアミノメチル)フェノール、1,8-ジアザビシクロ(5,4,0)-ウンデセン等が挙げられ、4-ジメチルアミノピリジン、1,8-ジアザビシクロ(5,4,0)-ウンデセンが好ましい。 Examples of the amine-based curing accelerator include trialkylamines such as triethylamine and tributylamine, 4-dimethylaminopyridine, benzyldimethylamine, 2,4,6, -tris (dimethylaminomethyl) phenol, and 1,8-diazabicyclo. Examples thereof include (5,4,0) -undecene, and 4-dimethylaminopyridine and 1,8-diazabicyclo (5,4,0) -undecene are preferable.
グアニジン系硬化促進剤としては、例えば、ジシアンジアミド、1-メチルグアニジン、1-エチルグアニジン、1-シクロヘキシルグアニジン、1-フェニルグアニジン、1-(o-トリル)グアニジン、ジメチルグアニジン、ジフェニルグアニジン、トリメチルグアニジン、テトラメチルグアニジン、ペンタメチルグアニジン、1,5,7-トリアザビシクロ[4.4.0]デカ-5-エン、7-メチル-1,5,7-トリアザビシクロ[4.4.0]デカ-5-エン、1-メチルビグアニド、1-エチルビグアニド、1-n-ブチルビグアニド、1-n-オクタデシルビグアニド、1,1-ジメチルビグアニド、1,1-ジエチルビグアニド、1-シクロヘキシルビグアニド、1-アリルビグアニド、1-フェニルビグアニド、1-(o-トリル)ビグアニド等が挙げられ、ジシアンジアミド、1,5,7-トリアザビシクロ[4.4.0]デカ-5-エンが好ましい。 Examples of the guanidine-based curing accelerator include dicyandiamide, 1-methylguanidine, 1-ethylguanidine, 1-cyclohexylguanidine, 1-phenylguanidine, 1- (o-tolyl) guanidine, dimethylguanidine, diphenylguanidine, and trimethylguanidine. Tetramethylguanidine, pentamethylguanidine, 1,5,7-triazabicyclo [4.4.0] deca-5-ene, 7-methyl-1,5,7-triazabicyclo [4.4.0] Deca-5-ene, 1-methylbiguanide, 1-ethylbiguanide, 1-n-butylbiguanide, 1-n-octadecylviguanide, 1,1-dimethylbiguanide, 1,1-diethylbiguanide, 1-cyclohexylbiguanide, 1 -Allylbiguanide, 1-phenylbiguanide, 1- (o-tolyl) biguanide and the like can be mentioned, with dicyandiamide and 1,5,7-triazabicyclo [4.4.0] deca-5-ene being preferred.
金属系硬化促進剤としては、例えば、コバルト、銅、亜鉛、鉄、ニッケル、マンガン、スズ等の金属の、有機金属錯体又は有機金属塩が挙げられる。有機金属錯体の具体例としては、コバルト(II)アセチルアセトナート、コバルト(III)アセチルアセトナート等の有機コバルト錯体、銅(II)アセチルアセトナート等の有機銅錯体、亜鉛(II)アセチルアセトナート等の有機亜鉛錯体、鉄(III)アセチルアセトナート等の有機鉄錯体、ニッケル(II)アセチルアセトナート等の有機ニッケル錯体、マンガン(II)アセチルアセトナート等の有機マンガン錯体等が挙げられる。有機金属塩としては、例えば、オクチル酸亜鉛、オクチル酸錫、ナフテン酸亜鉛、ナフテン酸コバルト、ステアリン酸スズ、ステアリン酸亜鉛等が挙げられる。 Examples of the metal-based curing accelerator include organic metal complexes or organic metal salts of metals such as cobalt, copper, zinc, iron, nickel, manganese, and tin. Specific examples of the organic metal complex include an organic cobalt complex such as cobalt (II) acetylacetonate and cobalt (III) acetylacetonate, an organic copper complex such as copper (II) acetylacetonate, and zinc (II) acetylacetonate. Examples thereof include organic zinc complexes such as iron (III) acetylacetonate, organic nickel complexes such as nickel (II) acetylacetonate, and organic manganese complexes such as manganese (II) acetylacetonate. Examples of the organic metal salt include zinc octylate, tin octylate, zinc naphthenate, cobalt naphthenate, tin stearate, zinc stearate and the like.
硬化促進剤の含有量は、本発明の効果を顕著に得る観点から、樹脂組成物中の不揮発成分を100質量%とした場合、好ましくは5質量%以下、より好ましくは3質量%以下、さらに好ましくは1質量%以下、特に好ましくは0.8質量%以下であり、例えば、0質量%以上、0.001質量%以上であり、好ましくは0.01質量%以上、より好ましくは0.05質量%以上、特に好ましくは0.1質量%以上である。 The content of the curing accelerator is preferably 5% by mass or less, more preferably 3% by mass or less, and further, when the non-volatile component in the resin composition is 100% by mass, from the viewpoint of remarkably obtaining the effect of the present invention. It is preferably 1% by mass or less, particularly preferably 0.8% by mass or less, for example, 0% by mass or more, 0.001% by mass or more, preferably 0.01% by mass or more, and more preferably 0.05. By mass or more, particularly preferably 0.1% by mass or more.
-その他の添加剤-
樹脂組成物は、不揮発成分として、その他の添加剤をさらに含有してよい。その他の添加剤としては、例えば、(メタ)アクリル樹脂、ラジカル重合性化合物等の光硬化性成分並びにその助剤としての希釈剤、光重合開始剤等;ゴム粒子等の有機充填材;シリコーン系レベリング剤、アクリルポリマー系レベリング剤等のレベリング剤;ベントン、モンモリロナイト等の増粘剤;シリコーン系消泡剤、アクリル系消泡剤、フッ素系消泡剤、ビニル樹脂系消泡剤等の消泡剤;ベンゾフェノン系紫外線吸収剤、ベンゾトリアゾール系紫外線吸収剤、サリチル酸系紫外線吸収剤等の紫外線吸収剤;尿素シラン等の接着性向上剤;トリアゾール系密着性付与剤、テトラゾール系密着性付与剤、トリアジン系密着性付与剤等の密着性付与剤;ヒンダードフェノール系酸化防止剤等の酸化防止剤;スチルベン誘導体等の蛍光増白剤;フッ素系界面活性剤、シリコーン系界面活性剤等の界面活性剤;リン系難燃剤(例えばリン酸エステル化合物、ホスファゼン化合物、ホスフィン酸化合物、赤リン)、窒素系難燃剤(例えば硫酸メラミン)、ハロゲン系難燃剤、無機系難燃剤(例えば三酸化アンチモン)等の難燃剤;リン酸エステル系分散剤、ポリオキシアルキレン系分散剤、アセチレン系分散剤、シリコーン系分散剤、アニオン性分散剤、カチオン性分散剤等の分散剤;ボレート系安定剤、チタネート系安定剤、アルミネート系安定剤、ジルコネート系安定剤、イソシアネート系安定剤、カルボン酸系安定剤、カルボン酸無水物系安定剤等の安定剤等が挙げられる。その他の添加剤は、1種を単独で用いてもよく、2種以上を任意の比率で組み合わせて用いてもよい。その他の添加剤の含有量は当業者であれば適宜設定できる。
-Other additives-
The resin composition may further contain other additives as a non-volatile component. Examples of other additives include (meth) acrylic resins, photocurable components such as radically polymerizable compounds, diluents as auxiliaries thereof, photopolymerization initiators and the like; organic fillers such as rubber particles; silicone-based Leveling agents such as leveling agents and acrylic polymer leveling agents; thickeners such as Benton and montmorillonite; defoaming agents such as silicone-based defoaming agents, acrylic defoaming agents, fluorine-based defoaming agents and vinyl resin-based defoaming agents. Agents; UV absorbers such as benzophenone-based UV absorbers, benzotriazole-based UV absorbers, salicylic acid-based UV absorbers; Adhesive improvers such as ureasilane; Triazole-based adhesion-imparting agents, tetrazole-based adhesion-imparting agents, triazine Adhesion-imparting agents such as system-adhesion-imparting agents; Antioxidants such as hindered phenol-based antioxidants; Fluorescent whitening agents such as stilben derivatives; Surfactants such as fluorine-based surfactants and silicone-based surfactants ; Phosphorus flame retardant (eg phosphoric acid ester compound, phosphazene compound, phosphinic acid compound, red phosphorus), nitrogen flame retardant (eg melamine sulfate), halogen flame retardant, inorganic flame retardant (eg antimony trioxide), etc. Flame retardant; Dispersants such as phosphate ester dispersants, polyoxyalkylene dispersants, acetylene dispersants, silicone dispersants, anionic dispersants, cationic dispersants; borate stabilizers, titanate stabilizers , Aluminate-based stabilizers, zirconate-based stabilizers, isocyanate-based stabilizers, carboxylic acid-based stabilizers, carboxylic acid anhydride-based stabilizers and the like. As the other additives, one type may be used alone, or two or more types may be used in combination at any ratio. The content of other additives can be appropriately set by those skilled in the art.
-有機溶剤-
樹脂組成物は、上述した不揮発成分以外に、揮発性成分として、さらに任意の有機溶剤を含有する場合がある。有機溶剤としては、公知のものを適宜用いることができ、その種類は特に限定されるものではない。有機溶剤としては、例えば、アセトン、メチルエチルケトン、メチルイソブチルケトン、シクロヘキサノン等のケトン系溶剤;酢酸メチル、酢酸エチル、酢酸ブチル、酢酸イソブチル、酢酸イソアミル、プロピオン酸メチル、プロピオン酸エチル、γ-ブチロラクトン等のエステル系溶剤;テトラヒドロピラン、テトラヒドロフラン、1,4-ジオキサン、ジエチルエーテル、ジイソプロピルエーテル、ジブチルエーテル、ジフェニルエーテル等のエーテル系溶剤;メタノール、エタノール、プロパノール、ブタノール、エチレングリコール等のアルコール系溶剤;酢酸2-エトキシエチル、プロピレングリコールモノメチルエーテルアセテート、ジエチレングリコールモノエチルエーテルアセテート、エチルジグリコールアセテート、γ-ブチロラクトン、メトキシプロピオン酸メチル等のエーテルエステル系溶剤;乳酸メチル、乳酸エチル、2-ヒドロキシイソ酪酸メチル等のエステルアルコール系溶剤;2-メトキシプロパノール、2-メトキシエタノール、2-エトキシエタノール、プロピレングリコールモノメチルエーテル、ジエチレングリコールモノブチルエーテル(ブチルカルビトール)等のエーテルアルコール系溶剤;N,N-ジメチルホルムアミド、N,N-ジメチルアセトアミド、N-メチル-2-ピロリドン等のアミド系溶剤;ジメチルスルホキシド等のスルホキシド系溶剤;アセトニトリル、プロピオニトリル等のニトリル系溶剤;ヘキサン、シクロペンタン、シクロヘキサン、メチルシクロヘキサン等の脂肪族炭化水素系溶剤;ベンゼン、トルエン、キシレン、エチルベンゼン、トリメチルベンゼン等の芳香族炭化水素系溶剤等を挙げることができる。有機溶剤は、1種単独で用いてもよく、2種以上を任意の比率で組み合わせて用いてもよい。
-Organic solvent-
The resin composition may further contain an arbitrary organic solvent as a volatile component in addition to the above-mentioned non-volatile component. As the organic solvent, known ones can be appropriately used, and the type thereof is not particularly limited. Examples of the organic solvent include ketone solvents such as acetone, methyl ethyl ketone, methyl isobutyl ketone and cyclohexanone; methyl acetate, ethyl acetate, butyl acetate, isobutyl acetate, isoamyl acetate, methyl propionate, ethyl propionate, γ-butyrolactone and the like. Ester-based solvent; Ether-based solvent such as tetrahydropyran, tetrahydrofuran, 1,4-dioxane, diethyl ether, diisopropyl ether, dibutyl ether, diphenyl ether; Alcohol-based solvent such as methanol, ethanol, propanol, butanol, ethylene glycol; 2-Acetic acid Ether ester solvents such as ethoxyethyl, propylene glycol monomethyl ether acetate, diethylene glycol monoethyl ether acetate, ethyl diglycol acetate, γ-butyrolactone, methyl methoxypropionate; esters such as methyl lactate, ethyl lactate, methyl 2-hydroxyisobutyrate, etc. Alcohol-based solvent; ether alcohol-based solvent such as 2-methoxypropanol, 2-methoxyethanol, 2-ethoxyethanol, propylene glycol monomethyl ether, diethylene glycol monobutyl ether (butyl carbitol); N, N-dimethylformamide, N, N- Amido-based solvents such as dimethylacetamide and N-methyl-2-pyrrolidone; Sulfoxide-based solvents such as dimethylsulfoxide; Nitrile-based solvents such as acetonitrile and propionitrile; aliphatic hydrocarbons such as hexane, cyclopentane, cyclohexane and methylcyclohexane System solvent: Aromatic hydrocarbon solvents such as benzene, toluene, xylene, ethylbenzene, and trimethylbenzene can be mentioned. The organic solvent may be used alone or in combination of two or more at any ratio.
有機溶剤の含有量は、特に限定されるものではないが、樹脂組成物中の全成分を100質量%としたとき、例えば、65質量%以下、60質量%以下、45質量%以下、40質量%以下、30質量%以下、20質量%以下、15質量%以下、10質量%以下、5質量%以下等であり得る。 The content of the organic solvent is not particularly limited, but when all the components in the resin composition are 100% by mass, for example, 65% by mass or less, 60% by mass or less, 45% by mass or less, 40% by mass. % Or less, 30% by mass or less, 20% by mass or less, 15% by mass or less, 10% by mass or less, 5% by mass or less, and the like.
樹脂組成物は、例えば、任意の調製容器に白色無機顔料、熱硬化性樹脂、また、必要に応じて、他の無機充填材、硬化剤、熱可塑性樹脂、硬化促進剤、その他の添加剤や有機溶剤を、任意の順で及び/又は一部若しくは全部同時に加えて混合することによって、製造することができる。また、各成分を加えて混合する過程で、温度を適宜設定することができ、一時的に又は終始にわたって、加熱及び/又は冷却してもよい。また、加えて混合する過程において又はその後に、樹脂組成物を、例えば、ミキサーなどの撹拌装置又は振盪装置を用いて撹拌又は振盪し、均一に分散させてもよい。また、撹拌又は振盪と同時に、真空下等の低圧条件下で脱泡を行ってもよい。 The resin composition can be, for example, a white inorganic pigment, a thermosetting resin, and, if necessary, other inorganic fillers, curing agents, thermoplastic resins, curing accelerators, and other additives in any preparation container. It can be produced by adding and mixing organic solvents in any order and / or partially or all at the same time. Further, in the process of adding and mixing each component, the temperature can be appropriately set, and heating and / or cooling may be performed temporarily or from beginning to end. Further, the resin composition may be uniformly dispersed by stirring or shaking using, for example, a stirring device such as a mixer or a shaking device in the process of adding and mixing, or thereafter. Further, at the same time as stirring or shaking, defoaming may be performed under low pressure conditions such as under vacuum.
本発明の硬化体を形成するために使用する樹脂組成物は、下地基板上に硬化体を簡便かつ効率よく設けることができる観点から、また、無機充填材成分面積の比(A0-5/A5-10)が特定範囲にある硬化体を実現し易い観点から、該樹脂組成物の層を含む樹脂シートの形態で用いることが好適である。 The resin composition used for forming the cured product of the present invention is from the viewpoint that the cured product can be easily and efficiently provided on the base substrate, and the ratio of the component areas of the inorganic filler (A 0-5 /). From the viewpoint that it is easy to realize a cured product in which A 5-10 ) is in a specific range, it is preferable to use it in the form of a resin sheet containing a layer of the resin composition.
<樹脂シート>
一実施形態において、樹脂シートは、支持体と、該支持体上に設けられた、上記樹脂組成物の層(以下、単に「樹脂組成物層」という。)を含む。
<Resin sheet>
In one embodiment, the resin sheet includes a support and a layer of the resin composition provided on the support (hereinafter, simply referred to as "resin composition layer").
支持体としては、例えば、プラスチック材料からなるフィルム、金属箔、離型紙が挙げられ、プラスチック材料からなるフィルム、金属箔が好ましい。 Examples of the support include a film made of a plastic material, a metal foil, and a release paper, and a film made of a plastic material and a metal foil are preferable.
支持体としてプラスチック材料からなるフィルムを使用する場合、プラスチック材料としては、例えば、ポリエチレンテレフタレート(PET)、ポリエチレンナフタレート(PEN)等のポリエステル、ポリカーボネート(PC)、ポリメチルメタクリレート(PMMA)等のアクリル、環状ポリオレフィン、トリアセチルセルロース(TAC)、ポリエーテルサルファイド(PES)、ポリエーテルケトン、ポリイミド等が挙げられる。中でも、ポリエチレンテレフタレート、ポリエチレンナフタレートが好ましく、安価なポリエチレンテレフタレートが特に好ましい。 When a film made of a plastic material is used as the support, the plastic material includes, for example, polyester such as polyethylene terephthalate (PET) and polyethylene naphthalate (PEN), and acrylic such as polycarbonate (PC) and polymethylmethacrylate (PMMA). , Cyclic polyolefin, Triacetyl Cellulose (TAC), Polyether Sulfide (PES), Polyether Ketone, Polyimide and the like. Of these, polyethylene terephthalate and polyethylene naphthalate are preferable, and inexpensive polyethylene terephthalate is particularly preferable.
支持体として金属箔を使用する場合、金属箔としては、例えば、銅箔、アルミニウム箔等が挙げられ、銅箔が好ましい。銅箔としては、銅の単金属からなる箔を用いてもよく、銅と他の金属(例えば、スズ、クロム、銀、マグネシウム、ニッケル、ジルコニウム、ケイ素、チタン等)との合金からなる箔を用いてもよい。 When a metal foil is used as the support, examples of the metal foil include copper foil, aluminum foil, and the like, and copper foil is preferable. As the copper foil, a foil made of a single metal of copper may be used, and a foil made of an alloy of copper and another metal (for example, tin, chromium, silver, magnesium, nickel, zirconium, silicon, titanium, etc.) may be used. You may use it.
支持体は、樹脂組成物層と接合する面にマット処理、コロナ処理、帯電防止処理を施してあってもよい。 The support may be matted, corona-treated, or antistatic-treated on the surface to be joined to the resin composition layer.
また、支持体としては、樹脂組成物層と接合する面に離型層を有する離型層付き支持体を使用してもよい。離型層付き支持体の離型層に使用する離型剤としては、例えば、アルキド樹脂、ポリオレフィン樹脂、ウレタン樹脂、及びシリコーン樹脂からなる群から選択される1種以上の離型剤が挙げられる。離型層付き支持体は、市販品を用いてもよく、例えば、アルキド樹脂系離型剤を主成分とする離型層を有するPETフィルムである、リンテック社製の「PET501010」、「SK-1」、「AL-5」、「AL-7」;東レ社製の「ルミラーT60」;帝人社製の「ピューレックス」;ユニチカ社製の「ユニピール」等が挙げられる。 Further, as the support, a support with a release layer having a release layer on the surface to be joined to the resin composition layer may be used. Examples of the release agent used for the release layer of the support with the release layer include one or more release agents selected from the group consisting of alkyd resin, polyolefin resin, urethane resin, and silicone resin. .. As the support with a release layer, a commercially available product may be used. For example, "PET501010" and "SK-" manufactured by Lintec Corporation, which are PET films having a release layer containing an alkyd resin-based mold release agent as a main component. 1 ”,“ AL-5 ”,“ AL-7 ”;“ Lumilar T60 ”manufactured by Toray Industries, Inc .;“ Purelex ”manufactured by Teijin Ltd.;“ Unipeel ”manufactured by Unitika Ltd.
支持体の厚さは、特に限定されないが、5μm~75μmの範囲が好ましく、10μm~60μmの範囲がより好ましい。なお、離型層付き支持体を使用する場合、離型層付き支持体全体の厚さが上記範囲であることが好ましい。 The thickness of the support is not particularly limited, but is preferably in the range of 5 μm to 75 μm, and more preferably in the range of 10 μm to 60 μm. When a support with a release layer is used, the thickness of the entire support with a release layer is preferably in the above range.
無機充填材成分面積の比(A0-5/A5-10)が特定範囲にある硬化体を実現し易い観点から、樹脂組成物層は、その最低溶融粘度が5000ポイズ以下であることが好ましく、より好ましくは2000ポイズ以下、さらに好ましくは1000ポイズ以下、特に好ましくは500ポイズ以下である。 From the viewpoint of facilitating the realization of a cured product in which the ratio of the component areas of the inorganic filler (A 0-5 / A 5-10 ) is in a specific range, the resin composition layer has a minimum melt viscosity of 5000 poise or less. It is preferable, more preferably 2000 poise or less, still more preferably 1000 poise or less, and particularly preferably 500 poise or less.
一実施形態において、樹脂シートは、さらに必要に応じて、その他の層を含んでいてもよい。斯かるその他の層としては、例えば、樹脂組成物層の支持体と接合していない面(即ち、支持体とは反対側の面)に設けられた、支持体に準じた保護フィルム等が挙げられる。保護フィルムの厚さは、特に限定されるものではないが、例えば、1μm~40μmである。保護フィルムを積層することにより、樹脂組成物層の表面へのゴミ等の付着やキズを抑制することができる。 In one embodiment, the resin sheet may further contain other layers, if necessary. Examples of such other layers include a protective film similar to the support provided on the surface of the resin composition layer that is not bonded to the support (that is, the surface opposite to the support). Be done. The thickness of the protective film is not particularly limited, but is, for example, 1 μm to 40 μm. By laminating the protective film, it is possible to suppress the adhesion and scratches of dust and the like on the surface of the resin composition layer.
樹脂シートは、例えば、液状の樹脂組成物をそのまま、或いは有機溶剤に樹脂組成物を溶解した樹脂ワニスを調製し、これを、ダイコーター等を用いて支持体上に塗布し、更に乾燥させて樹脂組成物層を形成させることにより製造することができる。 For the resin sheet, for example, a resin varnish prepared by dissolving the resin composition as it is in a liquid resin composition or in an organic solvent is applied onto a support using a die coater or the like, and further dried. It can be produced by forming a resin composition layer.
有機溶剤としては、樹脂組成物の成分として説明した有機溶剤と同様のものが挙げられる。有機溶剤は1種単独で使用してもよく、2種以上を組み合わせて使用してもよい。 Examples of the organic solvent include the same organic solvents as those described as the components of the resin composition. The organic solvent may be used alone or in combination of two or more.
乾燥は、加熱、熱風吹きつけ等の公知の方法により実施してよい。乾燥条件は特に限定されないが、樹脂組成物層中の有機溶剤の含有量が10質量%以下、好ましくは5質量%以下となるように乾燥させる。樹脂組成物(樹脂ワニス)中の有機溶剤の沸点によっても異なるが、例えば30質量%~60質量%の有機溶剤を含む樹脂組成物(樹脂ワニス)を用いる場合、50℃~150℃で3分間~10分間乾燥させることにより、樹脂組成物層を形成することができる。 Drying may be carried out by a known method such as heating or blowing hot air. The drying conditions are not particularly limited, but the resin composition layer is dried so that the content of the organic solvent is 10% by mass or less, preferably 5% by mass or less. Although it depends on the boiling point of the organic solvent in the resin composition (resin varnish), for example, when a resin composition (resin varnish) containing an organic solvent of 30% by mass to 60% by mass is used, the temperature is 50 ° C. to 150 ° C. for 3 minutes. The resin composition layer can be formed by drying for about 10 minutes.
樹脂シートは、ロール状に巻きとって保存することが可能である。樹脂シートが保護フィルムを有する場合、保護フィルムを剥がすことによって使用可能となる。 The resin sheet can be rolled up and stored. If the resin sheet has a protective film, it can be used by peeling off the protective film.
本発明の硬化体は、下地基板上に、少なくとも白色無機顔料を含む無機充填材成分を含有した上記樹脂組成物を設け、該樹脂組成物を硬化させることにより得られる。好ましくは、本発明の硬化体は、下地基板と樹脂組成物層とが接合するように、下地基板上に上記樹脂シートを積層した後、該樹脂組成物層を硬化させることにより得られる。 The cured product of the present invention can be obtained by providing the above resin composition containing an inorganic filler component containing at least a white inorganic pigment on a base substrate and curing the resin composition. Preferably, the cured product of the present invention is obtained by laminating the resin sheet on the base substrate so that the base substrate and the resin composition layer are bonded to each other, and then curing the resin composition layer.
下地基板と樹脂シートの積層は、プリント配線板の製造方法に関連して後述する工程(I)の条件にて実施してよい。また、樹脂組成物の硬化は、プリント配線板の製造方法に関連して後述する工程(II)の条件にて実施してよい。無機充填材成分面積の比(A0-5/A5-10)が特定範囲にある硬化体を実現し易い観点から、樹脂組成物を硬化させる前に予備加熱をしてもよく、加熱は予備加熱を含めて複数回行ってもよい。 The substrate and the resin sheet may be laminated under the conditions of step (I) described later in relation to the method for manufacturing a printed wiring board. Further, the curing of the resin composition may be carried out under the conditions of step (II) described later in relation to the method for manufacturing a printed wiring board. From the viewpoint of facilitating the realization of a cured product in which the ratio of the component areas of the inorganic filler (A 0-5 / A 5-10 ) is in a specific range, preheating may be performed before the resin composition is cured, and the heating may be performed. It may be performed a plurality of times including preheating.
[積層構造体]
本発明の積層構造体は、表面の少なくとも一部に導体層を備える基板(「下地基板」)と、該基板の上に設けられた本発明の硬化体とを含む。
[Laminated structure]
The laminated structure of the present invention includes a substrate having a conductor layer on at least a part of the surface (“underlying substrate”), and a cured body of the present invention provided on the substrate.
下地基板は、表面の少なくとも一部に導体層を備える限り特に限定されず、例えば、ガラスエポキシ基板、金属基板、ポリエステル基板、ポリイミド基板、BTレジン基板、熱硬化型ポリフェニレンエーテル基板等の基板の片面又は両面に導体層が形成されたものが挙げられる。また、導体層はパターン加工されていてもよい。基板の片面または両面に導体層(回路)が形成された基板は「内層回路基板」ということがある。またプリント配線板(光反射基板)を製造する際に、さらに絶縁層及び/又は導体層が形成されるべき中間製造物も本発明でいう「基板」に含まれる。光反射基板が部品内蔵回路板である場合、部品を内蔵した回路基板を使用してもよい。下地基板の上に設けられた本発明の硬化体の特徴や組成は、先述のとおりである。 The base substrate is not particularly limited as long as it has a conductor layer on at least a part of the surface, and is, for example, one side of a substrate such as a glass epoxy substrate, a metal substrate, a polyester substrate, a polyimide substrate, a BT resin substrate, and a thermosetting polyphenylene ether substrate. Alternatively, a conductor layer formed on both sides thereof may be mentioned. Further, the conductor layer may be patterned. A substrate in which a conductor layer (circuit) is formed on one side or both sides of a substrate is sometimes referred to as an "inner layer circuit board". Further, an intermediate product in which an insulating layer and / or a conductor layer should be further formed when manufacturing a printed wiring board (light reflecting board) is also included in the "board" in the present invention. When the light reflection board is a circuit board with built-in components, a circuit board with built-in components may be used. The characteristics and composition of the cured product of the present invention provided on the base substrate are as described above.
本発明の積層構造体は、硬化体の第1の主面近傍の領域に無機充填材成分リッチな相を有するため高い光反射率を呈する。また、本発明の積層構造体は、斯かる高い光反射率を、下地基板と硬化体との密着強度の低下なしに達成し得る。光反射率や密着強度に関しては、先述のとおりである。 The laminated structure of the present invention exhibits high light reflectance because it has a phase rich in the inorganic filler component in the region near the first main surface of the cured product. Further, the laminated structure of the present invention can achieve such a high light reflectance without a decrease in the adhesion strength between the base substrate and the cured body. The light reflectance and the adhesion strength are as described above.
[反射シート、プリント配線板]
本発明の反射シートは、本発明の硬化体を含む。また、本発明のプリント配線板は、本発明の反射シートを含む。図1に一例を示したように、プリント配線板1は、基板2上に反射シート3が形成されており、反射シート3の面31上に発光ダイオード(LED)等の光源4が配置されている。なお、基板2は、上記の「下地基板」に該当し(図1において導体層は図示せず)、反射シート3の面31は、上記の「第1の主面」に該当する。
[Reflective sheet, printed wiring board]
The reflective sheet of the present invention contains the cured product of the present invention. Further, the printed wiring board of the present invention includes the reflective sheet of the present invention. As an example shown in FIG. 1, in the printed wiring board 1, a
反射シートは、本発明の硬化体を含むことから、高い光反射率を呈すると共に、良好な下地密着性を呈する。光反射率や密着強度に関しては、先述のとおりである。 Since the reflective sheet contains the cured product of the present invention, it exhibits high light reflectance and good substrate adhesion. The light reflectance and the adhesion strength are as described above.
本発明のプリント配線板及び反射シートは、例えば、上述の樹脂シートを用いて下記(I)、(II)及び(III)の工程を含む方法により製造することができる。
(I)基板上に、樹脂シートの樹脂組成物層が基板と接合するように積層する工程
(II)樹脂組成物層を熱硬化して反射シートを形成する工程
(III)反射シートに光源を配置する工程
The printed wiring board and the reflective sheet of the present invention can be produced, for example, by using the above-mentioned resin sheet by a method including the following steps (I), (II) and (III).
(I) A step of laminating the resin composition layer of the resin sheet on the substrate so as to be bonded to the substrate (II) A step of thermosetting the resin composition layer to form a reflective sheet (III) A light source on the reflective sheet Placement process
工程(I)で用いる基板は、表面の少なくとも一部に導体層を備える限り特に限定されず、先述のとおり、例えば、表面に導体回路を備えた回路基板を用い得る。 The substrate used in the step (I) is not particularly limited as long as the conductor layer is provided on at least a part of the surface, and as described above, for example, a circuit board having a conductor circuit on the surface can be used.
基板と樹脂シートの積層は、例えば、支持体側から樹脂シートを基板に加熱圧着することにより行うことができる。樹脂シートを基板に加熱圧着する部材(以下、「加熱圧着部材」ともいう。)としては、例えば、加熱された金属板(SUS鏡板等)又は金属ロール(SUSロール)等が挙げられる。なお、加熱圧着部材を樹脂シートに直接プレスするのではなく、基板の表面凹凸に樹脂シートが十分に追随するよう、耐熱ゴム等の弾性材を介してプレスするのが好ましい。 The substrate and the resin sheet can be laminated, for example, by heat-pressing the resin sheet to the substrate from the support side. Examples of the member for heat-crimping the resin sheet to the substrate (hereinafter, also referred to as “heat-crimping member”) include a heated metal plate (SUS end plate or the like) or a metal roll (SUS roll). It is preferable not to press the heat-bonded member directly onto the resin sheet, but to press it through an elastic material such as heat-resistant rubber so that the resin sheet sufficiently follows the surface irregularities of the substrate.
基板と樹脂シートの積層は、真空ラミネート法により実施してよい。真空ラミネート法において、加熱圧着温度は、好ましくは60℃~160℃、より好ましくは80℃~140℃の範囲であり、加熱圧着圧力は、好ましくは0.098MPa~1.77MPa、より好ましくは0.29MPa~1.47MPaの範囲であり、加熱圧着時間は、好ましくは20秒間~400秒間、より好ましくは30秒間~300秒間の範囲である。積層は、好ましくは圧力26.7hPa以下の減圧条件下で実施する。 The substrate and the resin sheet may be laminated by a vacuum laminating method. In the vacuum laminating method, the heat crimping temperature is preferably in the range of 60 ° C. to 160 ° C., more preferably 80 ° C. to 140 ° C., and the heat crimping pressure is preferably 0.098 MPa to 1.77 MPa, more preferably 0. It is in the range of .29 MPa to 1.47 MPa, and the heat crimping time is preferably in the range of 20 seconds to 400 seconds, more preferably 30 seconds to 300 seconds. Lamination is preferably carried out under reduced pressure conditions with a pressure of 26.7 hPa or less.
積層は、市販の真空ラミネーターによって行うことができる。市販の真空ラミネーターとしては、例えば、名機製作所社製の真空加圧式ラミネーター、ニッコー・マテリアルズ社製のバキュームアップリケーター、バッチ式真空加圧ラミネーター等が挙げられる。 Lamination can be performed by a commercially available vacuum laminator. Examples of the commercially available vacuum laminator include a vacuum pressurizing laminator manufactured by Meiki Co., Ltd., a vacuum applicator manufactured by Nikko Materials, and a batch type vacuum pressurizing laminator.
積層の後に、常圧下(大気圧下)、例えば、加熱圧着部材を支持体側からプレスすることにより、積層された樹脂シートの平滑化処理を行ってもよい。平滑化処理のプレス条件は、上記積層の加熱圧着条件と同様の条件とすることができる。平滑化処理は、市販のラミネーターによって行うことができる。なお、積層と平滑化処理は、上記の市販の真空ラミネーターを用いて連続的に行ってもよい。 After laminating, the laminated resin sheet may be smoothed by pressing under normal pressure (under atmospheric pressure), for example, from the support side. The press conditions for the smoothing treatment can be the same as the heat-bonding conditions for the above-mentioned lamination. The smoothing process can be performed by a commercially available laminator. The laminating and smoothing treatment may be continuously performed using the above-mentioned commercially available vacuum laminator.
支持体は、工程(I)と工程(II)の間に除去してもよく、工程(II)の後に除去してもよい。無機充填材成分面積の比(A0-5/A5-10)が特定範囲にある硬化体を実現し易い観点から、工程(I)と工程(II)の間に支持体を除去することが好ましい。 The support may be removed between steps (I) and step (II) or after step (II). From the viewpoint of facilitating the realization of a cured product in which the ratio of the component areas of the inorganic filler (A 0-5 / A 5-10 ) is in a specific range, the support is removed between the steps (I) and the step (II). Is preferable.
工程(II)において、樹脂組成物層を熱硬化して反射シートを形成する。例えば、樹脂組成物層の熱硬化条件は、樹脂組成物の種類等によっても異なるが、硬化温度は好ましくは120℃~240℃、より好ましくは130℃~220℃、さらに好ましくは150℃~210℃である。硬化時間は好ましくは5分間~120分間、より好ましくは10分間~100分間、さらに好ましくは15分間~100分間とすることができる。 In step (II), the resin composition layer is thermally cured to form a reflective sheet. For example, the thermosetting conditions of the resin composition layer differ depending on the type of the resin composition and the like, but the curing temperature is preferably 120 ° C to 240 ° C, more preferably 130 ° C to 220 ° C, still more preferably 150 ° C to 210. ℃. The curing time can be preferably 5 minutes to 120 minutes, more preferably 10 minutes to 100 minutes, and even more preferably 15 minutes to 100 minutes.
樹脂組成物を硬化させる前に、樹脂組成物を硬化温度よりも低い温度にて予備加熱してもよい。例えば、樹脂組成物を熱硬化させるのに先立ち、50℃以上120℃未満(好ましくは60℃以上115℃以下、より好ましくは70℃以上110℃以下)の温度にて、樹脂組成物を5分間以上(好ましくは5分間~150分間、より好ましくは15分間~120分間、さらに好ましくは15分間~100分間)予備加熱してもよい。 Before curing the resin composition, the resin composition may be preheated at a temperature lower than the curing temperature. For example, prior to thermosetting the resin composition, the resin composition is heated at a temperature of 50 ° C. or higher and lower than 120 ° C. (preferably 60 ° C. or higher and 115 ° C. or lower, more preferably 70 ° C. or higher and 110 ° C. or lower) for 5 minutes. Preheating may be performed as described above (preferably 5 minutes to 150 minutes, more preferably 15 minutes to 120 minutes, still more preferably 15 minutes to 100 minutes).
反射シートは、光源から発せられる光の取り出し効率を高めるため、反射シートの光源側の面は、図1のような平面状以外に凹部を有していてもよい。 In order to increase the efficiency of extracting light emitted from the light source, the reflective sheet may have a concave portion on the surface of the reflective sheet on the light source side in addition to the planar shape as shown in FIG.
工程(III)において、光源を反射シートに配置する。例えば、反射シートの面に凹部を有する場合は、凹部内に光源を配置する。 In step (III), the light source is placed on the reflective sheet. For example, when the surface of the reflective sheet has a recess, the light source is arranged in the recess.
必要に応じて光源を電気的に接続した後、光源に封止処理等を行い、光源を固定してもよい。 If necessary, after electrically connecting the light source, the light source may be sealed or the like to fix the light source.
本発明のプリント配線板において、上記の反射シートは、層間絶縁層又はソルダーレジストとして含まれてもよい。したがって、一実施形態において、本発明のプリント配線板は、本発明の反射シートを層間絶縁層又はソルダーレジストとして含む。 In the printed wiring board of the present invention, the reflective sheet may be included as an interlayer insulating layer or a solder resist. Therefore, in one embodiment, the printed wiring board of the present invention includes the reflective sheet of the present invention as an interlayer insulating layer or a solder resist.
[半導体装置]
本発明の半導体装置は、本発明のプリント配線板を含む。本発明の半導体装置は、プリント配線板の導通箇所に、部品(半導体チップ)を実装することにより製造することができる。例えば、携帯端末、コンピューター、テレビ等の液晶ディスプレイのバックライト;照明器具の光源など、低電力で発光する発光ダイオード(LED)を実装した半導体装置が挙げられる。
[Semiconductor device]
The semiconductor device of the present invention includes the printed wiring board of the present invention. The semiconductor device of the present invention can be manufactured by mounting a component (semiconductor chip) on a conductive portion of a printed wiring board. For example, a semiconductor device equipped with a light emitting diode (LED) that emits light with low power, such as a backlight of a liquid crystal display such as a mobile terminal, a computer, or a television; or a light source of a lighting fixture.
以下、本発明を実施例により具体的に説明する。本発明はこれらの実施例に限定されるものではない。なお、以下において、量を表す「部」及び「%」は、別途明示のない限り、それぞれ「質量部」及び「質量%」を意味する。特に温度の指定が無い場合の温度条件及び圧力条件は、室温(25℃)及び大気圧(1atm)である。 Hereinafter, the present invention will be specifically described with reference to Examples. The present invention is not limited to these examples. In the following, "parts" and "%" representing quantities mean "parts by mass" and "% by mass", respectively, unless otherwise specified. When the temperature is not specified, the temperature and pressure conditions are room temperature (25 ° C.) and atmospheric pressure (1 atm).
<実施例1>
(1)樹脂組成物の調製
液状ビスフェノールA型エポキシ樹脂(三菱ケミカル社製「jER828EL」、エポキシ当量180g/eq.)4部、固体状フッ素原子含有エポキシ樹脂(三菱ケミカル社製「YX7760」、エポキシ当量245g/eq.)4部、ビフェニル骨格及びシクロヘキサン骨格含有フェノキシ樹脂((三菱ケミカル社製「YX7200B35」、重量平均分子量30,000、20μm膜光透過率(450nm)88%、固形分35質量%のMEK溶液)20部を、MEK8部に撹拌しながら加熱溶解させた。そこへ、酸化チタン(堺化学工業社製「PX3788」、フェニルシランカップリング剤(信越化学工業社「KBM-103」)処理済み、平均粒径0.26μm、比表面積13.2m2/g、波長500nmの光に対する反射率99%)10部、球形シリカ(アドマテックス社製「SO-C2」、メタクリル系シランカップリング剤(信越化学工業社「KBM-503」)処理済み、平均粒径0.5μm、波長500nmの光に対する反射率約80%)10部、ビスフェノールAF(セントラル硝子社製「BIS-AF」をMEKで不揮発成分50%に調整した溶液)4部、リン系硬化促進剤(北興化学工業社製「TBP-DA」)0.2部を混合し、高速回転ミキサーで均一に分散して、樹脂組成物(ワニス)を調製した。
<Example 1>
(1) Preparation of resin composition Liquid bisphenol A type epoxy resin (Mitsubishi Chemical Corporation "jER828EL", epoxy equivalent 180 g / eq.), 4 parts, solid fluorine atom-containing epoxy resin (Mitsubishi Chemical Corporation "YX7760", epoxy Equivalent 245 g / eq.) 4 parts, biphenyl skeleton and cyclohexane skeleton-containing phenoxy resin ((Mitsubishi Chemical Corporation "YX7200B35", weight average molecular weight 30,000, 20 μm film light transmittance (450 nm) 88%, solid content 35% by mass) 20 parts of MEK solution) was heated and dissolved in 8 parts of MEK while stirring. Titanium oxide (“PX3788” manufactured by Sakai Chemical Industry Co., Ltd., phenylsilane coupling agent (“KBM-103” manufactured by Shinetsu Chemical Industry Co., Ltd.)). Treated, average particle size 0.26 μm, specific surface area 13.2 m 2 / g, reflectance 99% for light with a wavelength of 500 nm) 10 parts, spherical silica (“SO-C2” manufactured by Admatex, methacrylic silane coupling) Agent (Shinetsu Chemical Industry Co., Ltd. "KBM-503") treated, average particle size 0.5 μm, reflectance about 80% for light with a wavelength of 500 nm) 10 parts, bisphenol AF (Central Glass Co., Ltd. "BIS-AF" MEK Mix 4 parts of a solution adjusted to 50% non-volatile component and 0.2 part of a phosphorus-based curing accelerator (“TBP-DA” manufactured by Hokuko Kagaku Kogyo Co., Ltd.) and uniformly disperse with a high-speed rotary mixer to form a resin composition. A thing (wanice) was prepared.
(2)樹脂シートの調製
支持体として、離型層付きPETフィルム(リンテック社製「PET501010」、厚さ38μm)を用意した。この支持体の離型層上に、上記(1)で調製した樹脂組成物を、乾燥後の樹脂組成物層の厚さが50μmとなるように均一に塗布した。その後、樹脂組成物を80℃で4分間加熱することで厚さが50μmの樹脂組成物層を含む樹脂シートを得た。
(2) Preparation of resin sheet As a support, a PET film with a release layer (“PET501010” manufactured by Lintec Corporation, thickness 38 μm) was prepared. The resin composition prepared in (1) above was uniformly applied onto the release layer of the support so that the thickness of the dried resin composition layer was 50 μm. Then, the resin composition was heated at 80 ° C. for 4 minutes to obtain a resin sheet containing a resin composition layer having a thickness of 50 μm.
(3)硬化体の製造
(i)回路基板の下地処理
ガラス布基材エポキシ樹脂両面銅張積層板(銅箔の厚さ18μm、基板の厚さ0.8mm、松下電工社製「R5715ES」)の両面に、エッチングにより回路パターンを形成し、面内銅面積が30%の内層回路基板を作製した。得られた内層回路基板の銅回路を、マイクロエッチング剤(メック社製「CZ8100」)で粗化処理した。
(3) Manufacture of cured product (i) Substrate treatment of circuit board Glass cloth base material Epoxy resin double-sided copper-clad laminate (copper foil thickness 18 μm, substrate thickness 0.8 mm, “R5715ES” manufactured by Matsushita Electric Industrial Co., Ltd.) A circuit pattern was formed on both sides of the surface by etching to prepare an inner layer circuit board having an in-plane copper area of 30%. The copper circuit of the obtained inner layer circuit board was roughened with a micro-etching agent (“CZ8100” manufactured by MEC).
(ii)樹脂シートのラミネート
上記(2)で調製した樹脂シートを、バッチ式真空加圧ラミネーター(名機製作所社製「MVLP-500」)を用いて、樹脂組成物層が内層回路基板と接合するように、下地処理した内層回路基板の両面にラミネートした。ラミネートは、30秒間減圧して気圧を13hPa以下とし、その後120℃、30秒間、圧力0.74MPaで圧着させることにより行った。
(Ii) Laminating of resin sheet The resin sheet prepared in (2) above is bonded to the inner layer circuit board by using a batch type vacuum pressurizing laminator (“MVLP-500” manufactured by Meiki Co., Ltd.). It was laminated on both sides of the base-treated inner layer circuit board so as to be used. Lamination was performed by reducing the pressure for 30 seconds to a pressure of 13 hPa or less, and then crimping at 120 ° C. for 30 seconds at a pressure of 0.74 MPa.
(iii)樹脂組成物層の熱硬化
支持体を剥離した後、180℃、90分間加熱して樹脂組成物層を硬化させた。これにより、回路基板と該回路基板上に設けられた硬化体とを含む積層構造体を得た。
(Iii) Thermal curing of the resin composition layer After the support was peeled off, the resin composition layer was cured by heating at 180 ° C. for 90 minutes. As a result, a laminated structure including a circuit board and a cured product provided on the circuit board was obtained.
<実施例2>
液状ビスフェノールA型エポキシ樹脂(三菱ケミカル社製「jER828EL」、エポキシ当量180g/eq.)4部と固体状フッ素原子含有エポキシ樹脂(三菱ケミカル社製「YX7760」、エポキシ当量245g/eq.)4部に代えて、水添液状エポキシ樹脂(三菱ケミカル社製「YX8000」、エポキシ当量205g/eq.)4部とビフェニル型エポキシ樹脂(三菱ケミカル社製「YX4000H」、エポキシ当量195g/eq.)4部をそれぞれ使用した以外は、実施例1と同様にして、樹脂組成物、樹脂シートを調製し、硬化体、積層構造体を製造した。
<Example 2>
Liquid bisphenol A type epoxy resin (Mitsubishi Chemical "jER828EL", epoxy equivalent 180 g / eq.) 4 parts and solid fluorine atom-containing epoxy resin (Mitsubishi Chemical "YX7760", epoxy equivalent 245 g / eq.) 4 parts Instead, 4 parts of hydrogenated liquid epoxy resin (Mitsubishi Chemical "YX8000", epoxy equivalent 205 g / eq.) And 4 parts of biphenyl type epoxy resin (Mitsubishi Chemical "YX4000H", epoxy equivalent 195 g / eq.) In the same manner as in Example 1, a resin composition and a resin sheet were prepared, and a cured product and a laminated structure were produced.
<実施例3>
(1)酸化チタン(堺化学工業社製「PX3788」、フェニルシランカップリング剤処理済み)の配合量を10部から20部に変更した点、及び(2)球形シリカ(アドマテックス社製「SO-C2」、メタクリル系シランカップリング剤処理済み)を配合しなかった点以外は、実施例1と同様にして、樹脂組成物、樹脂シートを調製し、硬化体、積層構造体を製造した。
<Example 3>
(1) The amount of titanium oxide ("PX3788" manufactured by Sakai Chemical Industry Co., Ltd., treated with phenylsilane coupling agent) was changed from 10 parts to 20 parts, and (2) spherical silica ("SO" manufactured by Admatex Co., Ltd.). A resin composition and a resin sheet were prepared in the same manner as in Example 1 except that "-C2" (treated with a methacrylicsilane coupling agent) was not blended, and a cured product and a laminated structure were produced.
<実施例4>
ビスフェノールAF(セントラル硝子社製「BIS-AF」をMEKで不揮発分50%に調整した溶液)を配合しなかった以外は、実施例1と同様にして、樹脂組成物、樹脂シートを調製し、硬化体、積層構造体を製造した。
<Example 4>
A resin composition and a resin sheet were prepared in the same manner as in Example 1 except that bisphenol AF (a solution prepared by adjusting "BIS-AF" manufactured by Central Glass Co., Ltd. to a non-volatile content of 50% with MEK) was not blended. A cured body and a laminated structure were manufactured.
<実施例5>
ビフェニル骨格及びシクロヘキサン骨格含有フェノキシ樹脂(三菱ケミカル社製「YX7200B35」、重量平均分子量30,000、固形分35質量%のMEK溶液)20部に代えて、無官能基アクリル樹脂(東亞合成社製「ARUFON UP-1020」、重量平均分子量2,000)7部を使用した以外は、実施例1と同様にして、樹脂組成物、樹脂シートを調製し、硬化体、積層構造体を製造した。
<Example 5>
Instead of 20 parts of a phenoxy resin containing a biphenyl skeleton and a cyclohexane skeleton ("YX7200B35" manufactured by Mitsubishi Chemical Co., Ltd., a MEK solution having a weight average molecular weight of 30,000 and a solid content of 35% by mass), a non-functional acrylic resin (manufactured by Toagosei Co., Ltd. " ARUFON UP-1020 ”, weight average molecular weight 2,000) 7 parts) were used, but a resin composition and a resin sheet were prepared in the same manner as in Example 1 to produce a cured product and a laminated structure.
<実施例6>
ビフェニル骨格及びシクロヘキサン骨格含有フェノキシ樹脂(三菱ケミカル社製「YX7200B35」、重量平均分子量30,000、固形分35質量%のMEK溶液)20部に代えて、低分子ポリフェニレンエーテル樹脂(SABIC社製「Noryl SA90」、分子量1700、20μm膜光透過率(450nm)85%)7部を使用した以外は、実施例1と同様にして、樹脂組成物、樹脂シートを調製し、硬化体、積層構造体を製造した。
<Example 6>
Instead of 20 parts of a phenoxy resin containing a biphenyl skeleton and a cyclohexane skeleton ("YX7200B35" manufactured by Mitsubishi Chemical Co., Ltd., a MEK solution having a weight average molecular weight of 30,000 and a solid content of 35% by mass), a low molecular weight polyphenylene ether resin ("Noryl" manufactured by SABIC Co., Ltd.) A resin composition and a resin sheet were prepared in the same manner as in Example 1 except that 7 parts (SA90”, molecular weight 1700, 20 μm film light transmittance (450 nm) 85%) were used, and a cured product and a laminated structure were prepared. Manufactured.
<比較例1>
(1)酸化チタン(堺化学工業社製「PX3788」、フェニルシランカップリング剤処理済み)の配合量を10部から4部に変更した点、及び(2)球形シリカ(アドマテックス社製「SO-C2」、メタクリル系シランカップリング剤処理済み)の配合量を10部から18部に変更した以外は、実施例1と同様にして、樹脂組成物、樹脂シートを調製し、硬化体、積層構造体を製造した。
<Comparative Example 1>
(1) The amount of titanium oxide ("PX3788" manufactured by Sakai Chemical Industry Co., Ltd., treated with phenylsilane coupling agent) was changed from 10 parts to 4 parts, and (2) spherical silica ("SO" manufactured by Admatex Co., Ltd.). A resin composition and a resin sheet were prepared in the same manner as in Example 1 except that the blending amount of "-C2" (treated with a methacrylicsilane coupling agent) was changed from 10 parts to 18 parts, and the cured product and laminated body were prepared. The structure was manufactured.
<比較例2>
(1)酸化チタン(堺化学工業社製「PX3788」、フェニルシランカップリング剤処理済み)の配合量を10部から40部に変更した点、及び(2)球形シリカ(アドマテックス社製「SO-C2」、メタクリル系シランカップリング剤処理済み)を配合しなかった点以外は、実施例1と同様にして、樹脂組成物、樹脂シートを調製し、硬化体、積層構造体を製造した。
<Comparative Example 2>
(1) The amount of titanium oxide ("PX3788" manufactured by Sakai Chemical Industry Co., Ltd., treated with phenylsilane coupling agent) was changed from 10 parts to 40 parts, and (2) spherical silica ("SO" manufactured by Admatex Co., Ltd.). A resin composition and a resin sheet were prepared in the same manner as in Example 1 except that "-C2" (treated with a methacrylicsilane coupling agent) was not blended, and a cured product and a laminated structure were produced.
<比較例3>
(1)樹脂組成物の調製
ビフェニル型エポキシ樹脂(日本化薬社製「NC3000H」、エポキシ当量約272g/eq.)3部、テトラキスヒドロキシフェニルエタン型エポキシ樹脂(三菱ケミカル社製「jER1031S」、エポキシ当量約200g/eq.)2部、ビスフェノールA型エポキシアクリレート(日本化薬社製「ZAR-2000」、酸価99mgKOH/g、不揮発成分70%)10部、希釈剤(日本化薬社製「DPHA」、ジペンタエリスリトールヘキサアクリレート、アクリル当量約96g/eq.)1部を、MEK6部とエチルジグリコールアセテート10部に撹拌しながら加熱溶解させた。そこへ、酸化チタン(堺化学工業社製「PX3788」、フェニルシランカップリング剤(信越化学工業社「KBM-103」)処理済み、平均粒径0.26μm、比表面積13.2m2/g、波長500nmの光に対する反射率99%)4部、球形シリカ(アドマテックス製「SO-C2」、メタクリル系シランカップリング剤(信越化学工業社「KBM-503」処理済み、平均粒径0.5μm、波長500nmの光に対する反射率約80%)4部、光重合開始剤(BASF社製「Irgacure819」、ビス(2,4,6-トリメチルベンゾイル)-フェニルフォスフィンオキサイド)0.04部を混合し、高速回転ミキサーで均一に分散して、樹脂組成物を調製した。
<Comparative Example 3>
(1) Preparation of resin composition Biphenyl type epoxy resin (Nippon Kayaku Co., Ltd. "NC3000H", epoxy equivalent about 272 g / eq.), 3 parts, tetrakis hydroxyphenyl ethane type epoxy resin (Mitsubishi Chemical Co., Ltd. "jER1031S", epoxy Equivalent about 200 g / eq.) 2 parts, bisphenol A type epoxy acrylate (Nippon Kayaku Co., Ltd. "ZAR-2000", acid value 99 mgKOH / g, non-volatile component 70%) 10 parts, diluent (Nippon Kayaku Co., Ltd. "ZAR-2000" DPHA ”, dipentaerythritol hexaacrylate, acrylic equivalent of about 96 g / eq.) Was dissolved by heating in 6 parts of MEK and 10 parts of ethyl diglycol acetate with stirring. There, titanium oxide (“PX3788” manufactured by Sakai Chemical Industry Co., Ltd., phenylsilane coupling agent (“KBM-103” manufactured by Shinetsu Chemical Industry Co., Ltd.)) has been treated, the average particle size is 0.26 μm, and the specific surface area is 13.2 m 2 / g. 4 parts of spherical silica (admatex "SO-C2", methacrylicsilane coupling agent (Shinetsu Chemical Industry Co., Ltd. "KBM-503" treated), average particle size 0.5 μm) , 4 parts of photopolymerization initiator (BASF "Irgacure819", bis (2,4,6-trimethylbenzoyl) -phenylphosphin oxide) 0.04 part. Then, it was uniformly dispersed with a high-speed rotary mixer to prepare a resin composition.
(2)樹脂シートの調製
上記(1)で調製した樹脂組成物を使用して、実施例1と同様にして、樹脂シートを調製した。調製された樹脂シートは、支持体と、該支持体上に設けられた感光性樹脂組成物層を含む。
(2) Preparation of Resin Sheet Using the resin composition prepared in (1) above, a resin sheet was prepared in the same manner as in Example 1. The prepared resin sheet includes a support and a photosensitive resin composition layer provided on the support.
(3)硬化体の製造
実施例1と同様にして、(i)回路基板の下地処理と(ii)樹脂シートのラミネートを実施した。次いで、支持体を剥離した後、感光性樹脂組成物層に、100mJ/cm2の紫外線で露光を行い光硬化させた。その後、感光性樹脂組成物層の全面に、現像液として30℃の1質量%炭酸ナトリウム水溶液をスプレー圧0.2MPaにて2分間のスプレー現像を行った。スプレー現像後、1J/cm2の紫外線照射を行い、さらに190℃、90分間加熱して感光性樹脂組成物層を硬化させた。これにより、回路基板と該回路基板上に設けられた硬化体とを含む積層構造体を得た。
(3) Production of cured product In the same manner as in Example 1, (i) the substrate treatment of the circuit board and (ii) the laminating of the resin sheet were carried out. Then, after the support was peeled off, the photosensitive resin composition layer was exposed to ultraviolet rays of 100 mJ / cm 2 and photo-cured. Then, a 1% by mass sodium carbonate aqueous solution at 30 ° C. was spray-developed on the entire surface of the photosensitive resin composition layer at a spray pressure of 0.2 MPa for 2 minutes. After spray development, ultraviolet irradiation of 1 J / cm 2 was performed, and the mixture was further heated at 190 ° C. for 90 minutes to cure the photosensitive resin composition layer. As a result, a laminated structure including a circuit board and a cured product provided on the circuit board was obtained.
以下、各種測定方法・評価方法について説明する。 Hereinafter, various measurement methods and evaluation methods will be described.
<無機充填材成分面積比の測定>
(1)断面試料の作製
実施例及び比較例で製造した積層構造体について、硬化体の第1の主面に垂直な方向における断面が露出するように断面出しを行い、断面試料を作製した。断面出しには、走査型電子顕微鏡付属の集束イオンビーム(FIB)を用いた。
<Measurement of area ratio of inorganic filler components>
(1) Preparation of cross-section sample The laminated structures produced in Examples and Comparative Examples were cross-sectioned so that the cross-section in the direction perpendicular to the first main surface of the cured product was exposed, and a cross-section sample was prepared. A focused ion beam (FIB) attached to a scanning electron microscope was used for cross-sectioning.
(2)無機充填材成分面積比の算出
走査型電子顕微鏡(エスアイアイ・ナノテクノロジー社製集束イオンビーム/走査イオン顕微鏡「SMI3050SE」)を用いて断面試料を観察し、第1の主面に垂直な方向における硬化体の断面に係るSEM像を得た。得られたSEM像について、硬化体の第1の主面からの距離がd1(μm)からd2(μm)までの領域の無機充填材成分面積Ad1-d2と、第1の主面からの距離がd2(μm)からd3(μm)までの領域の無機充填材成分面積Ad2-d3を測定した。そして、得られたAd1-d2値及びAd2-d3値から無機充填材成分面積比(kAd1-d2/Ad2-d3)を算出した。
具体的には、得られたSEM像を画像として保存し、画像解析ソフト(アメリカ国立衛生研究所製「ImageJ」)を使用して、樹脂成分部分を黒色、樹脂成分以外の無機充填材成分部分を白色として白黒2値化し、各領域について白色部分のピクセル数として無機充填材成分の面積Ad1-d2値及びAd2-d3値を導出した。無機充填材成分面積の比A0-5/A5-10の算出にあたっては、d1=0(μm)、d2=5(μm)、d3=10(μm)、k=1であり、測定領域の幅は7.5μmとした。測定は10箇所について実施し、得られた平均値を無機充填材成分面積の比A0-5/A5-10とした。
なお、無機充填材成分面積比の測定に際しては、(無機充填材成分部分のピクセル数)/(断面試料の断面の全ピクセル数)×100の値が、断面試料の無機充填材成分の体積%値±3の範囲となるように2値化閾値を設定し、条件を校正した。
(2) Calculation of component area ratio of inorganic filler A cross-sectional sample was observed using a scanning electron microscope (focused ion beam / scanning ion microscope "SMI3050SE" manufactured by SI Nanotechnology Co., Ltd.) and perpendicular to the first main surface. An SEM image relating to the cross section of the cured product in the above direction was obtained. With respect to the obtained SEM image, the inorganic filler component area Ad1-d2 in the region where the distance from the first main surface of the cured product is from d1 (μm) to d2 (μm) and the area from the first main surface. The inorganic filler component area A d2-d3 in the region where the distance was from d2 (μm) to d3 (μm) was measured. Then, the inorganic filler component area ratio (kA d1-d2 / A d2-d3 ) was calculated from the obtained Ad1-d2 value and Ad2-d3 value.
Specifically, the obtained SEM image is saved as an image, and the resin component portion is blackened using image analysis software (“ImageJ” manufactured by the National Institutes of Health), and the inorganic filler component portion other than the resin component is used. Was converted into black and white and binarized, and the area Ad1-d2 value and Ad2-d3 value of the inorganic filler component were derived as the number of pixels in the white portion for each region. In calculating the ratio A 0-5 / A 5-10 of the component area of the inorganic filler, d1 = 0 (μm), d2 = 5 (μm), d3 = 10 (μm), k = 1, and the measurement area. The width of was 7.5 μm. The measurement was carried out at 10 points, and the obtained average value was taken as the ratio of the inorganic filler component area A 0-5 / A 5-10 .
When measuring the area ratio of the inorganic filler component, the value of (number of pixels of the inorganic filler component portion) / (total number of pixels of the cross section of the cross-sectional sample) × 100 is the volume% of the inorganic filler component of the cross-sectional sample. The binarization threshold was set so that the value was in the range of ± 3, and the conditions were calibrated.
<光反射率の測定>
実施例及び比較例で製造した積層構造体を幅50mm、長さ50mmに切り出し、マルチチャンネル分光器(大塚電子社製、MCPD-7700)にて、波長460nmの光に対する反射率(%)を測定し、以下の基準で評価した。
<Measurement of light reflectance>
The laminated structure manufactured in Examples and Comparative Examples was cut into a width of 50 mm and a length of 50 mm, and the reflectance (%) with respect to light having a wavelength of 460 nm was measured with a multi-channel spectroscope (MCPD-7700, manufactured by Otsuka Electronics Co., Ltd.). However, it was evaluated according to the following criteria.
光反射率の評価基準:
◎:反射率が95%以上
○:反射率が90%以上95%未満
△:反射率が80%以上90%未満
×:反射率が80%未満
Evaluation criteria for light reflectance:
⊚: Reflectance is 95% or more ○: Reflectance is 90% or more and less than 95% Δ: Reflectance is 80% or more and less than 90% ×: Reflectance is less than 80%
<下地密着性の測定>
(1)銅箔の下地処理
電解銅箔(三井金属鉱山社製「3EC-III」、厚さ35μm)の光沢面をマイクロエッチング剤(メック社製メックエッチボンド「CZ-8101」)に浸漬して、銅表面の粗化処理(Ra値=1μm)を行い、防錆処理(CL8300)を施した。次いで、130℃のオーブンで30分間加熱処理した。得られた銅箔を、以下、CZ銅箔という。
<Measurement of substrate adhesion>
(1) Base treatment of copper foil The glossy surface of electrolytic copper foil (“3EC-III” manufactured by Mitsui Mining & Smelting Co., Ltd., thickness 35 μm) is immersed in a micro-etching agent (Mech Etch Bond “CZ-8101” manufactured by Mech Co., Ltd.). Then, the copper surface was roughened (Ra value = 1 μm) and rust-proofed (CL8300). Then, it was heat-treated in an oven at 130 ° C. for 30 minutes. The obtained copper foil is hereinafter referred to as CZ copper foil.
(2)樹脂シートのラミネート
実施例及び比較例で調製した樹脂シートを、CZ銅箔にラミネートし、銅箔付き樹脂シートを作製した。ラミネート条件は、実施例1の「(3)硬化体の製造」におけるラミネート条件と同じであった。
(2) Laminating of Resin Sheets The resin sheets prepared in Examples and Comparative Examples were laminated on CZ copper foil to prepare a resin sheet with copper foil. The laminating conditions were the same as the laminating conditions in "(3) Production of cured product" of Example 1.
(3)樹脂組成物の硬化
上記(2)で作製した銅箔付き樹脂シートを用いて、実施例1の「(3)硬化体の製造」における熱硬化条件あるいは比較例3の「(3)硬化体の製造」における光硬化/熱硬化条件と同様の条件で硬化させ、銅箔付きの硬化体を得た。詳細には、実施例1~6及び比較例1、2で調製した樹脂シートを用いて作製した銅箔付き樹脂シートについては実施例1と同じ熱硬化条件を、比較例3で調製した樹脂シートを用いて作製した銅箔付き樹脂シートについては比較例3と同じ光硬化/熱硬化条件を適用した。
(3) Curing of Resin Composition Using the resin sheet with copper foil produced in (2) above, the thermosetting conditions in "(3) Production of cured product" of Example 1 or "(3) of Comparative Example 3" A cured product with a copper foil was obtained by curing under the same conditions as the photo-curing / thermosetting conditions in "Manufacturing a cured product". Specifically, for the resin sheet with copper foil produced by using the resin sheets prepared in Examples 1 to 6 and Comparative Examples 1 and 2, the same thermosetting conditions as in Example 1 were applied to the resin sheet prepared in Comparative Example 3. The same photocuring / thermosetting conditions as in Comparative Example 3 were applied to the resin sheet with a copper foil prepared using the above.
(4)回路基板への固定
上記(3)で得た銅箔付き硬化体を、硬化体が回路基板と接するように、下地処理した回路基板の両面に接着剤(アロンアルファEX)を用いて接着した。下地処理した回路基板は、実施例1の「(3)硬化体の製造」で準備したものと同じであった。
次いで、実施例1の「(3)硬化体の製造」におけるラミネート条件と同じ条件にて、銅箔付き硬化体と回路基板とをラミネートした。これにより、CZ銅箔/硬化体/回路基板/硬化体/CZ銅箔の層構成を有する評価用サンプル得た。
(4) Fixing to the circuit board The cured body with copper foil obtained in (3) above is adhered to both sides of the circuit board that has been grounded so that the cured body is in contact with the circuit board, using an adhesive (Aron Alpha EX). did. The ground-treated circuit board was the same as that prepared in "(3) Production of cured product" of Example 1.
Next, the cured product with copper foil and the circuit board were laminated under the same conditions as the laminating conditions in "(3) Production of the cured product" of Example 1. As a result, an evaluation sample having a layer structure of CZ copper foil / cured body / circuit board / cured body / CZ copper foil was obtained.
(5)下地密着性(密着強度)の測定
上記(4)で得た評価用サンプルを150×30mmの小片に切断した。小片の銅箔部分に、カッターを用いて幅10mm、長さ100mmの部分の切込みをいれて、銅箔の一端を剥がしてつかみ具(ティー・エス・イー社製オートコム型試験機「AC-50C-SL」)で掴み、インストロン万能試験機を用いて、室温中にて、50mm/分の速度で垂直方向に35mmを引き剥がした時の荷重をJIS C6481に準拠して測定し、以下の基準で評価した。
(5) Measurement of substrate adhesion (adhesion strength) The evaluation sample obtained in (4) above was cut into small pieces of 150 × 30 mm. Use a cutter to make a notch in the copper foil part of a small piece with a width of 10 mm and a length of 100 mm, peel off one end of the copper foil, and use a gripper (TSE Autocom type testing machine "AC-". 50C-SL ”), and using an Instron universal tester, measure the load when the 35 mm is peeled off vertically at a speed of 50 mm / min at room temperature in accordance with JIS C6481. Evaluated according to the criteria of.
下地密着性の評価基準:
◎:密着強度が0.5kgf/cm以上
〇:密着強度が0.4kgf/cm以上、0.5kgf/cm未満
△:密着強度が0.3kgf/cm以上、0.4kgf/cm未満
×:密着強度が0.3kgf/cm未満
Evaluation criteria for substrate adhesion:
⊚: Adhesion strength is 0.5 kgf / cm or more 〇: Adhesion strength is 0.4 kgf / cm or more and less than 0.5 kgf / cm Δ: Adhesion strength is 0.3 kgf / cm or more and less than 0.4 kgf / cm ×: Adhesion Strength is less than 0.3kgf / cm
実施例及び比較例で製造した硬化体の不揮発成分使用量と、測定結果及び評価結果を表1に示す。 Table 1 shows the amount of non-volatile components used in the cured products produced in Examples and Comparative Examples, and the measurement results and evaluation results.
1 プリント配線板
2 基板
3 反射シート
31 反射シートの面
4 光源
1 Printed
Claims (14)
該硬化体中の不揮発成分を100質量%としたとき、白色無機顔料の含有量が20質量%以上であり、
該硬化体の、基板と接していない側の表面を第1の主面としたとき、
該硬化体の第1の主面に垂直な方向における硬化体の断面において、硬化体の第1の主面からの距離が0μmから5μmまでの領域における単位面積当たりの無機充填材成分の面積A0-5と、第1の主面からの距離が5μmから10μmまでの領域における単位面積当たりの無機充填材成分の面積A5-10とが、A0-5/A5-10>1.1を満たす、硬化体。 A cured product of a resin composition containing an inorganic filler component containing at least a white inorganic pigment, which is provided on a substrate having a conductor layer on at least a part of the surface thereof.
When the non-volatile component in the cured product is 100% by mass, the content of the white inorganic pigment is 20% by mass or more.
When the surface of the cured product on the side not in contact with the substrate is used as the first main surface,
Area A of the inorganic filler component per unit area in the region where the distance from the first main surface of the cured body is from 0 μm to 5 μm in the cross section of the cured body in the direction perpendicular to the first main surface of the cured body. 0-5 and the area A 5-10 of the inorganic filler component per unit area in the region where the distance from the first main surface is from 5 μm to 10 μm are A 0-5 / A 5-10 > 1. A cured product that satisfies 1.
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KR1020210119848A KR20220034679A (en) | 2020-09-11 | 2021-09-08 | Cured product |
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