JP5183639B2 - アルミナ質繊維集合体、その製造方法及び用途 - Google Patents
アルミナ質繊維集合体、その製造方法及び用途 Download PDFInfo
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- JP5183639B2 JP5183639B2 JP2009536976A JP2009536976A JP5183639B2 JP 5183639 B2 JP5183639 B2 JP 5183639B2 JP 2009536976 A JP2009536976 A JP 2009536976A JP 2009536976 A JP2009536976 A JP 2009536976A JP 5183639 B2 JP5183639 B2 JP 5183639B2
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- 239000000835 fiber Substances 0.000 title claims description 264
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims description 86
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 229920005989 resin Polymers 0.000 claims description 34
- 239000011347 resin Substances 0.000 claims description 34
- 229920001187 thermosetting polymer Polymers 0.000 claims description 19
- 239000000945 filler Substances 0.000 claims description 15
- 238000009826 distribution Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 14
- 230000000694 effects Effects 0.000 claims description 12
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 238000001493 electron microscopy Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 description 24
- 239000000047 product Substances 0.000 description 21
- 229920000647 polyepoxide Polymers 0.000 description 19
- 239000003822 epoxy resin Substances 0.000 description 17
- 238000000034 method Methods 0.000 description 15
- 238000010298 pulverizing process Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- -1 fluororesin Polymers 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 239000006087 Silane Coupling Agent Substances 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 3
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 2
- 239000004640 Melamine resin Substances 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
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- 230000003247 decreasing effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
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- 238000010334 sieve classification Methods 0.000 description 2
- 150000004756 silanes Chemical class 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 238000001721 transfer moulding Methods 0.000 description 2
- 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 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 1
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 1
- LVNLBBGBASVLLI-UHFFFAOYSA-N 3-triethoxysilylpropylurea Chemical compound CCO[Si](OCC)(OCC)CCCNC(N)=O LVNLBBGBASVLLI-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229920000106 Liquid crystal polymer Polymers 0.000 description 1
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 description 1
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 1
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004962 Polyamide-imide Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
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- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 235000008853 Zanthoxylum piperitum Nutrition 0.000 description 1
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- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 229920000800 acrylic rubber Polymers 0.000 description 1
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- 150000004982 aromatic amines Chemical class 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229920003244 diene elastomer Polymers 0.000 description 1
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 description 1
- 239000012767 functional filler Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- KBJFYLLAMSZSOG-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)aniline Chemical compound CO[Si](OC)(OC)CCCNC1=CC=CC=C1 KBJFYLLAMSZSOG-UHFFFAOYSA-N 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- SLYCYWCVSGPDFR-UHFFFAOYSA-N octadecyltrimethoxysilane Chemical compound CCCCCCCCCCCCCCCCCC[Si](OC)(OC)OC SLYCYWCVSGPDFR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 description 1
- 238000012546 transfer Methods 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
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-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
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/041—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with metal fibres
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/62236—Fibres based on aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/6224—Fibres based on silica
- C04B35/62245—Fibres based on silica rich in aluminium oxide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/526—Fibers characterised by the length of the fibers
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5264—Fibers characterised by the diameter of the fibers
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- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
- Nonwoven Fabrics (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Description
〈試料調整〉試料台に導電性カーボンテープを貼り、その上に試料の約0.5gを分散させた後、圧縮空気を吹きかけて余分な繊維を払い落とす。
〈測定〉走査型電子顕微鏡(SEM)(例えばJEOL製「JSM−5300」)に試料をセットし、倍率100倍で写真撮影をし、任意に選ばれた繊維1000本の繊維径及び繊維長を、市販器具(例えばミツトヨ社製デジタルノギス)を用い、繊維本数の頻度分布、平均繊維径、平均繊維長を測定する。なお、繊維長は国際的な標準サンプル(日立サイエンスシステムズ社製、日立標準メゾスケールHMS-2000)で補正する。その補正方法は、まず寸法校正用パターンピッチを試料測定の条件と同一条件で観察し、任意の長さのパターンピッチを10回繰り返して測定しその平均値を算出する。この平均値と標準サンプルに明記された平均値を用い、式、校正係数=(標準サンプルの試験報告書に記載される平均値)/(10回繰り返して測定されたパターンピッチの平均値)、を用いて校正係数を算出する。この校正係数を実際に測定した繊維長に掛けることにより補正された値が得られる。
分級点の数は、分級エッジブロックの配置数によって増減させることができる。本発明においては分級点を3点以上にすることもできる。
綿状のアルミナ-シリカ繊維の市販品{Al2O3:97質量%(α-アルミナ55質量%)、SiO2:3質量%、平均繊維径:3.8μm、繊維長が100μm〜10cmの繊維の本数の含有率:50%以上)}を、内径8cm、深さ20cmの鋼製モールドに150gを投入し、プレス圧力0〜30MPaでプレス粉砕した。このプレス粉砕品は表1、表2の参考例1に示す特性を有するものであった。
綿状のアルミナ-シリカ繊維の市販品をプレス粉砕するかわりにボールミル粉砕したこと以外は、実施例1と同様にしてアルミナ質繊維集合体を製造した。すなわち、内容積60Lのボールミルに、アルミナボール20kg(直径30mmボールを5kg、直径20mmのボールを7kg、直径10mmのボールを8kg)と、実施例1と同様な綿状のアルミナ−シリカ繊維の市販品を1kg投入し、回転速度30rpmで、1分間(比較例5)、5分間(比較例6)又は7分間(比較例7)粉砕し(注:表1、2の参考例2には、この7分間粉砕品の特性が示されている。)、このボールミル粉砕品を実施例1と同様にして分級処理した。
市販のアルミナ長繊維(Al2O3:70質量%、SiO2:30質量%、平均繊維径10μm、密度2.9g/cm3)を、繊維長が100μmとなるようにチョップドした。
分級処理して得られた繊維長が50μm未満を主体とするアルミナ質繊維集合体、繊維長が50〜200μmを主体とするアルミナ質繊維集合体、繊維長が200μm超を主体とするアルミナ質繊維集合体の各質量を測定し、総質量に対する繊維長が50〜200μmを主体とするアルミナ質繊維集合体の質量百分率を求め、アルミナ質繊維集合体の収率とした。
液状エポキシ樹脂(ジャパンエポキシレジン株式会社製、商品名「エピコート807」)100gに、アルミナ質繊維集合体を、10体積%又は15体積%配合し、測定温度を30℃、せん断速度を2/sで溶液の粘度(cps (mPa・S))を測定した。なお、アルミナ質繊維集合体の密度は3.63g/cm3とし、体積への換算を行った。
以下に示す配合割合で各材料を計量し、ビニール袋中でドライブレンドした後、ロール表面温度100℃のミキシングロールを用いて5分間混練を行い、冷却粉砕した。粉砕品をトランスファー成型機(温度175℃、トランスファー出力5.1MPa、成型時間90秒)で直径28mm、厚さ3mmの円板状のエポキシ樹脂硬化体を製造し、熱伝導率測定装置(アグネ社製「ART−TC−1型」)を用い、測定環境温度23℃で温度傾斜法にて熱伝導率を測定した。
[配合割合]
アルミナ質繊維集合体 214.7g(注:エポキシ樹脂硬化体の45体積%に相当。なお、アルミナ長繊維の集合体の場合は、密度が異なるため配合量を171gに変更し、エポキシ樹脂硬化体の45体積%とした。)
アミノ系シランカップリング剤 1.2g(信越化学工業社製商品名「KBE−903」)
エポキシ樹脂 37.2g(ジャパンエポキシレジン社製商品名「YX−4000H」)
エポキシ樹脂 17.1g(日本化薬社製商品名「ECON−1020」)
硬化剤 28.3g(群栄化学工業社製商品名「PSM−4261」)
ワックス 1.9g(クラリアントジャパン社製商品名「WAX−E」)
硬化促進剤 0.7g(北興化学工業社製商品名「TPP」)
Al2O3/SiO2の質量比が50/50〜100/0の範囲の各種アルミナ−シリカ繊維を用いたこと以外は、実施例2と同様にしてアルミナ質繊維集合体を製造し評価した。それらの結果を表3に示す。なお、繊維径の頻度分布は、実施例8〜10及び比較例9のいずれも、3μm未満が1%、3〜10μmが99%であった。
なお、本出願は、2007年10月11日付けで出願された日本特許出願(特願2007−265737)に基づいており、その全体が引用により援用される。また、ここに引用されるすべての参照は全体として取り込まれる。
Claims (11)
- 電子顕微鏡法で測定された繊維本数の頻度分布において、繊維長が50〜200μmの繊維の本数が70%以上(100%を含む)であり、繊維長が50μm未満の繊維の本数が30%以下(0を含む)、50〜100μmの繊維の本数が30〜50%、100μm超〜200μmの繊維の本数が30〜50%、200μm超の繊維の本数が20%以下(0を含む)であり、しかもAl2O3を70〜100質量%、SiO2を0〜30質量%含む熱硬化性樹脂フィラー用アルミナ質繊維集合体。
- 繊維長が50〜200μmの繊維の本数が80%以上(100%を含む)であり、繊維長が50μm未満の繊維の本数が10%以下(0を含む)、50〜100μmの繊維の本数が35〜45%、100μm超〜200μmの繊維の本数が35〜45%、200μm超の繊維の本数が15%以下(0を含む)、300μm超の繊維の本数が5%以下(0を含む)であり、しかも平均繊維径が3〜10μm、繊維径が3μm未満の繊維の本数が5%未満である、請求項1記載の熱硬化性樹脂フィラー用アルミナ質繊維集合体。
- Al2O3を70〜100質量%、SiO2を0〜30質量%含む綿状のアルミナ質繊維を、0.1〜20MPaの圧力を加えて粉砕した後、分級することを特徴とする請求項1又は2記載の熱硬化性樹脂フィラー用アルミナ質繊維集合体の製造方法。
- 分級点を繊維長が50μmと200μmとして分級を行い、両者の分級点間の繊維を捕集することを特徴とする請求項3記載の熱硬化性樹脂フィラー用アルミナ質繊維集合体の製造方法。
- 分級を、コアンダ効果を利用した気流分級装置を用いて行う請求項3又は4記載の熱硬化性樹脂フィラー用アルミナ質繊維集合体の製造方法。
- コアンダ効果を利用した気流分級装置が、コアンダブロックと、前記コアンダブロックから離れる方向に順に配置された第1の分級エッジブロックと第2の分級エッジブロックとを有し、更に、前記第1の分級エッジブロックの先端には第1の分級エッジが配置され、前記第2の分級エッジブロックの先端には第2の分級エッジが配置された気流分級装置であって、
前記コアンダブロック曲面で形成される円の中心点と前記第1の分級エッジの頂点とを結ぶ直線上において、前記第1の分級エッジの頂点と前記コアンダブロック表面までの距離f1が10〜30mmであることを特徴とする請求項5記載の熱硬化性樹脂フィラー用アルミナ質繊維集合体の製造方法。 - f1が10〜15mmであることを特徴とする請求項6記載の熱硬化性樹脂フィラー用アルミナ質繊維集合体の製造方法。
- コアンダ効果を利用した気流分級装置が、コアンダブロックと、前記コアンダブロックから離れる方向に順に配置された第1の分級エッジブロックと第2の分級エッジブロックとを有し、更に、前記第1の分級エッジブロックの先端には第1の分級エッジが配置され、前記第2の分級エッジブロックの先端には第2の分級エッジが配置された気流分級装置であって、
前記コアンダブロック曲面で形成される円の中心点と前記第2の分級エッジの頂点とを結ぶ直線上において、前記第2の分級エッジの頂点と前記コアンダブロック表面までの距離f2が30〜50mmであることを特徴とする請求項5〜7の何れか一項に記載の熱硬化性樹脂フィラー用アルミナ質繊維集合体の製造方法。 - f2が30〜40mmであることを特徴とする請求項8記載の熱硬化性樹脂フィラー用アルミナ質繊維集合体の製造方法。
- コアンダ効果を利用した気流分級装置において、原料供給ノズルから噴出させる空気圧が0.2〜0.3MPaであることを特徴とする請求項5〜9の何れか一項に記載の熱硬化性樹脂フィラー用アルミナ質繊維集合体の製造方法。
- 請求項1又は2記載の熱硬化性樹脂フィラー用アルミナ質繊維集合体を含有してなる熱硬化性樹脂硬化体。
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TWI401348B (zh) | 2013-07-11 |
US8273816B2 (en) | 2012-09-25 |
JPWO2009048000A1 (ja) | 2011-02-17 |
US8383714B2 (en) | 2013-02-26 |
CA2702170A1 (en) | 2009-04-16 |
CN101821439B (zh) | 2012-02-29 |
KR101191590B1 (ko) | 2012-10-15 |
KR20100057896A (ko) | 2010-06-01 |
CA2702170C (en) | 2012-12-18 |
EP2199446A1 (en) | 2010-06-23 |
TW200932981A (en) | 2009-08-01 |
WO2009048000A1 (ja) | 2009-04-16 |
EP2199446B1 (en) | 2013-04-24 |
US20120318897A1 (en) | 2012-12-20 |
US20100207054A1 (en) | 2010-08-19 |
CN101821439A (zh) | 2010-09-01 |
EP2199446A4 (en) | 2011-10-26 |
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