JP5292815B2 - 含フッ素エラストマー組成物 - Google Patents
含フッ素エラストマー組成物 Download PDFInfo
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- JP5292815B2 JP5292815B2 JP2008000997A JP2008000997A JP5292815B2 JP 5292815 B2 JP5292815 B2 JP 5292815B2 JP 2008000997 A JP2008000997 A JP 2008000997A JP 2008000997 A JP2008000997 A JP 2008000997A JP 5292815 B2 JP5292815 B2 JP 5292815B2
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- Prior art keywords
- fluorine
- perfluoro
- mol
- containing elastomer
- vinyl ether
- Prior art date
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229920001971 elastomer Polymers 0.000 title claims abstract description 30
- 239000000806 elastomer Substances 0.000 title claims abstract description 30
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 30
- 239000011737 fluorine Substances 0.000 title claims abstract description 30
- 239000000203 mixture Substances 0.000 title claims abstract description 28
- -1 alkyl vinyl ether Chemical compound 0.000 claims abstract description 56
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 229920001577 copolymer Polymers 0.000 claims description 24
- 239000004065 semiconductor Substances 0.000 claims description 11
- 239000003566 sealing material Substances 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 125000003545 alkoxy group Chemical group 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 239000011256 inorganic filler Substances 0.000 claims description 7
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 7
- 229920001973 fluoroelastomer Polymers 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 238000004381 surface treatment Methods 0.000 claims 1
- 238000007334 copolymerization reaction Methods 0.000 abstract description 18
- 239000003795 chemical substances by application Substances 0.000 abstract description 10
- 230000004580 weight loss Effects 0.000 abstract description 3
- 229920001897 terpolymer Polymers 0.000 description 11
- 238000004073 vulcanization Methods 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 230000006835 compression Effects 0.000 description 7
- 238000007906 compression Methods 0.000 description 7
- 238000006116 polymerization reaction Methods 0.000 description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 6
- FJKIXWOMBXYWOQ-UHFFFAOYSA-N ethenoxyethane Chemical compound CCOC=C FJKIXWOMBXYWOQ-UHFFFAOYSA-N 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- BLTXWCKMNMYXEA-UHFFFAOYSA-N 1,1,2-trifluoro-2-(trifluoromethoxy)ethene Chemical compound FC(F)=C(F)OC(F)(F)F BLTXWCKMNMYXEA-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 125000004093 cyano group Chemical group *C#N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000004816 latex Substances 0.000 description 4
- 229920000126 latex Polymers 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- YPNVMKOFVMQQHI-UHFFFAOYSA-N 2-(3-ethenoxypropoxy)propanenitrile Chemical compound N#CC(C)OCCCOC=C YPNVMKOFVMQQHI-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 3
- YOALFLHFSFEMLP-UHFFFAOYSA-N azane;2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-pentadecafluorooctanoic acid Chemical compound [NH4+].[O-]C(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YOALFLHFSFEMLP-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 3
- 235000019796 monopotassium phosphate Nutrition 0.000 description 3
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000010265 sodium sulphite Nutrition 0.000 description 3
- 229920006027 ternary co-polymer Polymers 0.000 description 3
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- 229920006169 Perfluoroelastomer Polymers 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 125000000391 vinyl group Chemical class [H]C([*])=C([H])[H] 0.000 description 2
- 239000013585 weight reducing agent Substances 0.000 description 2
- KHXKESCWFMPTFT-UHFFFAOYSA-N 1,1,1,2,2,3,3-heptafluoro-3-(1,2,2-trifluoroethenoxy)propane Chemical compound FC(F)=C(F)OC(F)(F)C(F)(F)C(F)(F)F KHXKESCWFMPTFT-UHFFFAOYSA-N 0.000 description 1
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
- SUTQSIHGGHVXFK-UHFFFAOYSA-N 1,2,2-trifluoroethenylbenzene Chemical compound FC(F)=C(F)C1=CC=CC=C1 SUTQSIHGGHVXFK-UHFFFAOYSA-N 0.000 description 1
- SKYXLDSRLNRAPS-UHFFFAOYSA-N 1,2,4-trifluoro-5-methoxybenzene Chemical compound COC1=CC(F)=C(F)C=C1F SKYXLDSRLNRAPS-UHFFFAOYSA-N 0.000 description 1
- GXZPMXGRNUXGHN-UHFFFAOYSA-N 1-ethenoxy-2-methoxyethane Chemical compound COCCOC=C GXZPMXGRNUXGHN-UHFFFAOYSA-N 0.000 description 1
- QCWQPRUOTXVNSB-UHFFFAOYSA-N 2,2,3,3,4,4,5,5,6,6-decafluoro-6-(1,2,2-trifluoroethenoxy)hexanenitrile Chemical compound FC(F)=C(F)OC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C#N QCWQPRUOTXVNSB-UHFFFAOYSA-N 0.000 description 1
- ZTNPVZNUIUCIEH-UHFFFAOYSA-N 2,3,3,3-tetrafluoro-2-[1,1,2,2,3,3-hexafluoro-3-(1,2,2-trifluoroethenoxy)propoxy]propanenitrile Chemical compound FC(F)=C(F)OC(F)(F)C(F)(F)C(F)(F)OC(F)(C#N)C(F)(F)F ZTNPVZNUIUCIEH-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- SELPMKPKZDLZTE-UHFFFAOYSA-N 6-ethenoxyhexanenitrile Chemical compound C=COCCCCCC#N SELPMKPKZDLZTE-UHFFFAOYSA-N 0.000 description 1
- 229940126062 Compound A Drugs 0.000 description 1
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 1
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 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
- 125000003118 aryl group Chemical group 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 239000006172 buffering agent Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical group FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- XJRBAMWJDBPFIM-UHFFFAOYSA-N methyl vinyl ether Chemical compound COC=C XJRBAMWJDBPFIM-UHFFFAOYSA-N 0.000 description 1
- 239000012778 molding material Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K3/1006—Materials in mouldable or extrudable form for sealing or packing joints or covers characterised by the chemical nature of one of its constituents
- C09K3/1009—Fluorinated polymers, e.g. PTFE
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/18—Monomers containing fluorine
- C08F214/26—Tetrafluoroethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/18—Monomers containing fluorine
- C08F214/26—Tetrafluoroethene
- C08F214/262—Tetrafluoroethene with fluorinated vinyl ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/315—Compounds containing carbon-to-nitrogen triple bonds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Sealing Material Composition (AREA)
Description
CF2=CF〔OCF2CF(CF3)〕xO(CF2)nCN
n:1〜4
x:1〜2
で表わされるパーフルオロ不飽和ニトリル化合物0.2〜2モル%、好ましくは0.4〜1.0モル%、さらに好ましくは0.7モル%の共重合組成を有するものが知られており、この含フッ素エラストマーはビスアミノフェノールまたは芳香族テトラミンによって硬化されるとされている。
HON=C(NH2)-(CF2)n-C(NH2)=NOH
n:1〜10
で表わされるビスアミドキシム化合物を加硫剤として加硫されることが、本出願人によって提案されている。この場合に用いられる含フッ素エラストマーとしては、(A)テトラフルオロエチレン45〜75モル%、(B)パーフルオロ(低級アルキルビニルエーテル)またはパーフルオロ(低級アルコキシ低級アルキルビニルエーテル)54.8〜20モル%および(C)パーフルオロ不飽和ニトリル化合物0.2〜5モル%よりなる共重合組成を有するものが用いられるとされており、各実施例では(A):(B):(C)モル比がそれぞれ63.5:34.9:1.6または68.8:30.0:1.2の共重合組成を有するものが含フッ素エラストマーとして用いられている。
CF2=CFOCF2CF(CF3)OCnF2n+1 (n:1〜5)
CF2=CFO(CF2)3OCnF2n+1 (n:1〜5)
CF2=CFOCF2CF(CF3)O(CF2O)mCnF2n+1 (n:1〜5、m:1〜3)
CF2=CFO(CF2)2OCnF2n+1 (n:1〜5)
これらの中で、特にCnF2n+1基がCF3基であるものが好んで用いられる。
CF2=CFO(CF2)nOCF(CF3)CN (n:2〜5)
CF2=CF[OCF2CF(CF3)]nO(CF2)mCN (n:1〜2、m:1〜6)
CF2=CFO(CF2)nCN (n:1〜8)
CF2=CF[OCF2CF(CF3)]nOCF2CF(CF3)CN (n:1〜2)
CF2=CFO(CF2)n(p-C6H4)CN (n:1〜6)
HON=C(NH2)-(CF2)n-C(NH2)=NOH
n:1〜10
で表わされるビスアミドキシム化合物が加硫剤として、含フッ素エラストマー100重量部当り0.2〜5重量部、好ましくは0.5〜2重量部の割合で添加して用いられる。
内容積100Lのステンレス鋼製オートクレーブ中に、蒸留水55kg、パーフルオロオクタン酸アンモニウム1800gおよびリン酸二水素カリウム782gを仕込んだ後、オートクレーブ内を窒素で置換し、次いで減圧した。そこに、
テトラフルオロエチレン〔TFE〕 1.5kg
パーフルオロ(メチルビニルエーテル)〔FMVE〕 1.1kg
パーフルオロ(3,7-ジオキサ-8-シアノ-1-ノネン)〔CEPVE〕 130g
を順次仕込み、60℃に昇温させた後、そこに過硫酸アンモニウム70gおよび亜硫酸ナトリウム12gを溶解させた5Lの水溶液として添加し、重合反応を開始させた。
TFE 73.5モル%
FMVE 24.9モル%
CEPVE 1.6モル%
内容積100Lのステンレス鋼製オートクレーブ中に、蒸留水51kg、パーフルオロオクタン酸アンモニウム900gおよびリン酸二水素カリウム782gを仕込んだ後、オートクレーブ内を窒素で置換し、次いで減圧した。そこに、
テトラフルオロエチレン〔TFE〕 1.6kg
パーフルオロ(メチルビニルエーテル)〔FMVE〕 1.1kg
パーフルオロ(3-オキサ-8-シアノ-1-オクテン)〔CPeVE〕 100g
を順次仕込み、60℃に昇温させた後、そこに過硫酸アンモニウム70gおよび亜硫酸ナトリウム12gを溶解させた5Lの水溶液として添加し、重合反応を開始させた。
TFE 73.9モル%
FMVE 24.8モル%
CPeVE 1.3モル%
テトラフルオロエチレン-パーフルオロ(メチルビニルエーテル)-パーフルオロ(3,7-ジオキサ-8-シアノ-1-ノネン)〔モル比 TFE 73.5:FMVE 24.9:CEPVE 1.6〕3元共重合体〔共重合体A〕100重量部に、ビスアミドキシム化合物(n=4)0.7重量部を加え、2本ロールミル上で40〜45℃の温度で混練した。混練物を180℃で30分間プレス加硫(一次加硫)した後、次の条件下でのオーブン加硫(二次加硫)を窒素ガス雰囲気下で行った。
90℃で4時間
90℃から204℃迄6時間かけて昇温
204℃で18時間
204℃から288℃迄6時間かけて昇温
288℃で18時間
実施例1において、共重合体Aの代わりに、テトラフルオロエチレン-パーフルオロ(メチルビニルエーテル)-パーフルオロ(3-オキサ-8-シアノ-1-オクテン) [モル比 TFE 73.9:FMVE 24.8:CPeVE 1.3]3元共重合体(共重合体B)が用いられた。
実施例1において、共重合体Aの代わりに、テトラフルオロエチレン-パーフルオロ(エチルビニルエーテル)-パーフルオロ(3,7-ジオキサ-8-シアノ-1-ノネン) [モル比 TFE 73.2:FMVE 25.8:CEPVE 1.0]3元共重合体(共重合体C;ムーニー粘度ML1+10(121℃)84)が用いられた。
実施例1において、共重合体Aの代わりに、テトラフルオロエチレン-パーフルオロ(メトキシエチルビニルエーテル)-パーフルオロ(3,7-ジオキサ-8-シアノ-1-ノネン) [モル比 TFE 73.3:FMVE 25.1:CEPVE 1.6]3元共重合体(共重合体D;ムーニー粘度ML1+10(121℃)88)が用いられた。
常態物性:DIN53505(硬度)
DIN53503(引張試験)
圧縮永久歪:ASTM Method B;P-24 Oリングについて、300℃または315℃、70時間 の条件下で測定
プラズマ照射試験(重量減少率):アルバック社製RBH3030使用
O2プラズマ
RF出力 1500W
照射時間 6時間
真空度0.1 Torr
粘着性試験:P24 Oリングを2枚の5cm角ステンレス板(SUS板)、アルミニウム板、シ リカガラス板またはシリコン板で挟み込み、15%圧縮した状態で80℃ に15時間加熱後、30分間室温条件下に冷却したものについて、これら 2枚の板を速さ100mm/分の速度で引っ張ったときの最大荷重を測定
実施例1において、共重合体Aの代りに、共重合単量体モル比 TFE 68.5:FMVE 29.9:CEPVE 1.6の3元共重合体(共重合体E;ムーニー粘度ML1+10(121℃)82)が用いられ、同様の加硫および測定が行われた。
実施例1において、共重合体Aの代りに、共重合単量体モル比 TFE 77.5:FMVE 21.1:CEPVE 1.4の3元共重合体(共重合体F;ムーニー粘度ML1+10(121℃)91)が用いられ、同様の加硫および測定が行われた。
実施例1において、共重合体Aの代りに、共重合単量体モル比 TFE 69.9:FMVE 28.8:CEPVE 1.3の3元共重合体(共重合体G;ムーニー粘度ML1+10(121℃)85)が用いられ、同様の加硫および測定が行われた。
表
実施例 比較例
測定項目 1 2 3 4 1 2 3
硬度(ショアーA) 83 85 82 80 69 88 71
引張試験
100%モジュラス(MPa) 7.1 7.7 6.4 6.5 2.4 9.2 2.6
破断強度 (MPa) 18.3 18.5 18.7 17.2 21.8 19.3 20.8
破断時伸び (%) 200 200 210 180 240 140 240
圧縮永久歪
300℃、70hrs (%) 20 19 21 21 18 46 19
315℃、70hrs (%) 26 30 34 28 60 68 55
プラズマ試験
重量減少率 (%) 40 39 40 42 48 35 52
粘着性試験
SUS板 (N) 92 95 97 94 127 88 130
Al板 (N) 101 98 99 105 107 101 118
シリカガラス板 (N) 62 60 65 61 91 55 90
シリコン板 (N) 32 35 38 36 62 30 80
Claims (7)
- (A)テトラフルオロエチレン72.8〜74.0モル%、(B)パーフルオロ(低級アルキルビニルエーテル)またはパーフルオロ(低級アルコキシ低級アルキルビニルエーテル)26.8〜24.0モル%および(C)パーフルオロ不飽和ニトリル化合物0.2〜3.0モル%よりなる共重合組成を有する含フッ素エラストマー100重量部当り、0.2〜5重量部のビスアミドキシム化合物を配合してなり、無機充填剤を含有していない含フッ素エラストマー組成物。
- ムーニー粘度ML 1+10 (121℃)が70〜115である含フッ素エラストマーが用いられた請求項1記載の含フッ素エラストマー組成物。
- 請求項1記載の含フッ素エラストマー組成物を加硫成形して得られたシール材。
- プラズマ照射用途に用いられる請求項3記載のシール材。
- 半導体製造装置用として用いられる請求項4記載のシール材。
- シリコンウェハーの表面処理加工室用として用いられる請求項5記載のシール材。
- ゲートバルブ用途に用いられる請求項4記載のシール材。
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JP2008000997A JP5292815B2 (ja) | 2008-01-08 | 2008-01-08 | 含フッ素エラストマー組成物 |
US12/812,060 US8188176B2 (en) | 2008-01-08 | 2008-11-13 | Fluorine-containing elastomer |
EP08869702.4A EP2230263B1 (en) | 2008-01-08 | 2008-11-13 | Fluorine-containing elastomer |
PCT/JP2008/070701 WO2009087814A1 (ja) | 2008-01-08 | 2008-11-13 | 含フッ素エラストマー |
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US4525539A (en) * | 1982-12-02 | 1985-06-25 | E. I. Du Pont De Nemours And Company | Vulcanizable nitrile-containing perfluoroelastomer |
JPH0259177A (ja) | 1988-08-26 | 1990-02-28 | Babcock Hitachi Kk | 溶接ヘッド |
JP2850943B2 (ja) | 1994-10-21 | 1999-01-27 | 日本メクトロン株式会社 | ビスアミドラゾン化合物よりなる含フッ素エラストマー用加硫剤 |
JP2770769B2 (ja) * | 1995-02-16 | 1998-07-02 | 日本メクトロン株式会社 | ビスアミドキシム化合物、その製造法およびそれを含有する含フッ素エラストマー組成物 |
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JPH11303998A (ja) * | 1998-04-16 | 1999-11-02 | Kobe Steel Ltd | 高圧容器の密封装置 |
EP1683837B1 (en) * | 1998-11-13 | 2008-09-10 | Daikin Industries, Ltd. | Fluoroelastomer and crosslinkable composition thereof |
JP2000309704A (ja) * | 1999-04-23 | 2000-11-07 | Daikin Ind Ltd | 架橋性エラストマー用フィラーおよびそれを含有する架橋性エラストマー組成物 |
EP1253172B1 (en) * | 1999-11-04 | 2012-03-14 | Daikin Industries, Ltd. | Use of molded elastomer comprising crosslinkable fluoroelastomer composition for semiconductor production apparatus |
JP2002012727A (ja) * | 2000-04-25 | 2002-01-15 | Nippon Mektron Ltd | 含フッ素エラストマー組成物 |
JP2003183402A (ja) * | 2001-10-12 | 2003-07-03 | Nichias Corp | 耐プラズマ性フッ素系エラストマーシール材 |
US7678858B2 (en) * | 2003-04-22 | 2010-03-16 | Daikin Industries, Ltd. | Fluorine-containing elastomer composition excellent in plasma-aging prevention effect and shaped article made thereof |
US7659347B2 (en) * | 2004-04-28 | 2010-02-09 | Daikin Industries, Ltd. | Fluorine-containing elastomer composition and molded article comprising the same |
US7538171B2 (en) * | 2004-11-25 | 2009-05-26 | Unimatec Co., Ltd. | Fluorine-containing copolymer |
US7300985B2 (en) * | 2004-12-21 | 2007-11-27 | 3M Innovative Properties Company | Fluoropolymers having pendant amidoxime or amidrazone structures |
US7488781B2 (en) * | 2005-05-25 | 2009-02-10 | Gore Enterprise Holdings, Inc. | High purity transparent perfluoroelastomer parts and a process to produce the same |
JP4534956B2 (ja) * | 2005-11-04 | 2010-09-01 | ユニマテック株式会社 | 含フッ素エラストマー組成物 |
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EP2230263B1 (en) | 2017-05-24 |
CN101910221A (zh) | 2010-12-08 |
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US8188176B2 (en) | 2012-05-29 |
JP2009161662A (ja) | 2009-07-23 |
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