JP6441525B2 - 樹脂組成物用フィラー、フィラー含有スラリー組成物、及びフィラー含有樹脂組成物 - Google Patents
樹脂組成物用フィラー、フィラー含有スラリー組成物、及びフィラー含有樹脂組成物 Download PDFInfo
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- JP6441525B2 JP6441525B2 JP2018075757A JP2018075757A JP6441525B2 JP 6441525 B2 JP6441525 B2 JP 6441525B2 JP 2018075757 A JP2018075757 A JP 2018075757A JP 2018075757 A JP2018075757 A JP 2018075757A JP 6441525 B2 JP6441525 B2 JP 6441525B2
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- 239000011342 resin composition Substances 0.000 title claims description 84
- 239000000945 filler Substances 0.000 title claims description 81
- 239000000203 mixture Substances 0.000 title claims description 9
- 239000002002 slurry Substances 0.000 title claims description 8
- 239000000463 material Substances 0.000 claims description 70
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- 239000011347 resin Substances 0.000 claims description 35
- 229920005989 resin Polymers 0.000 claims description 35
- 239000012756 surface treatment agent Substances 0.000 claims description 25
- 239000013078 crystal Substances 0.000 claims description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 11
- 150000003961 organosilicon compounds Chemical class 0.000 claims description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052753 mercury Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
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- 238000004383 yellowing Methods 0.000 description 11
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229910000077 silane Inorganic materials 0.000 description 4
- -1 silane compound Chemical class 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 239000011362 coarse particle Substances 0.000 description 2
- OJLGWNFZMTVNCX-UHFFFAOYSA-N dioxido(dioxo)tungsten;zirconium(4+) Chemical compound [Zr+4].[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O OJLGWNFZMTVNCX-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000008393 encapsulating agent Substances 0.000 description 2
- 229910000174 eucryptite Inorganic materials 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 description 2
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- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 125000001951 carbamoylamino group Chemical group C(N)(=O)N* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
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- 230000001747 exhibiting effect Effects 0.000 description 1
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- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
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- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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Description
前記結晶性シリカ質粒子材料の表面と反応乃至付着した有機ケイ素化合物からなる表面処理剤と、
を有するフィラー材料であり、
前記表面処理剤の量は、前記フィラー材料が負の熱膨張係数を示す範囲である樹脂組成物に含有させて用いるものである。
本実施形態の樹脂組成物用フィラーは、銀、銅、亜鉛、水銀、錫、鉛、ビスマス、カドミウム、クロム、コバルト、及びニッケルが表面に露出しないことが好ましい。これら金属が表面に露出すると、本実施形態の樹脂組成物用フィラーを充填した樹脂組成物が液体に接触したときに不純物として溶け出すおそれがあるためである。
表1の物性の結晶性シリカ質粒子材料A〜Dに対し、表2の組成となるようにシラザン及びシランカップリング剤を添加した。その後、粉体混合用ミキサーを用いて混合した後、乾燥して表面処理を完了し本試験例1〜13の樹脂組成物用フィラーを得た。作製した各試験例の樹脂組成物用フィラーを、フィラー充填率25質量%となるように樹脂材料としての液状エポキシ樹脂(ビスフェノールA:ビスフェノールF=50:50)に混合し、混合物を25°Cで24時間保持した。保持後の樹脂の酸化度合を混合物の色相の変化で評価した。赤変したものを「不可」、黄〜赤変したが程度の軽いものを「可」、変化が見られないものを「良」とした。結果を表2に示す。
試験例2、6、7、8、及び13の樹脂組成物用フィラーについて、熱膨張係数の評価を行った。それぞれの樹脂組成物用フィラーを、SPS焼結機を用いて800°C1時間で焼結させ、熱膨張測定用の試験片を作製した。各試験片の熱膨張率を測定した。測定装置は、TMA-Q400EM(TA Instruments製)、測定温度は、-50°C〜250°Cの範囲で測定した。結果を図2〜6に示す。また、図2〜6から算出した熱膨張係数の平均値を表2に示す。
次に、試験例2、8、及び13の樹脂組成物用フィラーについて、実際に樹脂組成物を調製したときの熱膨張係数を評価した。それぞれの試験例の樹脂組成物用フィラーをフィラー充填率37.5質量%となるように、樹脂材料としての液状エポキシ樹脂(ビスフェノールA:ビスフェノールF=50:50)とアミン系硬化剤を用いて樹脂硬化物を作製し、熱膨張率測定用試験片とした。これらの各試験片の熱膨張率を測定した。結果を図7に示す。
Claims (10)
- FAU型、FER型、LTA型、MFI型、及び/又はMWW型からなる結晶構造をもつ結晶性シリカ質粒子材料と、
前記結晶性シリカ質粒子材料の表面と反応乃至付着した有機ケイ素化合物からなる表面処理剤と、
を有する樹脂組成物用フィラーであり、
前記表面処理剤の量は前記樹脂組成物用フィラーが負の熱膨張係数を示す範囲である、実装材料に用いられる樹脂組成物に含有させて用いる樹脂組成物用フィラー。 - FAU型、FER型、LTA型、MFI型、及び/又はMWW型からなる結晶構造をもつ結晶性シリカ質粒子材料と、
前記結晶性シリカ質粒子材料の表面と反応乃至付着した有機ケイ素化合物からなる表面処理剤と、
を有する樹脂組成物用フィラーであり、
前記表面処理剤の量は前記樹脂組成物用フィラーが負の熱膨張係数を示す範囲であり、
銀、銅、亜鉛、水銀、錫、鉛、ビスマス、カドミウム、クロム、コバルト、及びニッケルが表面に露出しない、
樹脂組成物に含有させて用いる樹脂組成物用フィラー。 - 前記有機ケイ素化合物は、シラザン及び/又はシランカップリング剤から選ばれる何れか1種以上である、請求項1又は2に記載の樹脂組成物用フィラー。
- 全体の質量を基準としてアルミニウム元素の含有量が12%以下である請求項1〜3の何れか1項に記載の樹脂組成物用フィラー。
- 前記結晶構造がFAU型である、請求項1〜4の何れか1項に記載の樹脂組成物用フィラー。
- 請求項1〜5の何れか1項に記載の樹脂組成物用フィラーと、前記樹脂組成物用フィラーを分散する樹脂材料と、を有する実装材料用フィラー含有樹脂組成物。
- FAU型、FER型、LTA型、MFI型、及び/又はMWW型からなる結晶構造をもつ結晶性シリカ質粒子材料と、前記結晶性シリカ質粒子材料の表面と反応乃至付着した有機ケイ素化合物からなる表面処理剤と、をもつ樹脂組成物用フィラーと、
前記樹脂組成物用フィラーを分散する溶媒と、を有するフィラー含有スラリー組成物。 - 前記有機ケイ素化合物は、シラザン及び/又はシランカップリング剤から選ばれる何れか1種以上である、請求項7に記載のフィラー含有スラリー組成物。
- 全体の質量を基準としてアルミニウム元素の含有量が12%以下である請求項7又は8に記載のフィラー含有スラリー組成物。
- 前記結晶構造がFAU型である、請求項7〜9の何れか1項に記載のフィラー含有スラリー組成物。
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JP6564517B1 (ja) * | 2018-12-17 | 2019-08-21 | 株式会社アドマテックス | 電子材料用フィラー及びその製造方法、電子材料用樹脂組成物の製造方法、高周波用基板、並びに電子材料用スラリー |
JP7351477B2 (ja) * | 2019-07-23 | 2023-09-27 | 国立大学法人東京工業大学 | 樹脂組成物およびその樹脂成形体 |
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WO2023210791A1 (ja) * | 2022-04-28 | 2023-11-02 | 三菱ケミカル株式会社 | シリカライト、組成物、液状封止剤、樹脂複合材、封止材、封止材の製造方法、及び電子デバイス |
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US11613625B2 (en) | 2017-04-10 | 2023-03-28 | Admatechs Co., Ltd. | Filler for resinous composition, filler-containing slurry composition and filler-containing resinous composition |
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