CN101296971A - 碳化硅前体及其用途 - Google Patents
碳化硅前体及其用途 Download PDFInfo
- Publication number
- CN101296971A CN101296971A CNA2006800399547A CN200680039954A CN101296971A CN 101296971 A CN101296971 A CN 101296971A CN A2006800399547 A CNA2006800399547 A CN A2006800399547A CN 200680039954 A CN200680039954 A CN 200680039954A CN 101296971 A CN101296971 A CN 101296971A
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- CN
- China
- Prior art keywords
- scope
- multipolymer
- powder
- sih
- methyl
- Prior art date
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- Pending
Links
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 79
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000002243 precursor Substances 0.000 title description 29
- 239000000203 mixture Substances 0.000 claims abstract description 90
- 238000000034 method Methods 0.000 claims abstract description 64
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 41
- 239000000463 material Substances 0.000 claims abstract description 40
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 32
- -1 methoxy, ethoxy Chemical group 0.000 claims abstract description 27
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 27
- 125000001494 2-propynyl group Chemical group [H]C#CC([H])([H])* 0.000 claims abstract description 22
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 21
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Chemical group C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 125000004106 butoxy group Chemical group [*]OC([H])([H])C([H])([H])C(C([H])([H])[H])([H])[H] 0.000 claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 65
- 239000000843 powder Substances 0.000 claims description 54
- 239000000835 fiber Substances 0.000 claims description 42
- 239000004744 fabric Substances 0.000 claims description 38
- 229910052799 carbon Inorganic materials 0.000 claims description 36
- 239000007789 gas Substances 0.000 claims description 32
- 229910002804 graphite Inorganic materials 0.000 claims description 30
- 239000010439 graphite Substances 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 27
- 239000002002 slurry Substances 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 24
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000012298 atmosphere Substances 0.000 claims description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- WHJFNYXPKGDKBB-UHFFFAOYSA-N hafnium;methane Chemical compound C.[Hf] WHJFNYXPKGDKBB-UHFFFAOYSA-N 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 238000005728 strengthening Methods 0.000 claims description 8
- 150000005846 sugar alcohols Chemical class 0.000 claims description 8
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 7
- LRTTZMZPZHBOPO-UHFFFAOYSA-N [B].[B].[Hf] Chemical compound [B].[B].[Hf] LRTTZMZPZHBOPO-UHFFFAOYSA-N 0.000 claims description 7
- 230000002902 bimodal effect Effects 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 7
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 6
- 229910007948 ZrB2 Inorganic materials 0.000 claims description 5
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 claims description 5
- 229910021397 glassy carbon Inorganic materials 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- 229910026551 ZrC Inorganic materials 0.000 claims description 3
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- 239000002006 petroleum coke Substances 0.000 claims description 2
- 239000011301 petroleum pitch Substances 0.000 claims description 2
- 239000011819 refractory material Substances 0.000 claims 2
- 238000005520 cutting process Methods 0.000 claims 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims 1
- 229920001577 copolymer Polymers 0.000 abstract description 15
- 239000000126 substance Substances 0.000 description 31
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 28
- 239000011248 coating agent Substances 0.000 description 27
- 238000000576 coating method Methods 0.000 description 27
- 229920000642 polymer Polymers 0.000 description 22
- 239000000919 ceramic Substances 0.000 description 20
- 230000008595 infiltration Effects 0.000 description 20
- 238000001764 infiltration Methods 0.000 description 20
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 18
- 239000003795 chemical substances by application Substances 0.000 description 17
- 238000005516 engineering process Methods 0.000 description 17
- 239000000758 substrate Substances 0.000 description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 15
- 238000000197 pyrolysis Methods 0.000 description 15
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 13
- 239000002585 base Substances 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 12
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000001816 cooling Methods 0.000 description 9
- 238000003747 Grignard reaction Methods 0.000 description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 229920000049 Carbon (fiber) Polymers 0.000 description 7
- 239000004917 carbon fiber Substances 0.000 description 7
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 7
- 235000012239 silicon dioxide Nutrition 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 229910010082 LiAlH Inorganic materials 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 238000006198 methoxylation reaction Methods 0.000 description 5
- RSMUVYRMZCOLBH-UHFFFAOYSA-N metsulfuron methyl Chemical compound COC(=O)C1=CC=CC=C1S(=O)(=O)NC(=O)NC1=NC(C)=NC(OC)=N1 RSMUVYRMZCOLBH-UHFFFAOYSA-N 0.000 description 5
- 239000002159 nanocrystal Substances 0.000 description 5
- 150000004767 nitrides Chemical class 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 229920003257 polycarbosilane Polymers 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 230000002829 reductive effect Effects 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 208000034189 Sclerosis Diseases 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 239000002783 friction material Substances 0.000 description 4
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000002480 mineral oil Substances 0.000 description 4
- 235000010446 mineral oil Nutrition 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 229960001866 silicon dioxide Drugs 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 238000007669 thermal treatment Methods 0.000 description 4
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical group ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 239000003365 glass fiber Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 239000000080 wetting agent Substances 0.000 description 3
- 238000010626 work up procedure Methods 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- FYTPGBJPTDQJCG-UHFFFAOYSA-N Trichloro(chloromethyl)silane Chemical compound ClC[Si](Cl)(Cl)Cl FYTPGBJPTDQJCG-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 229910052735 hafnium Inorganic materials 0.000 description 2
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 229910001092 metal group alloy Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 229910052990 silicon hydride Inorganic materials 0.000 description 2
- 229910000104 sodium hydride Inorganic materials 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 235000015096 spirit Nutrition 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000009954 braiding Methods 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
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- 239000005357 flat glass Substances 0.000 description 1
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- 238000013007 heat curing Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 238000004093 laser heating Methods 0.000 description 1
- 239000012280 lithium aluminium hydride Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000010813 municipal solid waste Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 150000002829 nitrogen Chemical class 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
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- 238000009832 plasma treatment Methods 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- 230000002265 prevention Effects 0.000 description 1
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- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000007581 slurry coating method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000012312 sodium hydride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000012720 thermal barrier coating Substances 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Classifications
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Abstract
本发明提供一种包括共聚物的硅组合物。所述共聚物具有化学式H－[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn－H，其中R1为甲基、苯基、甲氧基、乙氧基或丁氧基；其中R2为烯丙基、炔丙基或乙炔基；且其中x+y+z＝1，条件是x、y和z不是0。本发明还提供了用于利用上述共聚物来制造基于碳化硅材料的方法和由此制造的物品。
Description
技术领域
本发明涉及碳化硅前体及其使用。本发明特别涉及三组分的碳化硅前体。
背景技术
已知碳硅烷聚合物是碳化硅陶瓷的前体。在Whitmarsh等人的美国专利5,153,295中说明了碳化硅前体的实例，这里以参引式将该专利的全部内容并入本文。这些聚合物常常指陶瓷前体聚合物。Whitmarsh等人的文章中所述的聚合物的特征在于Si-C单元之间的连接都是“首尾”相连，即Si与C相连。
作为多种基底形式和材料(包括固体表面、二维或三维纤维坯料(performs)、纱线、毛毡、编织原料、管孔(tube bores)和预成型部件)的涂覆材料，碳化硅具有特殊的用途。涂覆材料可以通过各种技术涂覆到基底上，其中首先通过例如涂抹、喷涂和液体渗透等方法将碳化硅前体组合物涂覆在基底上。然后将前体组合物固化，如果需要的话，进行热分解形成碳化硅涂层。可以由低分子量的可气化前体利用化学气相渗透和化学气相沉积在单个步骤或多重渐增步骤(multiple incremental steps)中形成不同厚度的涂层。
碳化硅是公认的具有广泛应用的陶瓷材料，例如电子领域、发动机部件、低摩擦轴承、热屏障涂层和环境屏障涂层、耐磨部件(例如刹车)和其他要求高强度、热稳定性、抗氧化性和抗蚀性、和低密度的应用中。因此，需要开发可用于生产碳化硅陶瓷材料的组合物。
发明内容
本发明提供一种硅组合物，其包括具有下式的共聚物：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1为甲基、苯基、甲氧基、乙氧基或丁氧基；
其中R2为烯丙基、炔丙基或乙炔基；和
其中在x、y和z不为0的前提下x+y+z＝1。
在一个实施方式中，本发明提供了一种用于制造基于碳化硅材料的方法，所述材料包括具有下式的共聚物：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1为甲基、苯基、甲氧基、乙氧基或丁氧基；
其中R2为烯丙基、炔丙基或乙炔基；和
其中在x、y和z不为0的前提下x+y+z＝1。
在另一个实施方式中，提供了一种用于制造组合物的方法，其包括：
a)将混合物置于模具中，其中所述混合物包括至少一种粉末、至少一种强化材料、液体糖醛、催化剂和具有下式的共聚物：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1为甲基、苯基、甲氧基、乙氧基或丁氧基；
其中R2为烯丙基、炔丙基或乙炔基；和
其中x+y+z＝1，且x、y和z不是0；
b)对模具施加在约500psi和约5000psi之间范围内的压力；和
c)将模制的混合物加热到在约700℃和约1200℃之间范围内的温度。
在本发明进一步的实施方式中，提供了一种用于制造组合物的方法，其包括：
a)将强化材料和浆料加入加热炉中，其中混合物包括至少一种粉末和具有下式的共聚物：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1为甲基、苯基、甲氧基、乙氧基或丁氧基；
其中R2为烯丙基、炔丙基或乙炔基；和
其中在x、y和z不为0的前提下x+y+z＝1；
b)对加热炉施加约100毫托至约500毫托的真空；和
c)将所述强化材料和浆料加热到在约1200℃和约1800℃之间范围内的温度。
发明详述
本发明公开的碳化硅前体是三组分的共聚物。所述共聚物可以用作粘合剂或涂料以生产最终的碳化硅材料。碳化硅前体共聚物具有带可控侧基的硅-碳首尾相连的骨架结构。
本发明的碳化硅前体为具有下式的共聚物：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1每次出现时独立代表甲基、苯基、甲氧基、乙氧基或丁氧基；其中R2每次出现时独立代表烯丙基、炔丙基或乙炔基；和在x、y和z不为0的前提下x+y+z＝1。因此，该共聚物包括三种组分。在一个实施方式中，n在约10和约140之间的范围内；且在一个实施方式中，n在约20和约80之间的范围内。本发明共聚物的分子量在约500Mn和约7000Mn之间的范围内，且在一个实施方式中，在约1000Mn和约4000Mn之间的范围内。
本发明的共聚物可以通过改变硅(Si)、碳(C)、氢(H)的化学计量比而发生化学计量变化。化学计量比可以通过改变取代基、R1和R2，以及改变x、y和z的值而控制和预定。因此，可以为了所选的应用而控制和预定由共聚物前体制成的最终的碳化硅产品的性质。当硅/碳的比为约1.0时——也称为化学计量的碳化硅(SiC)，SiC陶瓷的热稳定性最高且共聚物含有的硅氢化合物的量最大。硅氢化合物与金属、氧化物和碳反应。化学计量的SiC最适于在操作温度大于约1400℃、腐蚀性环境或氧化气氛下要求稳定性的应用。相对于化学计量的SiC而言，碳比例较高的共聚物产生带有过量碳的陶瓷，因此，反应性低于化学计量的SiC，且当使用例如碳化钛、碳化铪和碳化锆等金属填料时，易于形成在2000℃以上熔化的高熔点碳化物。这些碳比例较高的共聚物还作为脱模剂和纤维涂料。Si-H含量较低的共聚物的反应性低于化学计量的聚合物，且一般用作纤维涂料、脱模剂、玻璃纤维强化复合物的低成本基体材料和碳纤维强化复合物的基体，以及低摩擦材料，例如轴承。氢含量低一般是由于与化学计量的聚合物相比，聚合物中的硅原子上带有取代基的碳的数量大。
例如，在本发明的一个实施方式中，R1为甲基，R2为烯丙基，x在约0.6和约0.9之间的范围内，y在约0.1和约0.15之间的范围内，且z在约0.05和约0.1之间的范围内。
在一个实施方式中，R1为甲基，R2为烯丙基，x在约0.6和约0.9之间的范围内，y在约0.07和约0.08之间的范围内，且z在约0.07和约0.08之间的范围内。
在一个实施方式中，R1为苯基，R2为烯丙基，x在约0.6和约0.9之间的范围内，y在约0.1和约0.3之间的范围内，且z在约0.05和约0.3之间的范围内。
在一个实施方式中，R1为甲基，R2为乙炔基，x在约0.6和约0.9之间的范围内，y在约0.1和约0.3之间的范围内，且z在约0.05和约0.3之间的范围内。
在一个实施方式中，R1为甲基，R2为炔丙基，x在约0.6和约0.9之间的范围内，y在约0.1和约0.3之间的范围内，且z在约0.05和约0.3之间的范围内。
在一个实施方式中，R1为苯基，R2为炔丙基，x在约0.6和约0.9之间的范围内，y在约0.1和约0.3之间的范围内，且z在约0.05和约0.3之间的范围内。
在一个实施方式中，R1为甲基，R2为烯丙基，x在约0.1和约0.3之间的范围内，y在约0.6和约0.8之间的范围内，且z在约0.1和约0.2之间的范围内。
在一个实施方式中，R1为甲基，R2为烯丙基，x在约0.2和约0.25之间的范围内，y在约0.1和约0.2之间的范围内，且z在约0.55和约0.7之间的范围内。
在一个实施方式中，R1为苯基，R2为炔丙基，x在约0.2和约0.25之间的范围内，y在约0.1和约0.2之间的范围内，且z在约0.55和约0.7之间的范围内。
在一个实施方式中，R1为苯基，R2为烯丙基，x在约0.1和约0.3之间的范围内，y为0.4，且z在约0.35和约0.45之间的范围内。
在一个实施方式中，R1为甲基且R2每次出现时独立代表炔丙基或乙炔基。
在一个实施方式中，R1每次出现时独立代表苯基、甲氧基、乙氧基或丁氧基，且R2为烯丙基。
本发明的共聚物是通过由甲氧基化的氯代碳硅烷的格式偶联反应，然后使用任何有效的还原剂进行还原而得到的，所述还原剂例如氢化锂铝(LiAlH4)、氢化钠铝(NaAlH4)、氢化钠(NaH)等。
本发明的共聚物可以用于形成陶瓷材料。特别是，所述共聚物形成碳化硅陶瓷材料，其中硅-碳骨架聚合物通过硅-碳侧基中的氢来交联。这里所用的“陶瓷”指高纯度陶瓷、半陶瓷材料、近似陶瓷(near-ceramic)材料、无定形陶瓷材料、纳米晶体陶瓷材料等。陶瓷可以通过各种热和放射方法形成，所述方法包括对碳化硅前体的热解、等离子处理或等离子增强处理、激光加热、电弧成型和无氧燃烧。
在一个实施方式中，本发明的共聚物用于通过热和放射方法制造高纯度碳化硅陶瓷，所述方法引起共聚物的交联和固化。这里所用的“高纯度”指带有硅-碳骨架的陶瓷，即，碳化硅，其碳杂质含量为总陶瓷材料的约0.1wt％至约4wt％，氧杂质含量为总陶瓷材料的约0.1wt％至约4wt％，且其他杂质为ppm量级。在一个实施方式中，杂质的量低于总陶瓷材料的约0.1wt％。高纯度碳化硅陶瓷的固化一般在约160℃和约500℃之间的范围内的温度发生。在一个实施方式中，固化发生在约200℃和约300℃之间的范围内的温度。共聚物一般加热约30分钟和约240分钟之间的范围内的时间。典型的没有催化剂的热固化工艺是在约350℃和约400℃之间的范围内的温度下进行1小时。
本发明的碳化硅前体还可以用于生产硬化的近似陶瓷(near-ceramic)涂层和基质。这里所用的“近似陶瓷材料”指已经固化并加热的Si-基陶瓷前驱体材料，其含有Si-H键和C-H键。共聚物是通过大致除去(即，大于约80％)Si-H键而交联，同时保持大多数C-H键不动(即，大于约90％)，产生具有独特性质的材料，例如具有有机树脂的一些韧性但是可以在大于约500℃下使用且硬度大于约1000GPA的近似陶瓷材料。在一个实施方式中，近似陶瓷材料通过将碳化硅前体加热到约400℃和约650℃之间范围内的温度而生产。在一个实施方式中，碳化硅前体被加热到约500℃和约700℃之间范围内的温度。一般，500℃时前体共聚物保留了约40％的原始氢，而在700℃仅有25％保留下来(取决于前体共聚物中Si-H与C-H的比)。在一个实施方式中，共聚物的加热速率为约0.1℃/分钟至约15℃/分钟之间，优选加热速率为约0.5℃/分钟至约3℃/分钟，且保持约5分钟至约2小时。共聚物可以在惰性环境(例如，氮气、氩气或氦气)、氢气环境或上述环境的组合条件下加热，以生产近似陶瓷材料。
本发明的近似陶瓷材料可以用于基于玻璃纤维的电路板上，所述电路板的刚性大于约30GPa且热膨胀系数接近硅(约2-3ppm/℃)。本发明的近似陶瓷材料的其他用途包括防火、耐燃的柔性面板。
在一个实施方式中，生产了无定形碳化硅基陶瓷基质和涂料。这里所用的“无定形”指玻璃样的没有可分辨的晶体结构的碳化硅材料。一般，无定形碳化硅基陶瓷材料可以通过在惰性气体、氢气或其混合气氛下于约700℃和约1200℃之间范围的温度下加热本发明的共聚物而生产，且在一个实施方式中，温度为约850℃和约900℃之间的范围内。一般，加热速率为约0.1℃/分钟和约15℃/分钟之间的范围内，优选加热速率为约0.5℃/分钟至约3℃/分钟，且温度保持约5分钟至约2小时。还可以对模具施加约500psi至约5000psi的压力。
在一个实施方式中，可以在加热后渗透共聚物。在渗透过程中，将物品从炉中除去，置于真空中，基本上除去残余的空气(存在小于约99％的空气)，并注入本发明的共聚物将热解循环中聚合物陶瓷化收缩所形成的空隙/裂纹填满。在一个实施方式中，真空的条件为压力约100至约500毫托，温度约10℃至约80℃。渗透工艺之后一般是另一个热解循环。在一个实施方式中，发生在渗透之后的热解循环是在约700℃至约1200℃的温度下进行，且在一个实施方式中，温度为约850℃至约900℃。渗透和热解可以重复一般1和16个循环。一般，循环的次数越多，物品的孔隙度越低。可以制造孔隙度为约0.5％(其可以用作制造气密或无孔物品)至约45％(其可以用于过滤)的物品。在一个实施方式中，孔隙度为约2％至约10％。
无定形的SiC基质复合物少量用于居间能量摩擦材料，例如摩托车制动回转器、汽车制动回转器、高刚性电路板、用于航天的柔性C/SiC薄型结构、工业/化学工艺材料，例如蒸馏塔填充料等。
在一个实施方式中，生产了纳米晶体SiC-基陶瓷基质和涂料。一般，纳米晶体SiC-基材料可以通过将本发明的共聚物加热到约1200℃至约1800℃的温度而制造，且在一个实施方式中，加热到约1600℃至约1800℃。一般，加热速率为约0.1℃/分钟～约15℃/分钟，且在一个实施方式中，为约0.5℃/分钟～约3℃/分钟。一般，温度保持约5分钟至约3小时，且在一个实施方式中，保持约1小时至约2小时。在一个实施方式中，加热在惰性气体、氢气或其组合下进行。一般，对炉子施加的真空压力为约100毫托至约500毫托。
在一个实施方式中，共聚物可以按照上述说明渗透。渗透工艺后一般为另一个热解循环。在一个实施方式中，发生在渗透之后的热解循环是在约850℃至约1600℃的温度下进行，且在一个实施方式中，温度为约850℃至约1000℃。渗透和热解可以重复一般1和16个循环以生产孔隙度为约0.5％(16循环)至约45％(1循环)的纳米晶体、SiC-基陶瓷材料。在一个实施方式中，孔隙度在约2％至约10％之间的范围内。
纳米晶体SiC-基基质用在要求温度大于约1400℃的应用中，例如用于飞机、重型卡车、火车等的高能制动回转器。其他用途的实例包括航天器的热保护系统(其作为返回时的“隔热层”)或火箭排气喷嘴。经常在这个实施方式中，聚合物常常被填充一种或多种耐火粉末(例如二硼化铪、碳化铪、二硼化锆、氧化锆)或耐火金属(例如铪、锆、锶、钛或钽(一般是丁氧化物(butoxides)，其是可以与形成SiC的共聚物混溶的液体)。
在热处理之前，本发明所公开的碳化硅前体共聚物为液体形式。碳化硅共聚物前体可以作为在悬浮液中承载粉末的载体，用于涂覆纤维、纤维基复合物和编织结构。碳化硅共聚物还可以用于连接、密封或涂覆多孔和/或无孔材料。当涂覆多孔材料时，共聚物可以作为光滑剂、密封剂、表面硬化剂或其任何组合。“多孔材料”包括石墨、碳/碳(C/C)复合物和氧化物基陶瓷，例如氧化铝、耐火砖、耐火粘土、窑炉隔热体(furnace insulation)等。
本发明的碳化硅共聚物前体可以用于与各种基底形式和材料结合。一般的材料包括石墨、硅、二氧化硅(石英)、氧化铝、氧化锆、各种碳化物(例如碳化硼、碳化硅、碳化钨、铬等)、和其他氧化物和氮化物陶瓷。共聚物可以用作多孔基底上的密封涂料或多孔或无孔基底上的脱模剂。碳化硅共聚物前体可以用于形成模制的化合物，其中，前体一般与粉末混合并在模具中成型或压制。另外，碳化硅前体可以用于涂覆各种金属和金属合金。这些金属和金属合金包括铜、钢、不锈钢、镍合金、钛合金、铝合金、黄铜、钼、铬钢等。
当使用共聚物作为涂料时，其可以通过各种方法涂在基底表面，所述方法例如涂抹、浸涂、喷涂和液体渗透，然后分解形成碳化硅涂层。这里所用的术语“基底”指具有一个或多个可以沉积涂料的表面的物体。所述物体包括管、块体、纤维、包括单个纤维或纤维与其他物体的组合的织物、不规则形状的物体和涂覆的表面，例如碳涂覆的纤维或其他具有碳涂层或其他组合物(例如氮化物、碳化物、硼化物等)的形状。
在一个实施方式中，共聚物可以与粉末、晶须、短切纤维、连续纤维、板层(plies)、片晶、毛布等一起使用。可以使用包括铜、铝硼硅酸盐、碳化硅(SiC)、碳、沥青基碳、石墨、氧化铝、铝硅酸盐、S-玻璃、E-玻璃(S-玻璃是具有较高热容的高强度、低碱玻璃纤维，而E-玻璃基本上是“窗玻璃”纺成的纤维)和二氧化硅以及各种纤维结构(例如毛毡、机织物(woven)、麻花状物(braided)，短切纤维、编织物(knits))。铝硅酸盐纤维的实例包括但不限于Nextel 312、Nextel312BN、Nextel 440、Nextel 550、和Nextel 720，而Nextel 610是氧化铝(氧化铝)纤维(所有“Nextel”材料都由3M Company进行商标注册)。碳化硅型纤维的实例包括但不限于商品名是例如Tyranno SA、Tyranno ZMI(都由UBE Industries注册商标)；Hi-Nicalon、Hi-Nicalon Type S(Nippon Carbon，Inc.的商标)或Sylramic(Dow Corning/ATK的商标)的物质。
在一个实施方式中，非碳纤维的纤维涂层约为0.01微米至约0.55微米厚。可以使用纤维涂料增强在大于约500℃制造或使用的碳化硅陶瓷产品的韧性，所述涂料例如高温碳、氮化硼或氮化硼/碳化硅，或聚合物衍生的SiC、SiC-C或Si-C-O。
在一个实施方式中，本发明的SiC形成的共聚物可以作为碳-纤维增强材料的基质。碳-纤维增强材料的实例包括聚丙烯腈基碳纤维布、石油沥青基纤维、短切纤维、毛毡及其组合。在此情况下，当碳纤维是石油沥青(煤焦油)基纤维且在大于约2000℃加工时，不需要纤维涂料来保护由聚合物形成的纤维。但是，可以使用具有低氢含量和较高苯取代基含量的SiC基共聚物(与化学计量的SiC相比)来改善共聚物衍生的陶瓷基质与纤维的结合，因而增强组合物的强度。
在一个实施方式中，当使用碳纤维或基于聚丙烯腈(PAN)的布时，纤维或布必须用高温碳涂覆或在真空或惰性气体中于最少1600℃下热处理最少约2小时，以便稳定纤维并使纤维可以用于形成SiC的共聚物基质。
当将粉末加入共聚物时，形成浆料。浆料一般用于形成陶瓷涂覆的织物或陶瓷复合物的纤维。一般，粉末的量为混合物总量的约1wt％～约50wt％。在一个实施方式中，粉末的量为混合物总量的约2wt％～约25wt％。在一个实施方式中，粉末的量为混合物总量的约10wt％～约65wt％。用于光滑、硬化或密封多孔材料的浆料一般含有约5vol％～约20vol％的粉末，这取决于粉末的大小和需要的涂层厚度。
粉末包括石墨、硅、二氧化硅(石英)、氧化铝、氧化锆、各种碳化物(例如碳化硼、碳化硅、碳化钨、铬等)、和其他氧化物和氮化物陶瓷。还可以使用高温耐火碳化物、硼化物、氧化物和氮化物粉末，例如二硼化铪、碳化铪、二硼化锆、氧化锆等。粉末的进一步的实例包括单独的玻璃化碳、石油焦炭、铜、铁粉、钛、锆、氧化锆、二氧化硅(石英)、硅，和铝、硅、硼、钛、钼、钨、铪、锆、铌、铬、钽的硼化物、碳化物、氮化物和氧化物，或其混合物。在一个实施方式中，粉末的大小为约0.5微米至约45微米。这里定义的细粉的粉末大小为约10纳米～约7微米，优选为约0.4微米～约4微米。在一个实施方式中，可以使用双峰(bimodal)粉末。在一个实施方式中，双峰粉末包括约4微米至约7微米的颗粒和约0.5微米至约0.8微米的颗粒。
在一个实施方式中，共聚物可以含有约0.25wt％～约5wt％硼，其加入共聚物的形式为含有硼的络合物或通过溶解少量(1-5wt％)如癸硼烷等的物质。通常，用于成型化合物的起始组合物的聚合物含量可以为约5wt％～约25wt％，优选比例为约7％～约15％。选择粉末的量以为组合物提供对于压制、挤出或其他待用成型技术合适的稠度。
在一个实施方式中，将至少一种粉末加入共聚物可以增加最终的降解前陶瓷材料可以承受的温度。在一个实施方式中，加入至少一种粉末(例如二硼化铪、碳化铪、二硼化锆、氧化锆、碳化硅或氮化硅)生产在降解之前可以承受约1600℃～约2800℃温度的最终的陶瓷材料。
在一个实施方式中，加入至少一种粉末可以用于生产低热膨胀(小于约5ppm/℃)、高模量(大于约100GPa)的陶瓷纤维、玻璃纤维、和/或碳纤维强化电路板或封装的应用。该应用的粉末的实例包括但不限于碳化硅、碳化硼或氮化硅。
在一个实施方式中，加入至少一种粉末可以用于生产化学加工元件(例如蒸馏或气体洗涤(污染控制)塔填料)用的填充和结构材料。该应用的粉末的实例包括但不限于碳化硅、碳、石墨、碳化硼或氮化硅。
铂催化剂也可以用于形成最终的碳化硅材料。铂催化剂降低了聚合物凝胶或固化的温度。一般，铂催化剂是零级催化剂。零级铂催化剂的实例包括氯铂酸、和大多数铂络合物。在一个实施方式中，所用铂催化剂的量为所用共聚物质量的约1ppm～约15ppm。在一个实施方式中，铂催化剂的量为约15ppm至约50ppm。其他可选的凝胶剂/交联剂/固化剂包括硼-氢化合物，例如癸硼烷、含硅烷醇化合物，以及多数胺化合物。在一个实施方式中，可选的固化剂的用量为所用共聚物质量的约1ppm～约15ppm。在一个实施方式中，固化剂的量为约15ppm至约50ppm。
在一个实施方式中，可以将氧引入碳化硅陶瓷组合物作为硅-氧键。氧可以通过在碳化硅共聚物前体中使用甲氧基、乙氧基或丁氧基或通过在潮湿环境中加热碳化硅共聚物前体而引入。这里所用的“潮湿环境”指在环境中的相对湿度为至少约60％，以及至少约80％。一般，环境中的温度为约90℃至约200℃，以及在一些实施方式中为约125℃至约180℃。在潮湿环境中的加热一般进行约1小时～约6小时。在一个实施方式中，在潮湿环境中约160℃下加热共聚物约1小时至约2小时。一般，加入氧产生低介电陶瓷材料。在一个实施方式中，共聚物可以用于生产低介电涂料。这里所用的“低介电”指介电常数小于约-3.0。
在一个实施方式中，可以使用进一步的添加剂生产最终的碳化硅材料。添加剂包括液体糖醛和稀释剂，例如溶剂、非极性有机液体和湿润剂。液体糖醛的量为整个混合物重量的约5wt％至约15wt％。在一个实施方式中，液体糖醛的量为整个混合物重量的约25wt％至约50wt％。液体糖醛可用于形成玻璃化碳或石墨，用于控制最终的陶瓷材料的摩擦性。还可以使用溶剂稀释共聚物。溶剂的实例包括己烷、四氢呋喃(THF)、丁醚、甲苯、丙酮、或其他非极性有机溶剂。在一个实施方式中，溶剂的量为整个混合物重量的约10wt％至约95wt％。在一个实施方式中，溶剂的量为整个混合物重量的约10wt％至约20wt％。非极性有机液体包括矿物油(mineral spirits)等。在一个实施方式中，矿物油的量为整个混合物重量的约2wt％至约15wt％。湿润剂包括例如聚乙二醇、鱼油、油酸、多油酸(polyoleic acid)、乙二醇等。在一个实施方式中，湿润剂的量为整个混合物的约0.2wt％至约2wt％。
下面的实施例将会说明本发明的各种实施方式。
具体实施方式
本发明包括一种新型陶瓷前体聚碳硅烷的制备，所述新型陶瓷前体聚碳硅烷具有H-[SiH2CH2]xn[SiMe(H)CH2]yn[SiRHCH2]zn-H的组合物，其中R为H、烯丙基、炔丙基和乙烯基基团；在x、y和z不为0的前提下x+y+z＝1。
如下列方程所示，本发明的共聚物通过4步制备：
Cl3SiCH2Cl+1.75MeOH Cl1.25(OMe)1..75SiCH2Cl (1)
nCl1.25(OMe)1..75SiCH2Cl+znR2Cl+Mg+THF→
[Si(OMe)2CH2](1-z)n[SiR2(OMe)CH2]zn (2)
[Si(OMe)2CH2](1-z)n[SiR2(OMe)CH2]zn+ynMeCl2SiCH2Cl+Mg+THF→
[Si(OMe)2CH2](1-y-z)n[SiMe(Cl)CH2]yn[SiR2(OMe)CH2]zn (3)
[Si(OMe)2CH2]xn[SiMe(Cl)CH2]yn[SiR2(OMe)CH2]zn+LiAlH4→
[SiH2CH2]xn[SiMe(H)CH2]yn[SiR2(H)CH2]zn (4)
其中x＝1-y-z或x+y+z＝1
第一步是氯代甲基三氯硅烷的部分甲氧基化。甲氧基化的比例，即MeOH/Cl3SiCH2Cl的摩尔比为1.5～2.5。最优选的比例为1.75。所得甲氧基化产物直接用于后面的格氏反应而无需纯化。然后将烯丙基氯与Cl1.25(OMe)1.75SiCH2Cl在THF中一起混合。将该混合物加入Mg粉进行格氏反应。所得甲氧基取代的聚合物[Si(OMe)2CH2](1-z)n[SiR2(OMe)CH2]zn应当还含有一些[Si(OMe)ClCH2]单元，其可以按照[Si(OMe)2CH2]单元的相同方法被还原为[SiH2CH2]结构，因此[Si(OMe)2CH2](1-z)n[SiR2(OMe)CH2]zn式中不特别包含[Si(OMe)ClCH2]单元。将烯丙基氯和Cl1.25(OMe)1.75SiCH2Cl加入混合物之后，加入THF中的MeCl2SiCH2Cl以继续格氏反应。所得混合物在50℃下搅拌24小时。通过加入LiAlH4实现还原反应。通过水检查(aqueous work-up)还原反应所得的混合物将需要的聚合物分离。
由于存在大量SiH3，市售SMP-10(AHPCS-根据Whitmarsh等人的美国专利5,153,295)的保质期限于几个月。在本发明中，通过在格氏步骤中加入MeCl2SiCH2Cl，最终的聚碳硅烷的Si-H基团将会比市售的SMP-10少，特别是SiH3端基更少，这可以实质性增加聚合物的保质期。
(1)甲氧基化
将3494.5g(19mol)氯代甲基三氯硅烷置于装有均压滴液漏斗、磁力搅拌器、和配有氮气出口的回流冷凝器的5L三口圆底烧瓶中。连接这个氮气出口的聚乙烯管置于大塑料容器中的水中以吸收副产物HCl气体。惰性气体管连在滴液漏斗的顶部对烧瓶连续通入氮气。滴加1064g(33.25mol)无水甲醇大于3h，同时磁性搅拌反应溶液。通入氮气保持反应除去副产物HCl气体，所述HCl气体被水吸收。在甲醇加入完成后，在室温下进一步搅拌溶液12h。在这个过程中得到的最初产物的组成为约70-75％Cl(MeO)2SiCH2Cl、20-25％Cl2(MeO)SiCH2Cl和0-5％(MeO)3SiCH2Cl。该混合物直接用于下一步的反应无需纯化。
(2)由Cl1.25(OMe)1.75SiCH2Cl进行格氏偶联反应
将316.8g(13.2mol)Mg粉(-50目)和400ml无水四氢呋喃(THF)置于12L三口圆底烧瓶。所述烧瓶装有滴液漏斗、机械搅拌器、和配有气体入口并供应氮气的回流冷凝器。将1585g Cl1.25(OMe)1.75SiCH2Cl(9mol)与2L无水THF和76.5g(1mol)烯丙基氯在滴液漏斗中混合。当将Cl1.25(OMe)1.75SiCH2Cl混合物加入Mg粉时，格氏反应立刻开始。溶液变暖并成为暗棕色。加入过程中，通过调节原料的加入速率并用冷水冷却反应烧瓶使反应混合物保持在温和的回流状态。在3h内加入反应原料。所得混合物在室温下搅拌30-60分钟。在这个步骤中，形成式为[Si(OMe)2CH2]0.8n[Si(烯丙基)(OMe)CH2]0.1n的聚合物。
(3)由MeCl2SiCH2Cl进行的格氏反应
将163.5g(1mol)MeCl2SiCH2Cl和600ml无水THF在与上述反应相同的滴液漏斗中混合。2小时内将所得溶液加入Cl1.25(OMe)1.75SiCH2Cl格氏反应所得的混合物中。由MeCl2SiCH2Cl开始的格氏反应与由Cl1.25(OMe)1.75SiCH2Cl开始的格氏反应非常相似。当反应溶液再次变暖时，通过冷水将其冷却。在完全加入MeCl2SiCH2Cl之后，所得混合物在室温下搅拌1h。然后将加热罩置于12L烧瓶下面，将混合物加热到50℃过夜以完成偶联反应。在这个步骤中，形成式[Si(OMe)2CH2]0.8n[SiMeClCH2]0.1n[Si(烯丙基)(OMe)CH2]0.1n的聚合物(烯丙基-甲氧基聚碳硅烷)。
(4)还原
将带有(3)得到的混合物的反应烧瓶在冰/水浴中冷却。然后加入1L无水THF和200g LiAlH4粒以还原烯丙基-甲氧基聚碳硅烷。反应溶液变暖且LiAlH4粒逐渐溶解。当溶液太粘稠不能搅拌时，再加入1L THF。还原的放热阶段约为2h。当放热阶段结束时，将12L烧瓶置于加热罩下并在强烈搅拌下将还原反应加热到50℃过夜。
(5)检查(work-up)
在30L塑料容器中将2.2L浓HCl与10kg碎冰和1.5L己烷混合。用机械搅拌器强烈搅拌溶液。在大于30分钟将由还原反应(4)得到的混合物倒入快速搅拌的冷己烷/HCl溶液中。一旦还原混合物加入完毕，将检查溶液(work-up solution)再搅拌10分钟。停止搅拌后，再水层上出现橙黄色的相。分离有机相并用500ml稀HCl溶液(1M)洗涤，然后用Na2SO4干燥12h。最后，通过旋转蒸发仪去除溶剂(己烷/THF)得到403g清澈粘稠黄色聚合物。该聚合物具有化学式[SiH2CH2]0.8n[SiMe(H)CH2]0.1n[Si(烯丙基)(H)CH2]0.1n且分子量一般分布于1000和7000之间的范围。
实施例1
用下列工艺制造电子基底用薄陶瓷复合板：
从商品名为“Nextel 312”的一卷铝硼硅酸盐纤维布上切下尺寸为12.5英寸长×12.5英寸宽的七个布层片(fabric plies)，然后将布层片涂上由本发明共聚物与32vol％细氧化铝粉末混合组成的浆料，其中R1为甲基且R2为烯丙基，x在0.8-0.9的范围内，y在0.05-0.1范围内，且z在0.05-0.1的范围内。涂覆的布层片按照0°、60°、-60°、90°、-60°、60°、0°堆叠(该角度是指经纱或原纤维束相对于垂直方向的定位，所述垂直方向定义为0度)。将布层片堆置于带有脱模片(商品名为“
”，DuPont制造)的1/4”厚的钢板中。将第二片
置于布层片堆上。将一组0.065”厚金属衬垫置于布层片堆各面的板上以控制厚度。第二钢板设在
片上盖住层片。组件置于预热到150℃的液压驱动平压机。平压机靠近衬垫且温度以2℃/分钟的速率升到400℃，并保持1小时。然后将平压机冷却并移除组件。将压制的板从组件中移除，剥去
。然后将板置于两个平滑石墨板之间，并将组件置于惰性气体炉中热解。该炉具有不锈钢整流器以看有惰性气氛并除去氧。将该炉以2℃/分钟的速率加热到250℃，1℃/分钟的速率到650℃，3℃/分钟的速率到800-900℃。然后以大于5℃/分钟的速率冷却该炉。一旦冷却，从组件中取出板并掸去过量的疏松粉末。将板置于不透液体的容器中，将容器置于真空室中真空渗透。将真空室抽真空到小于250毫托的压力并保持1/2小时。使碳化硅聚合物缓慢进入真空室并涂覆板直到完全渗透。板被液体聚合物覆盖以后，真空保持1/2小时。然后将空气通入真空室，并将板从液体聚合物中移除。将板上过量的聚合物擦去并将板置于钼片上防止与石墨板结合。将第二钼片置于板的顶部，然后是第二石墨板。将组件置于惰性气体炉并按照上述说明处理。将热解循环和真空渗透重复4-6次以上，或直到质量增益(mass gain)小于以前板质量的2％(前一热解循环后的板质量)。所得的板的纤维体积分数大于40％且厚度约为0.050-0.075英寸。
在一个实施方式中，上述实施例可以通过简单地增加涂覆布的层片的数量和保持所需厚度用的衬垫或间隔的厚度而用于生产较厚的元件(已经示范了厚达2英寸的板)。
实施例2
用以下工艺制造非常薄的高刚性复合板：
从一卷1k束T-300(聚丙烯腈-PAN基)碳纤维布上切下尺寸为12.5英寸长×12.5英寸宽的4个布层片(fabric plies)，所述碳纤维布在真空炉中1800℃下热处理了最少2小时。然后将布层片涂上由本发明共聚物与42vol％双峰(4-7微米/0.5-0.8微米)SiC粉末组成的浆料，其中R1为甲基且R2为乙炔基，x在0.70-0.80的范围内，y在0.05-0.1的范围内，且z在0.05和0.1之间的范围内。涂覆的布层片按照0°、60°、-60°、90°堆叠。将布层片堆置于涂有硫酸纸脱模片的1/2”厚的平滑石墨板上。将第二片硫酸纸置于布层片堆上。将一组0.032英寸厚金属衬垫置于布层片堆各面的板上以控制厚度。第二石墨板设在硫酸纸片上盖住层片。组件置于液压驱动惰性气体热压机中。热压机靠近衬垫且温度以1-2℃/分钟的速率在氩气下升到650-850℃，并保持1小时。然后将热压机冷却并移除组件。将压制的板从组件中移除，剥去脱模剂并掸去疏松的粉末。将板置于不透液体的容器中，将容器置于真空室中。将真空室抽真空到小于250毫托的压力并保持1/2小时。使碳化硅聚合物缓慢进入真空室并涂覆板直到完全渗透。板被液体聚合物覆盖以后，真空保持1/2小时。然后将空气通入真空室，并将板从液体聚合物中移除。将板上过量的聚合物擦去并将板置于钼片上防止与石墨板结合。将第二钼片置于板的顶部，然后是第二石墨板。将组件置于惰性气体炉并加热到650-850℃的温度(取决于纤维类型)处理。将真空渗透和热解循环重复4-6次以上，或直到增加的质量(mass gain)小于以前板质量的2％。所得的板的纤维体积分数大于40％且厚度为约0.030-0.048英寸。
在一个实施方式中，上述实施例可以通过简单地增加涂覆布的层片的数量和保持所需厚度用的衬垫或间隔的厚度而用于生产较厚的元件(已经示范了厚达2英寸的板)。在一个实施方式中，也可以使用真空热压机代替惰性气体热压机。实施例3
按照如下工艺使用本发明的共聚物制造具有高导热导电性能的低摩擦材料，其中R1为苯基，R2为烯丙基，x为0.15，y为0.45，且z为0.4：
将200g的短切铜纤维(约5mm长)与50g筛过的(200目)热解的糠醛混合。将材料干混合直到均匀分布。将25g共聚物与50g糠醛液体混合。将液体聚合物混合物加入上述粉末混合物中，充分搅拌直到均匀混合。然后将混合物压入矩形模具中，并施加1000psi的压力。然后将部件移出模具，擦去多余的树脂并将部件置于石墨板上。将部件和板置于惰性气体炉中并以0.25-0.5℃/分钟的速率在氮气下加热到850-900℃并保持1小时。然后以小于5℃/分钟的速率将该部件冷却到室温。掸去疏松粉末。将部件置于不透液体的容器中，将容器置于真空室中。将真空室抽真空到小于250毫托的压力并保持1/2小时。使共聚物缓慢进入真空室并涂覆板直到完全渗透。板被液体聚合物覆盖以后，真空保持1/2小时。然后将空气通入真空室，并将板从液体聚合物中移除。将板上过量的聚合物擦去并将板置于钼片上防止与石墨板结合。将组件置于惰性气体炉并在氩气下以1-2℃/分钟的速率加热到850-900℃并保持1小时。冷却后，掸去过量的热解聚合物，且所述部件可以用于最终的机械加工。该部件例如可以用作马达电刷、低摩擦轴承或滑动密封件。其他使用包括例如电车滑动器(troller slipper)、输电整流器、或轴衬(busing)。典型地，所述材料的摩擦系数小于约0.2，导热率为大于约100w/m-deg-K，且导电率大于约1 ohm。
在一个实施方式中，低摩擦材料是用占总混合物重量的约50％～约80％的短切铜纤维、占总混合物重量的约5％至约15％玻璃化碳粉末以及占总混合物重量的约2％至约10％的石墨粉末生产的。
实施例4
用以下工艺生产具有非常高热容的碳纤维增强材料：
使用本发明的共聚物(其中R1为甲基且R2为烯丙基，x在0.8-0.9的范围内，y在0.05-0.1的范围内，且z在0.05-0.1的范围内)、二硼化铪粉末、碳化铪粉末和SiC粉末制造浆料。浆料组合物为约60-75wt％二硼化铪粉末、约5-10wt％碳化铪粉末、约1-5wt％形成硅酸盐的材料(例如氧化锆粉末)(所有粉末的大小为0.5-4微米)，和15-25wt％本发明的共聚物，其中R1为苯基且R2为烯丙基，x在0.8-0.9的范围内，y在0.05-0.1的范围内，且z在0.05-0.1的范围内。聚合物含量按照最佳浆料的流变性质所需而调节。将3K tow Granoc CN-80平纹沥青基碳纤维的层片切成13”x13”大小。通过将每个层片穿过Teflon滚筒2次以保证均匀的负载从而用浆料将层片均匀涂覆。一旦涂覆，将12个层片使用“准各向同性”的方式堆叠，并置于涂有硫酸纸脱模板的1/2”厚的平滑石墨板上。将第二片硫酸纸置于层片堆上。将一组0.125”厚金属衬垫置于层片堆各面的板上以控制厚度。第二石墨板设在硫酸纸片上盖住层片。组件置于液压驱动惰性气体热压机中。热压机靠近衬垫且温度以1-2℃/分钟的速率在氩气下升到约850-900℃的温度，并保持约1小时。然后将热压机冷却并移除组件。将压制的板从组件中移除，剥去脱模剂并掸去疏松的粉末。将板置于不透液体的容器中，将容器置于真空室中。将真空室抽真空到小于250毫托的压力并保持1/2小时。使碳化硅聚合物缓慢进入真空室并涂覆板直到完全渗透。板被液体聚合物覆盖以后，真空保持1/2小时。然后将空气通入真空室，并将板从液体聚合物中移除。将板上过量的聚合物擦去并将板置于钼片上防止板与石墨板结合。将第二钼片置于板的顶部，然后是第二石墨板。将组件置于惰性气体炉并按照上述说明处理。将真空渗透和热解循环重复4-6次以上，或直到增加的质量(mass gain)小于以前板质量的2％。所得的板的纤维体积分数大于40％且厚度约为0.120英寸。该板可以短时间(约5-15分钟)承受高达约4500°F的温度。
实施例5
用以下工艺制造耐高温、耐化学品或耐辐射元件：
将由Cytec Corporation获得的AS-4碳纤维(PAN基碳纤维)布编织成涂覆的平碳钢芯以形成1.5”ID管。将共聚物变体(其中R1为苯基，R2为烯丙基，x在0.2-0.4的范围内，y在0.4-0.6的范围内，且z在0.1-0.2的范围内)与SiC粉末混合，使得粉末与聚合物的质量比为70％。将混合物/浆料用氧化锆研磨介质碾磨至少2小时以形成均匀的浆料。将浆料涂在所编织的管上(但其在芯上时)使管的质量增益与未涂覆的已编织材料相比为50％和100％之间。较高的质量增益提供更强更密的管。一旦涂覆，将管置于惰性气体炉中，并以1-3℃(优选2℃)/分钟的速率加热到850℃并保持1小时。然后将部件以5℃/分钟以下的速率冷却。一旦冷却，将管从芯中移开，并切成需要的长度。通过下述方式完成进一步的致密化和强化：将管浸在上述浆料中1/2小时，移开部件，并排除多余的浆料用于再利用。然后将部件置于石墨或钢盘上，并置于惰性气体炉中，并以1-3℃(优选2℃)/分钟的速率加热到850℃并保持小时。然后将部件以不超过5℃/分钟的速率冷却。如果需要，可以使用SiC浆料或纯的聚合物(neat polymer)进行进一步的循环，以生产更强、更密、更气密的元件。由上述工艺或小小改进的路线制成的部件可以用于以下方面：
1.作为装配式或再渗透化学工艺设备，例如蒸馏或洗涤塔填料或塔结构。
2.使用紧密多层编织管和至少8个用浆料或纯树脂的渗透循环生产气密热交换管。
3.使用紧密多层编织物或长丝缠绕构件中的SiC纤维和至少8个用浆料或纯树脂的渗透循环生产气密高温核燃料棒管。
4.可使用的非碳纤维，例如Nextel 312、Nextel 312BN、Nextel 440(氧化铝-二氧化硅-硼纤维)、Nextel 550、650、720-氧化铝-二氧化硅纤维和Nextel 610-氧化铝纤维(所有Nextels都是3M Company的商品名)；碳化硅纤维，例如TyrannoSA、Tyranno ZMI(都是UBE Industries的商品名)，Hi Nicalon、Hi-Nicalon TypeS(Nippon Carbon，Inc的商品名)或Sylramic(Dow Corning/ATK的商品名)。
5.可通过辊压浆料涂覆的织物和以上工艺制造管。
实施例6
组合物或陶瓷基底的表面平整和硬化通过以下工艺进行：
生产包括共聚物变型(其中R1为苯基且R2为烯丙基，x在0.3-0.5的范围内，y在0.2-0.3的范围内，且z在0.3-0.5的范围内)、己烷、矿物油(mineral spirits)和SiC粉末的浆料。所述浆料包括重量百分比为58％的SiC粉末和30％的碳化硅聚合物。将聚合物用5.6％己烷溶剂、5.6％矿物油和0.5％聚乙二醇湿润剂稀释。用氧化锆介质碾磨浆料最少2小时。一旦碾磨，将浆料涂再或旋涂再基底表面并干燥。
为了低温应用(即，小于约500℃)用两步固化工艺固化涂层按照如下工艺进行：第一步在潮湿空气中(湿度大于约70％)于约160℃～约180℃加热至少1小时。第二步在惰性气体中加热到400-500℃并保持至少1小时。
用于高温应用(即，大于约500℃)按照如下工艺进行：将涂覆的基底置于惰性气体炉中并以约0.5℃/分钟～约1℃/分钟的速率加热到约850℃并保持1小时。然后将部件以约5℃/分钟以下的速率冷却到室温。然后对所得带有纯树脂的涂层进行固化和/或热解循环，然后用于进一步硬化和光滑涂层。
上述工艺可以用于密封/降低多孔氧化铝/SiC管和坩锅的孔隙度，提供更加气密的元件和密封的/硬化的石墨和碳/碳复合材料。
实施例7
按照如下工艺制造可紫外固化、介电常数可变的表面和平整涂层：
通过旋涂或喷涂将本发明的共聚物(其中R1为甲基，R2为乙炔基，x在0.3-0.5的范围内，y在0.2-0.3的范围内，且z在0.3-0.4的范围内)涂在基底(例如陶瓷电路板或硅晶片)上。将涂层暴露在UV-B照射下通过乙炔基交联固化聚合物。或者，通过提供流动的潮湿空气(即，湿度大于约70％)并将基底加热到约160℃～约180℃将氧引入涂层以而降低介电常数。涂层可以通过在惰性气体中于约350℃～约500℃温度下加热而进一步硬化。可以使用上述工艺在电子基底上生产非常薄的(0.2-1.2微米)涂层。
实施例8
利用如下工艺制造用于摩托车、汽车和卡车的陶瓷复合物制动回转器：
从一卷1k束T-300(聚丙烯腈基)碳纤维布上切下尺寸为12.5英寸长×12.5英寸宽的12个布层片(fabric plies)，所述碳纤维布在真空炉中1800℃下热处理了最少2小时。然后将布层片涂上由本发明共聚物与42vol％双峰(4-7微米/0.5-0.8微米)SiC粉末组成的浆料，其中R1为甲基且R2为烯丙基，x在0.15-0.25的范围内，y在0.45-0.5的范围内，且z在0.3和0.5的范围内。涂覆的布层片按照0°、60°、-60°、90°堆叠。将布层片堆置于涂有硫酸纸脱模片的1/2”厚的平滑石墨板上。将第二片硫酸纸置于布层片堆上。将一组0.120英寸厚金属衬垫置于布层片堆各面的板上以控制厚度。第二石墨板设在硫酸纸片上盖住层片。组件置于液压驱动惰性气体热压机中。热压机靠近衬垫且温度以1-2℃/分钟的速率在氩气下升到650-850℃，并保持1小时。然后将热压机冷却并移除组件。将压制的板从组件中移除，剥去脱模剂并掸去疏松的粉末。将板置于不透液体的容器中，将容器置于真空室中。将真空室抽真空到小于250毫托的压力并保持1/2小时。
使第二类形成碳化硅的共聚物(形成更加化学计量的SiC，其中R1为甲基，R2为烯丙基，x在0.75-.85的范围内，y在0.05-0.1的范围内，且z在0.1-0.2的范围内)缓慢进入真空室并涂覆板直到完全渗透。板被液体聚合物覆盖以后，真空保持1/2小时。然后将氮气通入真空室将真空室加压约50psi。保持压力约2小时且真空室慢慢放气(大于1/2小时)直到达到大气压。将板从液体聚合物中移除。将板上过量的聚合物擦去并将板置于钼片上防止与石墨板结合。将第二钼片置于板的顶部，然后是第二石墨板。将组件置于惰性气体炉并加热到约850℃～约1000℃进行处理。将真空渗透、压力渗透和热解循环重复4-6次以上，或直到增加的质量(mass gain)小于以前板质量的2％。所得的板的纤维体积部分大于40％且厚度为约0.120-0.135英寸。
应当理解上述公开的各种内容、特征和功能或其可替代的方案均可以在其他不同的系统或应用中理想地组合。本领域技术人员可以随后作出各种目前难以预见的替代、改良、变型和改进，这些都应包括在本发明的权利要求范围内。
Claims (63)
1.一种硅组合物，其包括具有下式的共聚物：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1为甲基、苯基、甲氧基、乙氧基、或丁氧基；
其中R2为烯丙基、炔丙基或乙炔基；并且
其中在x、y和z不为0的前提下x+y+z＝1。
2.根据权利要求1所述的组合物，其中R1为甲基，R2为烯丙基，x在约0.6和约0.9之间的范围内，y在约0.1和约0.15之间的范围内，且z在约0.05和约0.1之间的范围内。
3.根据权利要求1所述的组合物，其中R1为甲基，R2为烯丙基，x在约0.6和约0.9之间的范围内，y在约0.07和约0.08之间的范围内，且z在约0.07和约0.08之间的范围内。
4.根据权利要求1所述的组合物，其中R1为苯基，R2为烯丙基，x在约0.6和约0.9之间的范围内，y在约0.1和约0.3之间的范围内，且z在约0.05和约0.3之间的范围内。
5.根据权利要求1所述的组合物，其中R1为甲基，R2为乙炔基，x在约0.6和约0.9之间的范围内，y在约0.1和约0.3之间的范围内，且z在约0.05和约0.3之间的范围内。
6.根据权利要求1所述的组合物，其中R1为甲基，R2为炔丙基，x在约0.6和约0.9之间的范围内，y在约0.1和约0.3之间的范围内，且z在约0.05和约0.3之间的范围内。
7.根据权利要求1所述的组合物，其中R1为苯基，R2为炔丙基，x在约0.6和约0.9之间的范围内，y在约0.1和约0.3之间的范围内，且z在约0.05和约0.3之间的范围内。
8.根据权利要求1所述的组合物，其中R1为甲基，R2为烯丙基，x在约0.1和约0.3之间的范围内，y在约0.6和约0.8之间的范围内，且z在约0.1和约0.2之间的范围内。
9.根据权利要求1所述的组合物，其中R1为甲基，R2为烯丙基，x在约0.2和约0.25之间的范围内，y在约0.1和约0.2之间的范围内，且z在约0.55和约0.7之间的范围内。
10.根据权利要求1所述的组合物，其中R1为苯基，R2为炔丙基，x在约0.2和约0.25之间的范围内，y在约0.1和约0.2之间的范围内，且z在约0.55和约0.7之间的范围内。
11.根据权利要求1所述的组合物，其中R1为苯基，R2为烯丙基，x在约0.1和约0.2之间的范围内，y在约0.40和约0.45之间的范围内，且z在约0.40和约0.45之间的范围内。
12.根据权利要求1所述的组合物，其进一步包括至少一种粉末。
13.根据权利要求12所述的组合物，其中所述粉末的大小在约0.5微米和约45微米之间的范围内。
14.根据权利要求12所述的组合物，其中所述粉末包括二硼化铪、碳化铪、二硼化锆、碳化锆、碳化硅、氮化硅、碳化硼、石墨、或其组合。
15.一种硅组合物，其包括具有下式的共聚物：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1为甲基；
其中R2为炔丙基、或乙炔基；以及
其中在x、y和z不为0的前提下x+y+z＝1。
16.一种硅组合物，其包括具有下式的共聚物：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1为苯基、甲氧基、乙氧基或丁氧基；
其中R2为烯丙基；且
其中在x、y和z不为0的前提下x+y+z＝1。
17.一种用于制造基于碳化硅的材料的方法，其包括加热具有下式的共聚物：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1为甲基、苯基、甲氧基、乙氧基或丁氧基；
其中R2为烯丙基、炔丙基或乙炔基；和
其中在x、y和z不为0的前提下x+y+z＝1。
18.根据权利要求17所述的方法，其中将所述共聚物加热到在约160℃和约500℃之间的范围内的温度。
19.根据权利要求18所述的方法，其中将所述共聚物加热一段在约30分钟和约240分钟之间范围内的时间。
20.根据权利要求17所述的方法，其中所述共聚物与基于铂的催化剂一起被加热。
21.根据权利要求17所述的方法，其中所述共聚物在至少约60％的相对湿度下加热到约90℃和约200℃之间范围内的温度达1小时到约6小时。
22.根据权利要求17所述的方法，其中R2是乙炔基团。
23.根据权利要求22所述的方法，其中通过紫外(UV)照射将所述共聚物固化。
24.根据权利要求17所述的方法，其中所述共聚物被加热到在约400℃和约650℃之间范围内的温度。
25.根据权利要求24所述的方法，其中在惰性气体、氢气或其混合气氛的环境下将所述共聚物加热。
26.根据权利要求17所述的方法，其中将所述共聚物加热到在约700℃和约1200℃之间范围内的温度。
27.根据权利要求26所述的方法，其中将所述共聚物在惰性气体、氢气或其混合气氛的环境下加热。
28.根据权利要求17所述的方法，其中将所述共聚物加热到在约1200℃和约1800℃之间范围内的温度.
29.根据权利要求28所述的方法，其中将所述共聚物在惰性气体、氢气或其混合气氛的环境下加热。
30.根据权利要求17所述的方法，其中将所述共聚物与大小在约0.5微米和约45微米之间范围内的粉末化耐火材料相混合。
31.根据权利要求30所述的方法，其中所述粉末化耐火材料为二硼化铪、碳化铪、二硼化锆、碳化锆、碳化硅、氮化硅或其组合。
32.根据权利要求17所述的方法，其中将所述共聚物与碳化硅、碳化硼、氮化硅、碳、石墨或其组合相混合。
33.根据权利要求17所述的方法，其中R1为甲基，且R2为炔丙基或乙炔基。
34.根据权利要求17所述的方法，其中R1为苯基、甲氧基、乙氧、或丁氧基；且R2为烯丙基。
35.由权利要求17所述方法制造的基于碳化硅的材料。
36.根据权利要求35所述的基于碳化硅的材料，其含有少于约0.1％的杂质。
37.根据权利要求35所述的基于碳化硅的材料，其具有基本为1∶1的硅与碳化学计量比。
38.根据权利要求35所述的基于碳化硅的材料，其具有可控的硅、碳和氢比例。
39.一种用于制造组合物的方法，其包括：
a)将混合物置于模具中，其中所述混合物包括至少一种粉末、至少一种强化材料、液体糖醛、催化剂和具有下式的共聚物：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1为甲基、苯基、甲氧基、乙氧基或丁氧基；
其中R2为烯丙基、炔丙基或乙炔基；和
其中在x、y和z不为0的前提下x+y+z＝1；
b)对模具施加在约500psi和约5000psi之间范围内的压力；和
c)将模制的混合物加热到在约700℃和约1200℃之间范围内的温度。
40.根据权利要求39所述的方法，其中所述至少一种粉末包括玻璃化碳粉末、石墨粉末、氮化硼、氮化硅、石油焦炭、铜粉、铁粉、钛粉、锆粉或其组合。
41.根据权利要求39所述的方法，其中所述至少一种强化材料为短切铜纤维。
42.根据权利要求41所述的方法，其中所述短切铜纤维在总混合物重量的约50％和约80％之间的范围内。
43.根据权利要求40所述的方法，其中所述粉末是玻璃化碳粉末，其在总混合物重量的约5％和约15％之间的范围内。
44.根据权利要求40所述的方法，其中所述粉末为石墨粉末，其在总混合物重量的约2％和约10％之间的范围内。
45.根据权利要求39所述的方法，其中所述共聚物在总混合物重量的约5％和约15％之间的范围内。
46.根据权利要求39所述的方法，其中所述液体糖醛在总混合物重量的约5％和约15％之间的范围内。
47.根据权利要求39所述的方法，其中所述加热步骤以约0.1℃/分钟和约1℃/分钟之间范围内的速率进行。
48.根据权利要求39所述的方法，其中加热步骤包括在约850℃和约900℃之间范围内的温度下保持约1小时和约8小时之间的范围内的一段时间。
49.根据权利要求39所述的方法，其进一步包括以下步骤：
d)在约10℃和约80℃之间的范围内的温度下对所述模制的混合物施加约100毫托至约500毫托的真空；
e)将共聚物加入所述模制的混合物，其中所述共聚物具有下式：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1为甲基、苯基、甲氧基、乙氧基或丁氧基；
其中R2为烯丙基、炔丙基或乙炔基；和
其中在x、y和z不为0的前提下x+y+z＝1；和
f)将所述共聚物和所述模制的混合物加热到在约700℃和约1200℃之间范围内的温度。
50.根据权利要求49所述的方法，其中加入所述共聚物的步骤进一步包括向模制混合物加入带有催化剂的液体糖醛的步骤。
51.根据权利要求50所述的方法，其中加入共聚物的所述步骤进一步包括以下条件：所述共聚物在总加入混合物重量的约50％和75％之间的范围内，以及所述液体糖醛在所述总加入混合物的重量的25％和50％之间的范围内。
52.由权利要求39所述的方法制得的物品。
53.根据权利要求52所述的物品，其摩擦系数为小于约0.2，导热性大于约100w/m-deg-K，且导电性大于约1 ohm。
54.根据权利要求52所述的物品，其中所述物品为马达电刷、电车滑动器、输电整流器、轴承或轴衬。
55.一种用于制造组合物的方法，其包括：
a)将强化材料和浆料加入加热炉中，其中所述混合物包括至少一种粉末和具有下式的共聚物：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1为甲基、苯基、甲氧基、乙氧基、或丁氧基；
其中R2为烯丙基、炔丙基或乙炔基；和
其中在x、y和z不为0的前提下x+y+z＝1；
b)对加热炉实施约100毫托至约500毫托的真空；和
c)将所述强化材料和浆料加热到在约1200℃和约1800℃之间范围内的温度。
56.根据权利要求55所述的方法，其中所述加热步骤持续一段在约1小时和约3小时之间范围内的时间。
57.根据权利要求55所述的方法，其中所述浆料包括占所述浆料重量的约10％和约65％之间范围内的双峰碳化硅粉末。
58.根据权利要求57所述的方法，其中所述双峰碳化硅粉末包括在约4微米和约7微米之间范围内的颗粒和在约0.5微米和约0.8微米之间范围内的颗粒。
59.根据权利要求55所述的方法，其中所述强化材料为基于聚丙烯腈的碳纤维布、基于石油沥青的纤维、短切纤维、毛毡或其组合。
60.根据权利要求55所述的方法，进一步包括以下步骤：
d)在约10℃和约80℃之间范围内的温度下对所述加热炉施加约100毫托至约500毫托的真空以基本除去空气；
e)将共聚物加入模制的混合物，其中所述共聚物具有下式：
H-[SiH2CH2]xn[Si(R1)HCH2]yn[SiH(R2)CH2]zn-H
其中R1为甲基、苯基、甲氧基、乙氧基或丁氧基；
其中R2为烯丙基、炔丙基或乙炔基；和
其中在x、y和z不为0的前提下x+y+z＝1；和
f)将所述共聚物和模制混合物加热到约850℃和约1000℃之间范围内的温度。
61.根据权利要求60所述的方法，其中重复步骤(d)至步骤(f)以生产开放孔隙度为约2％和约10％的物品。
62.通过权利要求55制成的物品。
63.根据权利要求62所述的物品，其中所述物品为制动回转器。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102549100A (zh) * | 2009-09-25 | 2012-07-04 | 磁性流体技术（美国）公司 | 高强度结合及涂布混合物 |
| CN101768457B (zh) * | 2010-01-28 | 2013-03-13 | 鞍钢股份有限公司 | 非煤系复合添加剂及其在炼焦中的应用 |
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| JP2019531418A (ja) * | 2016-09-28 | 2019-10-31 | フリー フォーム ファイバーズ リミテッド ライアビリティ カンパニー | 耐火性添加剤を含む多組成繊維および製造方法 |
| US10676391B2 (en) | 2017-06-26 | 2020-06-09 | Free Form Fibers, Llc | High temperature glass-ceramic matrix with embedded reinforcement fibers |
| EP3645279A4 (en) | 2017-06-27 | 2021-05-26 | Free Form Fibers, LLC | FUNCTIONAL HIGH PERFORMANCE FIBER STRUCTURE |
| KR102584736B1 (ko) | 2018-10-02 | 2023-10-05 | 로저스코포레이션 | 코팅된 질화 붕소를 포함하는 인쇄회로기판 서브스트레이트 |
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-
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- 2005-10-25 US US11/257,905 patent/US20070093587A1/en not_active Abandoned
-
2006
- 2006-10-23 EP EP06839501A patent/EP1940922A2/en not_active Withdrawn
- 2006-10-23 CA CA002626380A patent/CA2626380A1/en not_active Abandoned
- 2006-10-23 KR KR1020087011590A patent/KR20080071987A/ko not_active Application Discontinuation
- 2006-10-23 WO PCT/US2006/060148 patent/WO2007051089A2/en active Application Filing
- 2006-10-23 RU RU2008120660/04A patent/RU2008120660A/ru not_active Application Discontinuation
- 2006-10-23 CN CNA2006800399547A patent/CN101296971A/zh active Pending
- 2006-10-23 JP JP2008538138A patent/JP2009513805A/ja active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102549100A (zh) * | 2009-09-25 | 2012-07-04 | 磁性流体技术（美国）公司 | 高强度结合及涂布混合物 |
| CN101768457B (zh) * | 2010-01-28 | 2013-03-13 | 鞍钢股份有限公司 | 非煤系复合添加剂及其在炼焦中的应用 |
| CN104140537A (zh) * | 2014-07-21 | 2014-11-12 | 航天材料及工艺研究所 | 一种杂化液态前驱体、制备方法及采用该前驱体制备ZrC-SiC超高温陶瓷及其复合材料的方法 |
| CN104140537B (zh) * | 2014-07-21 | 2017-05-10 | 航天材料及工艺研究所 | 一种杂化液态前驱体、采用该前驱体制备ZrC‑SiC超高温陶瓷及其复合材料的方法 |
| CN109762351A (zh) * | 2018-12-24 | 2019-05-17 | 湖南鑫长胜材料科技有限公司 | 一种改性沥青及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| CA2626380A1 (en) | 2007-05-03 |
| RU2008120660A (ru) | 2009-12-10 |
| US20070093587A1 (en) | 2007-04-26 |
| KR20080071987A (ko) | 2008-08-05 |
| WO2007051089A2 (en) | 2007-05-03 |
| EP1940922A2 (en) | 2008-07-09 |
| JP2009513805A (ja) | 2009-04-02 |
| WO2007051089A3 (en) | 2007-11-22 |
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