DK170841B1 - Carbonfibriller, fremgangsmåde til fremstilling deraf, kompositioner indeholdende dem samt anvendelse deraf - Google Patents
Carbonfibriller, fremgangsmåde til fremstilling deraf, kompositioner indeholdende dem samt anvendelse deraf Download PDFInfo
- Publication number
- DK170841B1 DK170841B1 DK376286A DK376286A DK170841B1 DK 170841 B1 DK170841 B1 DK 170841B1 DK 376286 A DK376286 A DK 376286A DK 376286 A DK376286 A DK 376286A DK 170841 B1 DK170841 B1 DK 170841B1
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- Prior art keywords
- carbon
- approx
- fibril
- fibrils
- process according
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 83
- 239000000203 mixture Substances 0.000 title claims description 25
- 238000004519 manufacturing process Methods 0.000 title description 5
- 239000002245 particle Substances 0.000 claims abstract description 64
- 238000000034 method Methods 0.000 claims abstract description 62
- 239000003054 catalyst Substances 0.000 claims abstract description 58
- 150000001875 compounds Chemical class 0.000 claims abstract description 53
- 229910052751 metal Inorganic materials 0.000 claims abstract description 30
- 239000002184 metal Substances 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 21
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 17
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 230000005670 electromagnetic radiation Effects 0.000 claims abstract description 8
- 239000011159 matrix material Substances 0.000 claims abstract description 8
- 229920000620 organic polymer Polymers 0.000 claims abstract description 5
- 239000003990 capacitor Substances 0.000 claims abstract description 4
- 229920000592 inorganic polymer Polymers 0.000 claims abstract description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 65
- 230000008569 process Effects 0.000 claims description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 230000015572 biosynthetic process Effects 0.000 claims description 15
- 239000002243 precursor Substances 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- -1 cumole Chemical compound 0.000 claims description 9
- 150000002430 hydrocarbons Chemical class 0.000 claims description 9
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 8
- 239000004917 carbon fiber Substances 0.000 claims description 8
- 229930195733 hydrocarbon Natural products 0.000 claims description 8
- 125000003118 aryl group Chemical group 0.000 claims description 7
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 claims description 6
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 6
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 claims description 6
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims description 6
- 239000002296 pyrolytic carbon Substances 0.000 claims description 6
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 5
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 5
- 239000004215 Carbon black (E152) Substances 0.000 claims description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001294 propane Substances 0.000 claims description 3
- 230000003014 reinforcing effect Effects 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 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 claims description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 3
- 230000002787 reinforcement Effects 0.000 abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 32
- 238000006243 chemical reaction Methods 0.000 description 24
- 229910052786 argon Inorganic materials 0.000 description 16
- 239000000835 fiber Substances 0.000 description 13
- 239000000047 product Substances 0.000 description 8
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- 239000011521 glass Substances 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- RWGFKTVRMDUZSP-UHFFFAOYSA-N cumene Chemical compound CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 description 4
- 238000001493 electron microscopy Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000000635 electron micrograph Methods 0.000 description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910018404 Al2 O3 Inorganic materials 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-NJFSPNSNSA-N Carbon-14 Chemical compound [14C] OKTJSMMVPCPJKN-NJFSPNSNSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910015189 FeOx Inorganic materials 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 229920000265 Polyparaphenylene Polymers 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 241000158147 Sator Species 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
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- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 239000003733 fiber-reinforced composite Substances 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001239 high-resolution electron microscopy Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000003345 natural gas 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
- 150000002823 nitrates Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000011214 refractory ceramic Substances 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-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
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B01J35/58—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/38—Fibrous materials; Whiskers
- C04B14/386—Carbon
-
- 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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/111—Fine ceramics
- C04B35/117—Composites
-
- 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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in 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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
-
- 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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Description
DK 170841 B1
Den foreliggende opfindelse angår fremstilling af grafit-carbonfibriler med et stort overfladeareal, et højt Young's elasticitetsmodul og stor trækstyrke. Mere specifikt angår den sådanne fibriler, der er fremstillet katalytisk ud fra 5 billige, lettilgængelige carbonprecursorer uden behov for de sædvanlige og kostbare grafitiseringstemperaturer (ca.
2900°C).
Fiberarmerede kompositmaterialer bliver stadig vigtigere, fordi deres mekaniske egenskaber, især styrke, stivhed og 10 hårdhed, er bedre end egenskaberne af de enkelte bestanddele deraf eller af andre ikke-kompositmaterialer. Kompositmaterialer fremstillet af carbonfibre har udmærket styrke og stivhed pr. vægtenhed og finder derfor stor anvendelse inden for rumfarten og til sportsartikler. Deres høje pris forhindrer 15 imidlertid mere udbredt anvendelse af dem.
Carbonfibre fremstilles for tiden ved kontrolleret pyrolyse af kontinuerlige filamenter af organiske precursor-polymerer, især cellulose eller polyacrylonitril, under omhyggeligt opretholdt trækpåvirkning, hvilket er nødvendigt for at sikre 20 god orientering af de anisotrope lag af carbonatomer i de færdige filamenter. Deres høje pris er en følge af prisen på de præformede organiske fibre, vægttabet ved carboniseringen, den langsomme carboniseringshastighed i dyrt udstyr og den omhyggelige håndtering, der er nødvendig for at undgå brud i 25 de kontinuerlige filamenter.
Der er foregået en intens udvikling af metoder til spinding og carbonisering af carbonhydrid-begfibre for at reducere prisen på precursorfilamenterne og vægttabet. Hidtil har forbehandlingen af begen, spindebetingelserne og de efter-30 behandlinger, der kræves for at sikre korrekt orientering af lagene af carbonatomer i slutprodukterne, været omtrent lige så dyr som den ovenfor nævnte metode, der involverer organiske polymerer. Begge metoder kræver anvendelse af kontinuerlige filamenter for at opnå god orientering og de bedst 35 mulige egenskaber. Der er en praktisk nedre grænse for fiber- 2 DK 170841 B1 diameter, 6-8 μπι, under hvilken brud på fibrene under spindingen og efterbehandlingen bliver for omfattende.
En fuldstændig forskellig indgangsvinkel til carbonfiberdan-nelse omfatter fremstilling af carbonfilamenter ved kataly-5 tisk nedbrydning ved metaloverflader af en række carbonholdi-ge gasser, fx C0/H2, carbonhydrider og acetone. Disse filamenter findes i en lang række morfologier (fx lige, snoede, spiralformede, forgrenede) og diametre (fx fra tiere af Ångstrøm til tiere af mikrometer). Der fås sædvanligvis en 10 blanding af filamentmorfologier, der hyppigt blandes med andet, ikke-trådformet carbon (jfr. Baker og Harris, Chemistry and Physics of Carbon vol. 14, 1978). De oprindeligt dannede carbonfilamenter overtrækkes ofte med dårligt organiseret termisk carbon. Kun relativt ligekædede filamenter, der 15 har relativt store grafitområder orienteret med deres C-akser vinkelret på fiberaksen og kun har lidt eller intet termisk carbonovertræk, vil give de egenskaber af høj styrke og modulus, der kræves til armeringsanvendelser.
De fleste publikationer, der omhandler dannelse af trådformet 20 carbon, dokumenterer ikke den bestemte type filamenter, der dannes, således at det er umuligt at bestemme, om filamenterne er egnede til armeringsanvendelser. Fx beskriver Baker et al. i britisk patentskrift nr. 1.469.930 (1977), at der dannes carbonfilamenter, når en acetylen eller diolefin 25 nedbrydes over katalysatorpartikler ved 675-775°C. Der gives imidlertid ingen beskrivelse af disse filamenters struktur. I europæisk offentliggørelsesskrift nr. 56.004 (1982) beskriver Tates og Baker dannelsen af trådformet carbon over FeOx-substrater, men heller ikke her er der nogen oplysninger om 30 strukturen af de dannede carbonfilamenter. Bennett et al. beskriver i United Kingdom Atomic Energy Authority Report AERE-R7407 dannelsen af trådformet carbon ved katalytisk nedbrydning af acetone, men giver heller ikke nogen oplysninger om morfologien og dermed egnetheden til armeringsan-35 vendelser af det dannede carbon.
DK 170841 B1 3
Flere grupper af forskere har beskrevet dannelsen af lige-kædede carbonfilamenter ved katalytisk nedbrydning af carbon-hydrider. Oberlin, Endo og Koyama har beskrevet, at aromatiske carbonhydrider såsom benzen omdannes til carbonfibre med 5 metalkatalysatorpartikler ved temperaturer på ca. 1100°C (Carbon 14, 1976, s. 133). Carbonfilamenterne indeholder en velordnet grafitkerne med en omtrentlig diameter som en katalysatorpartikel, omgivet af et overtræk af mindre ordnet termisk carbon. Diameteren af de færdige filamenter ligger i 10 området 0,1-80 μπι. Forfatterne udleder, at grafitkernen vokser hurtigt og katalytisk, og at termisk carbon derefter aflej res derpå, men angiver, at de to processer ikke kan adskilles, "da de statistisk set er ledsagefænomener" (Journal of Crystal Growth 32, 1976, s. 335). De naturlige fibre, 15 der er overtrukket med termisk carbon, har lav styrke og stivhed og er ikke anvendelige som armeringsfyldstof i kom-positmaterialer. En yderligere behandling ved en høj temperatur på 2500-3000°C er nødvendig for at omdanne hele filamentet til godt ordnet grafitcarbon. Selv om denne procedure kan 20 være en forbedring af den vanskelige og kostbare pyrolyse af præformede organiske fibre under trækpåvirkning, har den den ulempe, at der kræves en totrinsproces med fibervækst og grafitbehandling ved høj temperatur. Desuden anfører forfatterne ingenting om tilsigtet katalysatorfremstilling, og 25 katalysatorpartikler synes at være tilfældigt forekommende. I nyere publikationer undersøges fremstillingen af katalysatorpartikler, men de to processer med katalytisk kernevækst og aflejring af termisk carbon er igen ikke adskilt (Extended Abstracts, 16th Biennial Conference on Carbon, 1983, s. 523).
30 Tibbetts har beskrevet dannelsen af ligekædede carbonfibre ved pyrolyse af naturgas i rør af rustfrit stål af type 304 ved temperaturer på 950-1075°C (Appl. Phys. Lett. 42(8), 1983, s. 666). Fibrene angives at vokse i to trin i lighed med det, der er beskrevet af Koyama og Endo, hvor fibrene 35 først bliver længere katalytisk og dernæst bliver tykkere ved pyrolytisk aflejring af carbon. Tibbetts anfører, at disse trin er "overlappende" og ikke kan give vækst af filamenter 4 DK 170841 B1 fri for pyrolytisk aflejret carbon. Desuden er Tibbetts' fremgangsmåde uigennemførlig i kommerciel henseende af i det mindste to grunde. For det første forekommer indledning af fibervaekst kun efter langsom carbonisering af stålrøret 5 (typisk ca. 10 timer), hvilket fører til en langsom samlet hastighed for fiberproduktion. For det andet opbruges reaktionsrøret under fiberdannelsesprocessen, hvilket gør kommerciel opskalering vanskelig og kostbar.
Det har nu overraskende vist sig, at det er muligt katalytisk 10 at omdanne carbonhydridprecursorer til carbonfilamenter, der i det væsentlige er frie for pyrolytisk aflej ret termisk carbon, hvorved man undgår det fortykningstrin, der i den kendte teknik er angivet som "overlappende" og "en ledsagende omstændighed" til det trin, hvorunder filamentet bliver 15 længere. Denne evne gør det muligt direkte at danne fibriler med høj styrke, der er nyttige til armering af matricer, til fremstilling af elektrodematerialer med et meget stort overfladeareal og til beskyttelse af genstande mod elektromagnetisk bestråling.
20 Den foreliggende opfindelse angår en i det væsentlige cylindrisk særskilt carbonfibril eller en gruppe bestående af sådanne fibriler, hvori hver fibril omfatter en indre del samt en af kullag bestående ydre del, hvilke er anbragt i det væsentlige koncentrisk omkring fibrilens cylinderakse, hvil-25 ken fibril eller gruppe af fibriller er ejendommelige ved, at hver fibril har en i det væsentlige konstant diameter samt en længde, som er større end ca. 102 gange diameteren, at hver fibril har et særskilt indre kerneområde samt et ordnet ydre område som består af flere katalytisk dannede i det væsent-30 lige kontinuerlige lag af ordnede carbonatomer, hvis ydre diameter er mellem 3,0 og 70 nm, og idet fibrilen eller fibrilerne er i det væsentlige frie for pyrolytisk aflej ret carbon.
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Fibrilens indre kerne kan være hul eller kan indeholde car-bonatoraer, som er mindre ordnede end de ordnede carbonatomer i det ydre område, som er grafitagtigt af natur.
Fibrilen eller fibrilerne ifølge den foreliggende opfindelse 5 kan fremstilles ved en fremgangsmåde, der er ejendommelig ved, at en katalysator i form af én eller flere metalholdige partikler bringes i kontakt med en precursor i form af en gas-formig, carbonholdig forbindelse ved en temperatur, der for at undgå signifikant dannelse af pyrolytisk carbon på den 10 katalytisk dannede ydre region af fibrillen er under den carbonholdige forbindelses termiske nedbrydningstemperatur, idet forholdet på tørvægtbasis mellem den carbonholdige forbindelse og den metalholdige partikel er i det mindste ca. 100:1.
15 Kontakten mellem den metalholdige partikel og den carbonholdige forbindelse kan udføres i nærværelse af en forbindelse, fx C02, H2 eller H20, som er i stand til at reagere med carbon og danne gasformige produkter.
Hensigtsmæssige carbonholdige forbindelser omfatter carbon-20 hydrider, herunder aromatiske carbonholdige forbindelser, fx benzen, toluen, xylen, cumen, ethylbenzen, naphthalen, phen-anthren, anthracen eller blandinger deraf; ikke-aromatiske carbonholdige forbindelser, fx methan, ethan, propan, ethy-len, propylen eller acetylen eller blandinger deraf; og 25 carbonholdige forbindelser indeholdende oxygen, fx formaldehyd, acetaldehyd, acetone, methanol eller ethanol eller blandinger deraf; og også carbonmonoxid.
Den hensigtsmæssige metalholdige partikel kan være en jern-, cobalt- eller nikkelholdig partikel med en diameter på mellem 30 ca. 3,5 og ca. 70 nm.
Sådanne partikler kan være anbragt på et kemisk kompatibelt, ildfast underlag, fx et underlag af aluminiumoxid, carbon eller et silikat, herunder et aluminiumsilikat.
6 DK 170841 B1 I én udførelsesform er overfladen af den metalholdige partikel opvarmet uafhængigt, fx ved elektromagnetisk bestråling, til en temperatur på ca. 850-1800°C, idet partiklens temperatur er højere end den gasformige, carbonholdige forbindelses 5 temperatur.
I en specifik udførelsesform bringes den metalholdige partikel i kontakt med den carbonholdige forbindelse i et tidsrum på fra ca. 10 sekunder til ca. 180 minutter ved et tryk på fra ca. 1/10 atmosfære til ca. 10 atmosfærer. I denne ud-10 førelsesform er den metalholdige partikel en jernholdig partikel, den gasformige carbonholdige forbindelse er benzen, reaktionstemperaturen er 900-1150°C, og forholdet mellem den carbonholdige forbindelse og den metalholdige partikel er større end ca. 1000:1. Kontakten kan udføres i nærværelse af 15 gasformig hydrogen. Desuden kan den jernholdige partikel være anbragt på et kemisk kompatibelt, ildfast underlag af fx aluminiumoxid eller carbon.
De ifølge opfindelsen fremstillede fibriler har en i det væsentlige konstant diameter. I én udførelsesform er de 20 metalholdige partikler præformede.
Fibrilerne er nyttige i kompositmaterialer med en matrix af fx en organisk polymer, en uorganisk polymer eller et metal.
I én udførelsesform inkorporeres fibrilerne i strukturmaterialer ved en armeringsmetode. I andre udførelsesformer kan 25 fibrilerne anvendes for at forbedre et materiales elektriske eller termiske ledningsevne, for at forbedre overfladearealet af en elektrode eller en elektrolytisk kondensatorplade, for at udgøre et underlag for en katalysator eller for at beskytte en genstand mod elektromagnetisk bestråling.
30 Opfindelsen beskrives nærmere under henvisning til tegningen, på hvilken fig. 1 viser en dispersion af katalysatorpartikler, der består af Fe304, DK 170841 B1 7 fig. 2 viser en dispersion af katalysatorpartikler, der består af Fe304, fig. 3 viser katalysatorpartikler indkapslet i 50-150 Å tykke carbonkapper, 5 fig. 4 viser flere fibriler med en diameter på 100-450 Å sammen med katalysatorunderlag og reaktionsrester, og fig. 5 viser en fibril med en diameter på ca. 250 Å sammen med katalysatorunderlag og reaktionsrester.
Ifølge den foreliggende opfindelse kan der fremstilles én 10 eller flere i det væsentlige cylindriske carbonfibriler, idet disse er ejendommelig ved, at hver fibril har en i det væsentlige konstant diameter samt en længde, som er større end ca. 102 gange diameteren, at hver fibril har et særskilt indre kerneområde samt et ordnet ydre område som består af 15 flere katalytisk dannede i det væsentlige kontinuerlige lag af ordnede carbonatomer, hvis ydre diameter er mellem 3,0 og 70 nm, og idet fibrilen eller fibrilerne er i det væsentlige frie for pyrolytisk aflejret carbon. I nærværende beskrivelse og krav er udtrykket "cylindrisk" anvendt i sin brede geo-20 metriske betydning, dvs. overfladen aftegnet af en lige linje, der går parallelt med en fastsat lige linje og gennemskærer en kurve. En cirkel eller en ellipse er kun to af de mange mulige kurver af cylinderen.
Det indre kerneområde af fibrilen kan være hult eller kan 25 omfatte carbonatomer, der er mindre ordnede end de ordnede carbonatomer i det ydre område. I nærværende beskrivelse og krav betegner "ordnede carbonatomer" grafitområder med deres C-akser i det væsentlige vinkelrette på fibrilens cylindriske akse.
30 I én udførelsesform er fibrilens længde større end ca. 103 gange fibrilens diameter. I en anden udførelsesform er fibrilens længde større end ca. 104 gange fibrilens diameter. I én udførelsesform er fibrilens diameter mellem ca. 7 og ca. 25 nm. I en anden udførelsesform har det indre kerneområde en 35 diameter på over ca. 2 nm.
8 DK 170841 B1
Mere specifikt omfatter en fremgangsmåde til fremstilling af én eller flere i det væsentlige cylindriske særskilte carbon-fibriler ifølge den foreliggende opfindelse, at en katalysator, dvs. én eller flere metalholdige partikler bringes i 5 kontakt med en precursor, dvs. en gasformig, carbonholdig forbindelse, ved en temperatur, der er under den carbonholdi-ge forbindelses termiske nedbrydningstemperatur, for at undgå signifikant dannelse af pyrolytisk carbon på den katalytisk dannede ydre del af fibrilen. Forholdet på tørvægtbasis 10 mellem den carbonholdige forbindelse (precursor) og den metalholdige partikel (katalysator) er i det mindste 100:1.
Det antages, at en række carbonholdige forbindelser er egnede som precursorer, når de anvendes med en hensigtsmæssig kombination af reaktionsparametre. I én udførelsesform, som er 15 eksemplificeret i nærværende beskrivelse, er precursoren benzen. Andre påtænkte egnede precursorer omfatter carbon-hydrider og carbonmonoxid. Den carbonholdige precursorfor-bindelse kan være aromatisk, fx benzen (eksemplificeret heri), toluen, xylen, cumen, ethylbenzen, naphthalen, phen-20 anthren, anthracen eller blandinger deraf. Alternativt kan den carbonoldige forbindelse være ikke-aromatisk, fx methan, ethan, propan, ethylen, propylen eller acetylen eller blandinger deraf. Den carbonholdige forbindelse kan også indeholde oxygen, fx alkoholer såsom methanol eller ethanol, ketoner 25 såsom acetone og aldehyder såsom formaldehyd eller acetal-dehyd eller blandinger deraf.
Vigtige reaktionsparametre ud over den bestemte precursor omfatter katalysatorsammensætning og -forbehandling, katalysatorunderlag, precursortemperatur, katalysatortemperatur, 30 reaktionstryk, opholdstid eller væksttid og sammensætning af tilført materiale, herunder tilstedeværelsen og koncentrationerne af eventuelle fortyndingsmidler (fx Ar) eller forbindelser, der kan reagere med carbon og danne gasformige produkter (fx C02, H2 eller H20) . Det antages, at reaktions-35 parametrene i høj grad er afhængige af hinanden, og at den DK 170841 B1 9 hensigtsmæssige kombination af reaktionsparametre vil afhænge af den specifikke carbonholdige precursorforbindelse.
Det antages endvidere, at en række overgangsmetalholdige partikler er egnede som katalysatorer, når de anvendes med en 5 hensigtsmæssig kombination af reaktionsparametre. I en for tiden foretrukken udførelsesform er den metalholdige partikel en partikel med en diameter på mellem ca. 3,5 og ca. 70 nm og indeholder jern, cobalt eller nikkel eller en legering eller blanding deraf.
10 I én udførelsesform bringes den metalholdige partikel i kontakt med den carbonholdige forbindelse i nærværelse af en forbindelse, der kan reagere med carbon og danne gasformige produkter. I én sådan udførelsesform er den forbindelse, der kan reagere med carbon, C02, H2 eller H20.
15 Det er ønskeligt, at katalysatorpartiklerne har rimeligt ensartet diameter, og at de er isolerede fra hinanden eller i det mindste holdes sammen i kun svagt forbundne aggregater. Partiklerne behøver ikke være i en aktiv form, før de indføres i reaktionsbeholderen, sålænge som de let aktiveres ved 20 en hensigtsmæssig forbehandling eller under reaktionsbetingelserne. Valget af en bestemt række forbehandlingsbetingelser afhænger af den specifikke katalysator og carbonholdige forbindelse, der anvendes, og kan også afhænge af andre reaktionsparametre som beskrevet ovenfor. Eksempler på for-25 behandlingsbetingelser er anført i nedenstående eksempler. De metalholdige partikler kan udfældes som metaloxider, -hydroxider, -carbonater, -carbonylater, -nitrater, etc. til optimal fysisk form. Velkendte kolloidteknikker til udfældning og stabilisering af ensartede, meget små partikler kan 30 anvendes. Fx er de teknikker, der er beskrevet af Spiro et al. i J. Am. Chem. Soc. 8(12), 1966, s. 2721-2726; 89(22), 1967, s. 5555-5559 og 5559-5562, til udfældning af hydrati-seret ferrioxid som let dispergerbare ensartede kugler med en diameter på nogle få nanometer, velegnede til katalysator-35 fremstilling. Disse katalysatorpartikler kan aflej res på 10 DK 170841 B1 kemisk kompatible, ildfaste underlag. Sådanne underlag skal forblive faste under reaktionsbetingelserne, må ikke forgifte katalysatoren og må være lette at adskille fra produktfibri-lerne, efter at disse er blevet dannet. Aluminiumoxid, car-5 bon, kvarts, silikater og aluminiumsilikater såsom mullit er alle egnede underlagsmaterialer. For at de let kan fjernes, er deres foretrukne fysiske form tynde film eller plader, som let kan fjernes ind i og ud af reaktionsbeholderen.
Små metalpartikler kan også dannes ved termolyse af metal-10 holdig damp i selve reaktionsbeholderen. Fx kan jernpartikler dannes ud fra ferrocendamp. Denne metode har den fordel, at fibrilvæksten indledes i hele reaktorvolumenet, hvilket giver højere produktivitet, end når katalysatorpartiklerne indføres på underlag.
15 Reaktionstemperaturen skal være tilstrækkelig høj til at få katalysatorpartiklerne til at være aktive til fibrildannelse og dog tilstrækkelig lav til at undgå betydelig termisk nedbrydning af den gasformige carbonholdige forbindelse under dannelse af pyrolytisk carbon. De præcise temperaturgrænser 20 vil afhænge af det specifikke katalysatorsystem og den specifikke gasformige carbonholdige forbindelse, der anvendes. Fx er benzen kinetisk termisk stabil op til ca. 1100°C, methan op til ca. 950°C og acetylen op til ca. 500°C. I de tilfælde, hvor termisk nedbrydning af den gasformige carbonholdige 25 forbindelse forekommer ved en temperatur tæt ved eller under den temperatur, der kræves for en aktiv fibrildannende katalysator, kan katalysatorpartiklen opvarmes selektivt til en temperatur, som er højere end temperaturen af den gasformige carbonholdige forbindelse. En sådan selektiv opvarmning kan 30 fx opnås ved elektromagnetisk bestråling.
Carbonfibrilen ifølge den foreliggende opfindelse kan fremstilles ved et hvilket som helst ønsket tryk, og det optimale tryk afhænger af økonomiske overvejelser. Reaktionstrykket er fortrinsvis mellem 1/10 og 10 atmosfærer. Reaktionstrykket er 35 mere foretrukket atmosfærisk tryk.
11 DK 170841 Bl I én eksemplificeret udførelsesform fremstilles fibrilen ved i ca. 180 minutter og ved et tryk på ca. 1 atmosfære at bringe en hensigtsmæssig jernholdig partikel i kontakt med benzen (gasformig) i en ca. 9:1 hydrogen/benzenblanding ved 5 en temperatur på ca. 900°C, idet forholdet på tørvægtbasis mellem den carbonholdige forbindelse og den jernholdige partikel er større end ca. 1000:1. I en anden eksemplificeret udførelsesform fremstilles fibrilen ved i fra ca. 1 til ca. 5 minutter og ved et tryk på ca. 1 atmosfære at bringe en hen-10 sigtsmæssig jernholdig partikel i kontakt med benzen (gasformig) i en ca. 9:1 hydrogen/benzenblanding ved en temperatur på ca. 1100°C, idet forholdet på tørvægtbasis mellem den carbonholdige forbindelse og den jernholdige partikel er større end ca. 1000:1. I en foretrukken udførelsesform for 15 denne fremgangsmåde er den jernholdige partikel anbragt på et kemisk kompatibelt, ildfast underlag som beskrevet ovenfor.
Et sådant ildfast underlag er fortrinsvis aluminiumoxid.
Fibriler, der er fremstillet ifølge den foreliggende opfindelse, er efter fremstilling i høj grad grafitagtige. De 20 enkelte grafitcarbonlag er arrangeret koncentrisk omkring fiberens længdeakse ligesom vækstringene på et træ eller ligesom en rulle sekskantet hønsenet. Der er sædvanligvis en hul kerne med en diameter på nogle få nanometer, som kan være helt eller delvis fyldt med mindre ordnet carbon. Hvert 25 carbonlag rundt om kernen kan strække sig op til så meget som flere hundrede nanometer i aksial retning. Afstanden mellem tilgrænsende lag kan bestemmes ved højopløsningselektronmikroskopi og bør kun være en smule større end den afstand, der ses i enkeltkrystalgrafit, dvs. ca. 0,339-0,348 nm.
30 Der findes ingen metoder til direkte måling af de fysiske egenskaber hos sådanne små fibriler. Imidlertid er stivheden af kompositmaterialer indeholdende fibrilerne som forventet ud fra Young's moduli, som er blevet målt på større, godt grafitiserede carboner.
12 DK 170841 B1 I et andet aspekt angår opfindelsen et kompositraateriale, som omfatter carbonfibriler som beskrevet ovenfor, herunder kompositmaterialer, der tjener som strukturmaterialer. Et sådant kompositmateriale kan også omfatte en matrix af pyro-5 lytisk eller ikke-pyrolytisk carbon eller en organisk polymer såsom fx en polyamid-, polyester-, polyether-, polyimid-, polyphenylen-, polysulfon-, polyurethan- eller epoxyharpiks. Foretrukne udførelsesformer omfatter elastomerer og termoplast iske eller termohærdede materialer.
10 I en anden udførelsesform er matricen af kompositmaterialet en uorganisk polymer, fx et keramisk materiale eller polymert råt fiberglas, pladeglas og andet formet glas, silikat-kera-mikmaterialer og andre ildfaste keramikmaterialer såsom aluminiumoxid, siliciumcarbid, siliciumnitrid og bornitrid.
15 I endnu en udførelsesform er matricen af kompositmaterialet et metal. Egnede metaller omfatter aluminium, magnesium, bly, kobber, wolfram, titan, niobium, hafnium, vanadium og legeringer og blandinger deraf.
Carbonfibrilerne er også nyttige til forskellige andre an-20 vendelser. Én udførelsesform er en metode til forøgelse af overfladearealet af en elektrode eller elektrolytisk kondensatorplade ved dertil at fastgøre én eller flere carbonfibri-ler ifølge opfindelsen. I en anden udførelsesform kan fibri-len anvendes ved en metode til at understøtte en katalysator, 25 hvilken metode omfatter, at en katalysator fastgøres til fibrilen. En sådan katalysator kan være en elektrokemisk katalysator.
Carbonfibrilerne er også nyttige ved en metode til forøgelse af et materiales elektriske ledningsevne. Ifølge denne metode 30 inkorporeres der i materialet en til forøgelse af den elektriske ledningsevne virksom mængde carbonfibriler.
En yderligere anvendelse af carbonfibrilerne er ved en metode til forøgelse af et materiales varmeledningsevne. Ved denne DK 170841 B1 13 metode inkorporeres der i materialet en til forøgelse af varmeledningsevnen virksom mængde carbonfibriler.
Endnu en anvendelse af carbonfibrilerne er ved en metode til beskyttelse af en genstand mod elektromagnetisk bestråling.
5 Ved denne metode inkorporeres der i genstanden en virksom beskyttende mængde carbonfibriler.
Opfindelsen belyses nærmere ved nedenstående eksempler 11-33. Eksemplerne 1-10 beskriver fremstillingen af katalysatorer til anvendelse i fremgangsmåden ifølge opfindelsen.
10 EKSEMPLER
Materialer Følgende materialer, der er anvendt i nedenstående eksempler, kan fås fra kommercielle kilder: Benzen (reagenskvalitet),
Fe(N03)3 · 9H20 (Baker Analyzed Crystal), FeS04-7H20 (Baker 15 Analyzed Granular), KN03 (Baker Analyzed Crystal) og NaHC03 (Baker Analyzed Crystal) kan alle fås fra J.T. Baker Chemical Company, Phillipsburg, New Jersey, USA. CO (C.P. Grade) kan fås fra Air Products and Chemicals, Inc., Allentown, Pennsylvania, USA. KOH (C.P. Pellets) kan fås fra Mallinckrodt Inc., 20 Lodi, New Jersey, USA. Det i eksemplerne anvendte vand var deioniseret. Vycor®-glasrør kan fås fra Corning Glass Works, Corning, New York, USA.
Davison® SMR-37-1534 SRA-aluminiumoxid er et or-boehmit med en gennemsnitlig krystallitstørrelse på 15 Å, en gennemsnitlig 25 agglomeratstørrelse på 0,2 μm og en gennemsnitlig partikelstørrelse på 15 μτη.
Degussa® Aluminum Oxid C er et y-aluminiumoxid med et overfladeareal på 100 m2/g, en gennemsnitlig partikelstørrelse på 200 Å og en tilsyneladende rumvægt på 60 g/1.
14 DK 170841 B1
Cabot® Sterling R V-9348 carbonpulver er en kønrøg med et minimalt carbonindhold på 99,5%, et overfladeareal på 25 m2/g, en gennemsnitlig partikelstørrelse på 750 Å og en tilsyneladende massefylde på 78,11 kg/cm2.
5 Analyser
Alle elektronmikrografer blev optaget på et Zeiss® EM-10-elektronmikroskop.
Katalysatorfremstilling EKSEMPEL 1 10 Fremstilling af katalysator 1
Der blev fremstillet en magnetitdispersion ifølge metoden beskrevet af Sugimoto og Matijevic, J. Colloid & Interfacial Sci. 74, 1980, s. 227. Elektronmikroskopi viser, at partikelstørrelsen er i området 175-400 Å, idet 260 Å er det omtrent-15 lige gennemsnit (fig. 1 og 2).
EKSEMPEL 2
Fremstilling af katalysator 2 I en 118,3 cm3 bredhalset glaskrukke med en magnetomrører blev der anbragt 10 g Davison® SMR-37-1534 SRA-aluminiumoxid-20 pulver. Til det omrørte pulver blev der dråbevis sat 0,81 M Fe(N03)3 i H20 til punktet for begyndende våd tilstand. Der krævedes 4,1 ml.
EKSEMPEL 3
Fremstilling af katalysator 3 25 En portion af det ifølge eksempel 2 vundne våde pulver blev opvarmet i krukken under omrøring på en varm plade, indtil DK 170841 B1 15 det var tørt. Temperaturen blev holdt under det punkt, ved hvilket der blev udviklet N0X.
EKSEMPEL 4
Fremstilling af katalysator 4 5 En portion Davison® SMR-37-1534 SRA-aluminiumoxidpulver blev calcineret i en luftstrøm ved 900°C i 90 minutter i et Vycor®-rør. I en 118,3 cm3 bredhalset krukke med magnetom-rører blev der anbragt 1,9977 g af det calcinerede A1203. Medens det blev omrørt, blev der dråbevis tilsat 0,81 M 10 Fe (N03) 3-opløsning i H20 indtil begyndende våd tilstand. Der krævedes 0,6 ml. Det våde pulver blev tørret under omrøring på en varm plade.
EKSEMPEL 5
Fremstilling af katalysator 5 15 I et 10,16 cm serumpolymerisationsrør forsynet med hætte blev der vejet 0,44 g Degussa® Aluminum Oxid C (fumed Al203).
Røret blev lukket med hætte og skyllet med argon, hvorefter der blev injiceret 1 ml 0,5 M KOH, 1 ml 2,0 M KN03 og 6 ml forfiltreret deioniseret vand. Blandingen blev skyllet med 20 argon i 5 minutter, og derefter blev der injiceret 2,0 ml 0,101 M FeS04. Blandingen blev skyllet med argon i 1 minut. Røret blev anbragt i et 90°C varmt oliebad, og argonskylningen fortsattes i 5 minutter. Skylningen blev standset, og rolig nedbrydning begyndte. (Oliebadets temperaturregulering 25 var mangelfuld, og temperaturen steg til 105°C. Badet blev afkølet tilbage til 90°C.) Den samlede nedbrydningstid var 2 timer.
Efter henstand skilte systemet i et hvidt bundfald og en klar supernatant. Det blev centrifugeret, supernatanten blev 30 dekanteret, og bundfaldet blev resuspenderet i forfiltreret, deioniseret vand. Dette blev gentaget yderligere to gange.
16 DK 170841 B1
Den endelige supernatants pH-værdi var ca. 8,5. Vandet blev dekanteret, og bundfaldet blev blæst halvtørt med argon og resuspenderet i ethanol.
EKSEMPEL 6 5 Fremstilling af katalysator 6
En portion Davison® SMR-37-1534 SRA-aluminiumoxidpulver blev calcineret i 2 timer i en luftstrøm ved 900°C i et VycorArør.
1 g af produktet blev anbragt i et 10,16 cm polymerisations-rør forsynet med hætte, og der blev tilsat tilstrækkelig 1,6 10 M Fe (N03) 3-opløsning til fuldstændigt at dække aluminiumoxid-et. Røret blev lukket med hætte og evakueret, indtil bob-1ingen ophørte. Røret blev åbnet, og den overskydende væske blev frafiltreret gennem et filter med M-glasfritte. Den fugtige kage blev calcineret i en keramikskål i 1 time i en 15 luftstrøm ved 500°C.
EKSEMPEL 7
Fremstilling af katalysator 7 I en centrifugeflaske blev 6,06 g Fe (N03) 3 9H20 opløst i 50 ml forfiltreret deioniseret H20. Til opløsningen blev der sat 20 2,52 g NaHC03. Når skumningen ophørte, blev opløsningen skyllet med argon i 5 minutter. Produktet Fe203-solen var en klar opløsning.
En portion Cabot® Sterling R V-9348 carbonpulver blev calcineret i en argonstrøm i en Vycor®-skål i et mullitrør ved 25 1100°C i 1 time. Det blev afkølet til stuetemperatur under argon. I et 10,16 cm polymerisationsrør blev der anbragt tilstrækkeligt carbon til at udgøre et lag på 0,64 cm. Røret blev evakueret, og der blev tilsat 2 ml Fe203-opløsning. Når boblingen ophørte, blev røret åbnet, og suspensionen blev 30 filtreret på en tragt med M-glasfritte. Kagen blev lufttørret DK 170841 B1 17 og opvarmet i 1 time ved 500°C under en argonstrøm i et Vycor®-rør. EKSEMPEL 8
Fremstilling af katalysator 8 I et 10,16 cm polymerisationsrør blev en portion på 0,4876 g 5 calcineret Cabot® Sterling R V-9348 carbonpulver evakueret, og der blev tilsat 2,0 ml 0,81 M Fe (N03) 3-opløsning. Når bob-lingen ophørte, blev røret åbnet, og kagen blev lufttørret.
EKSEMPEL 9
Fremstilling af katalysator 9 10 Der blev fremstillet en pellet ved at komprimere Cabot®
Sterling R V-9348 pulver i et presseværktøj af rustfrit stål (til fremstilling af KBR-skiver til infrarød). 0,12 g af pelleten blev evakueret i et 10,16 cm polymerisationsrør, og der blev tilsat 0,05 ml frisk fremstillet Fe203-sol (frem-15 stillet som beskrevet i eksempel 7). Røret blev åbnet, og det faste stof blev lufttørret.
EKSEMPEL 10
Fremstilling af katalysator 10 1 et 10,16 cm polymerisationsrør blev 0,23 g Davison® SMR-37- 20 1534 SRA-aluminiumoxid evakueret, som var blevet calcineret i 2 timer ved 900°C i luft, og der blev tilsat 2,0 ml frisk fremstillet Fe203-sol (fremstillet som beskrevet i eksempel 7). Røret blev åbnet, og det faste stof blev filtreret ud på et filter med M-glasfritte. Kagen blev lufttørret.
18 DK 170841 B1
Fibri1 syn tesekørsi er EKSEMPEL 11-23
Eksempel 11-23 beskriver fibrilsyntesekørsler. Forsøgsbetingelserne og -resultaterne er vist i tabel 1. Medmindre 5 andet er angivet, var fibrilprecursoren benzen som en ca. 9:1 hydrogen/benzenblanding, og gasstrømningshastighederne var 300 ml/minut for H2 og Ar; 300 ml/minut CO og 100 ml/minut for CO/H2; 300 ml/minut Ar eller H2 gennem benzen ved 20°C for Ar/C6H6 eller H2/C6H6 (ca. 9:1 volumenforhold Ar eller 10 H2/C6H6) . Luft og hydrogen var hele tiden adskilt ved en kort argonskylning af reaktionsbeholderen. Forsøgsprotokollerne var ens i hver kørsel og er beskrevet i detaljer for eksempel 11, 15 og 28.
a) EKSEMPEL 11 15 En katalysator, der var fremstillet ifølge den i eksempel 1 beskrevne fremgangsmåde, blev ultrasonisk dispergeret i vand og overført til en keramikskål. Skålen blev anbragt i centrum af et 2,54 cm's Vycor®-rør i en elektrisk ovn ved stuetemperatur. Katalysatoren blev bragt fra stuetemperatur til 20 500°C i løbet af 15 minutter under en strøm af argon. Ved denne temperatur ændredes gasblandingen til en 9:1 hydrogen/benzenblanding. Denne komposition blev ledt ind i reaktionsbeholderen i 60 minutter.
Carbonhydridstrømmen blev standset og erstattet med argon, og 25 reaktionsbeholderen blev afkølet til stuetemperatur. Skålen blev fjernet fra røret, og en mængde carbon blev skrabet af den. Dette carbon blev ultrasonisk dispergeret i ethanol, og en 10 mikroliters prøve blev undersøgt ved elektronmikroskopi. Mikrograferne viste, at de fleste af jernpartiklerne var 30 indkapslede i 50-150 Å tykke carbonkapper (fig. 3).
DK 170841 B1 19 b) EKSEMPEL 15
En katalysator, der var fremstillet som beskrevet i eksempel 2, blev dispergeret i en keramikskål. Skålen blev anbragt i et 2,54 cm's Vycor®-rør i den samme elektriske ovn, som blev 5 anvendt i eksempel 11.
Ovnens temperatur blev hævet fra stuetemperatur til 500°C og holdt på 500°C i 60 minutter under luft. Reaktionsbeholderen blev kort skyllet med argon. Temperaturen blev derefter øget fra 500°C til 900°C i løbet af 15 minutter under hydrogen og 10 holdt på 900°C i 60 minutter under samme hydrogenstrøm.
Gasstrømmen blev derefter ændret til benzen-mættet hydrogen i 180 minutter ved 900°C. Efter afkøling til stuetemperatur under argon blev der fremstillet en prøve ifølge den i eksempel 11 beskrevne fremgangsmåde, og prøven blev undersøgt 15 ved elektronmikroskopi. Elektronmikrograferne viste flere fibriler med en diameter på 100-450 Å (fig. 4).
C) EKSEMPEL 28
En katalysator, der var fremstillet som beskrevet i eksempel 3, blev dispergeret i en keramikskål. Skålen blev anbragt i 20 et 2,54 cm's mullitrør i den samme elektriske ovn, som blev anvendt i eksempel 11.
Ovnens temperatur blev hævet fra stuetemperatur til 500°C i løbet af 15 minutter og blev holdt på 500°C i 60 minutter under luft. Reaktionsbeholderen blev kort skyllet med argon.
25 Temperaturen blev derefter øget fra 500°C til 900°C i løbet af 20 minutter under hydrogen og holdt på 900°C i 60 minutter under samme hydrogenstrøm. Temperaturen blev derefter hævet yderligere til 1100°C i løbet af 20 minutter, idet den samme hydrogenstrøm blev opretholdt.
30 Gasstrømmen blev derefter ændret til benzen-mættet hydrogen i 5 minutter ved 100°C. Efter afkøling til stuetemperatur under 20 DK 170841 B1 argon blev der fremstillet en prøve ifølge den i eksempel 11 beskrevne fremgangsmåde, og prøven blev undersøgt ved elektronmikroskopi. Elektronmikrografer viste fibriler med diametre i området fra 30 til 300 Å (fig. 5).
5 De eksempler, som ikke resulterer i dannelse af fibriller (eksempler 11-13, 17-27 og 32-33) er sammenligningseksempler.
I de eksempler, hvor der sker fibrildannelse, blev der dannet fibriller med en i det væsentlige konstant diameter mellem ca. 3,5 og 70 nm, en længde på mere end ca. 104 diameteren, 10 og med et afgrænset indre kerneområde og et ydre område bestående af flere katalytisk dannede, i det væsentlige kontinuerlige grafitagtige lag af ordnede carbonatomer. Fibril-lerne var i det væsentlige fri for pyrolytisk aflej ret carbon, og det indre kerneområde omfattede carbonatomer, som var 15 mindre ordnede end de ordnede carbonatomer af det ydre område, og havde en diameter på ca. 7-25 nm. De eksempler, der resulterede i fibrildannelse, anvendte et forhold mellem den carbonholdige forbindelse og den metalholdige forbindelse på mindst ca. 100:1.
20 TABEL 1
Fibrilsyntesekørsler
Eks. Vækst- Kataly- Vækst- Forbehandlings- Fibriler nr. temp, sator tid betingelser Ja/Nej 25 (°C) nr. (min.) II 500 1 60 25-500°C i 15 min. (Ar) Nej 12 750 l1 420 23-750°C i 40 min. (Ar) Nej 13 800 3 15 22-500°C i 15 min. (luft) Nej 30 5000C i 60 min. (luft) 500-900°C i 15 min. (H2) 900°C i 60 min. (H2) 900-800°C i 11 min. (H2) 14 900 l2 180 26-350°C i 20 min. (H2) Ja 35 350°C i 15 min. (H2) DK 170841 B1 21 350-400°C i 10 min. (CO/H2) 400°C i 210 min. (CO/H2) 400-900°C i 26 min. (Ar) 15 900 2 180 500°C i 60 min. (luft) Ja 5 500-900°C i 15 min. (H2) 900°C i 60 min. (H2) 16 900 4 180 24-900°C i 35 min. (Ar) Ja 900°C i 60 min. (H2) 17 900 3 15 80-500°C i 15 min. (luft) Nej 10 500°C i 60 min. (luft) 500-900°C i 15 min. (H2) 900°C i 60 min. (H2) 18 900 3 60 22-500°C i 15 min. (luft) Nej 500°C i 60 min. (luft) 15 500-750°C i 10 min. (H2) 750°C i 70 min. (H2) 750-500°C i 15 min. (H2) 500°C i 60 min. (Ar/C6H6) 500°C i 90 min. (H2) 20 500-900°C i 20 min. (H2) 19 900 9 60 90-900°C i 30 min. (H2) Nej 9000C i 60 min. (H2) 9000C i 25 min. (Ar) 20 900 1 60 26-900°C i 25 min. (Ar) Nej 25 21 900 1 5 220-900°C i 20 min. (Ar) Nej 22 1000 1 5 252-1000°C i 30 min. (Ar) Nej 23 1000 1 120 31-1000°C i 85 min. (H2/C6H6)Nej 24 1100 5 5 24-500°C i 15 min. (Ar) Nej 500-900°C i 15 min. (H2) 30 900°C i 60 min. (H2) 900-1100°C i 15 min. (H2) 25 1100 10 1 24-500°C i 55 min. (luft) Nej 500°C i 60 min. (luft) 500-1100°C i 30 min. (H2) 35 100°C i 30 min. (H2) 26 1100 9 1 140-500°C i 10 min. (Ar) Nej 500°C i 60 min. (Ar) 500-1100°C i 26 min. (H2) 22 DK 170841 B1 1100°C i 60 min. (H2) 273 1100 5 5 25-500°C i 20 min. (Ar) Nej 500-900°C i 20 min. (H2) 900°C i 60 min. (H2) 5 900-1100°C i 15 min. (H2) 28 1100 3 5 25-500°C i 15 min. (luft) Ja 500°C i 60 min. (luft) 500-900°C i 20 min. (H2) 900°C i 60 min. (H2) 10 900-1100°C i 20 min. (H2) 29 1100 3 1 85-500°C i 10 min. (luft) Ja 500°C i 60 min. (luft) 500-900°C i 20 min. (H2) 900°C i 60 min. (H2) 15 1 900-1100°C i 10 min. (H2) 30 1100 6 5 42-500°C i 15 min. (Ar) Ja 500-900°C i 15 min. (H2) 900°C i 60 min. (H2) 900-1100°C i 15 min. (H2) 20 31 1100 3 5 26-500°C i 20 min. (luft) Ja 500°C i 60 min. (luft) 500-750°C i 10 min. (H2) 750°C i 60 min. (H2) 750-500°C i 10 min. (H2) 25 500°C i 60 min. (Ar/C6H6) 500°C i 90 min. (H2) 500-1100°C i 30 min. (Ar) 32 1150 8 1 98-500°C i 20 min. (Ar) Nej 500°C i 60 min. (Ar) 30 500-750°C i 10 min. (H2) 750°C i 30 min. (H2) 750-1150°C i 20 min. (Ar) 1150°C i 15 min. (Ar) 33 1150 7 1 30-1150°C i 45 min. (H2) Nej 35 1150°C i 15 min. (H2)
Claims (45)
1. I det væsentlige cylindrisk særskilt carbonfibril eller en 10 gruppe bestående af sådanne fibriler, hvori hver fibril omfatter en indre del samt en af kullag bestående ydre del, hvilke er anbragt i det væsentlige koncentrisk omkring fi-brillens cylinderakse, kendetegnet ved, at hver fibril har en i det 15 væsentlige konstant diameter samt en længde, som er større end ca. 102 gange diameteren, at hver fibril har et særskilt indre kerneområde samt et ordnet ydre område som består af flere katalytisk dannede i det væsentlige kontinuerlige lag af ordnede carbonatomer, hvis ydre diameter er mellem 3,0 og 20 70 nm, og idet fibrilen eller fibrilerne er i det væsentlige frie for pyrolytisk aflejret carbon.
1. Katalysator 1 blev opvarmet fra 27°C til 350°C i løbet af 10 minutter under H2, fra 350°C til 500°C på 30 minutter under CO/H2, holdt ved 500°C i 240 minutter under CO/H2 5 og afkølet til stuetemperatur før anvendelsen.
2. Fibril ifølge krav 1, kendetegnet ved, at kernen er hul.
2. Katalysator 1 var anbragt på en carbonfiber.
3. Fibril ifølge krav 1, 25 kendetegnet ved, at det indre kerneområde omfatter carbonatomer, som er mindre ordnede end de ordnede carbonatomer i det ydre område.
3. Tilførslen var ca. 18:1 H2:C6H6 .
4. Fibril ifølge krav 1, kendetegnet ved, at de ordnede carbonatomer er 30 grafitagtige. DK 170841 B1
5. Fibril ifølge krav 1, kendetegnet ved, at længden er større end ca. 103 gange diameteren.
6. Fibril ifølge krav 1, 5 kendetegnet ved, at længden er større end ca. 104 gange diameteren.
7. Fibril ifølge krav 1, kendetegnet ved, at diameteren er mellem ca. 7 og og ca. 25 nm.
8. Fibril ifølge krav 1, kendetegnet ved, at det indre kerneområde har en diameter på over ca. 2 nm.
9. Fremgangsmåde til fremstilling af én eller flere i det væsentlige cylindriske carbonfibriler ifølge krav 1, 15 kendetegnet ved, at en katalysator i form af én eller flere metalholdige partikler bringes i kontakt med en precursor i form af en gasformig, carbonholdig forbindelse ved en temperatur, der for at undgå signifikant dannelse af pyrolytisk carbon på den katalytisk dannede ydre region af 20 fibrilen er under den carbonholdige forbindelses termiske nedbrydningstemperatur, idet forholdet på tørvægtbasis mellem den carbonholdige forbindelse og den metalholdige partikel er i det mindste ca. 100:1.
10. Fremgangsmåde ifølge krav 9, 25 kendetegnet ved, at kontakten mellem den metalholdige partikel og den carbonholdige forbindelse udføres i nærværelse af en forbindelse, der er i stand til at reagere med carbon og danne gasformige produkter.
11. Fremgangsmåde ifølge krav 10, 30 kendetegnet ved, at den forbindelse, der er i stand til at reagere med carbon, er C02, H2 eller H20. DK 170841 B1
12. Fremgangsmåde ifølge krav 9, kendetegnet ved, at den carbonholdige forbindelse er carbonmonoxid.
13. Fremgangsmåde ifølge krav 9, 5 kendetegnet ved, at den carbonholdige forbindelse er et carbonhydrid.
14. Fremgangsmåde ifølge krav 9, kendetegnet ved, at den carbonholdige forbindelse indeholder oxygen.
15. Fremgangsmåde ifølge krav 14, kendetegnet ved, at den carbonholdige forbindelse er formaldehyd, acetaldehyd, acetone, methanol, ethanol eller blandinger deraf.
16. Fremgangsmåde ifølge krav 9, 15 kendetegnet ved, at den carbonholdige forbindelse er aromatisk.
17. Fremgangsmåde ifølge krav 16, kendetegnet ved, at den aromatiske carbonholdige forbindelse er benzen, toluen, xylen, cumol, ethylbenzen, 20 naphthalen, phenanthren, anthracen eller blandinger deraf.
18. Fremgangsmåde ifølge krav 9, kendetegnet ved, at den carbonholdige forbindelse er ikke-aromatisk.
19. Fremgangsmåde ifølge krav 9, 25 kendetegnet ved, at den carbonholdige forbindelse er methan, ethan, propan, ethylen, propylen eller acetylen eller blandinger deraf. DK 170841 B1
20. Fremgangsmåde ifølge krav 9, kendetegnet ved, at den metalholdige partikel er en jern-, cobalt- eller nikkelholdig partikel med en diameter på mellem ca. 3,5 og ca. 70 nm.
21. Fremgangsmåde ifølge krav 9, kendetegnet ved, at den metalholdige partikel er anbragt på et kemisk kompatibelt, ildfast underlag.
22. Fremgangsmåde ifølge krav 21, kendetegnet ved, at underlaget er aluminiumoxid.
23. Fremgangsmåde ifølge krav 21, kendetegnet ved, at underlaget er carbon.
24. Fremgangsmåde ifølge krav 21, kendetegnet ved, at underlaget er et silikat.
25. Fremgangsmåde ifølge krav 21, 15 kendetegnet ved, at silikatet er et aluminiumsilikat .
26. Fremgangsmåde ifølge krav 9, kendetegnet ved, at reaktionstiden er fra ca. 10 sekunder til ca. 180 minutter, trykket er fra ca. 1/10 atmos-20 fære til ca. 10 atmosfærer, den metalholdige partikel er en jernholdig partikel, den carbonholdige forbindelse er benzen, temperaturen er fra ca. 900°C til ca. 1150°C, og forholdet på tørvægtbasis mellem benzen og den jernholdige partikel er i det mindste ca. 1000:1.
27. Fremgangsmåde ifølge krav 26, kendetegnet ved, at reaktionstiden er ca. 180 minutter, trykket er ca. 1 atmosfære, den carbonholdige forbindelse er benzen i en ca. 9:1 volumenblanding af hydro-gen/benzen, og temperaturen er ca. 900°C. DK 170841 B1
28. Fremgangsmåde ifølge krav 26, kendetegnet ved, at reaktionstiden er fra ca. 1 til ca. 5 minutter, trykket er ca. 1 atmosfære, den carbon-holdige forbindelse er benzen i en ca. 9:1 volumenblanding af 5 hydrogen/benzen, og temperaturen er ca. 1100°C.
29. Fremgangsmåde ifølge krav 26, kendetegnet ved, at den jernholdige partikel er anbragt på et kemisk kompatibelt, ildfast underlag.
30. Fremgangsmåde ifølge krav 29, 10 kendetegnet ved, at det ildfaste underlag er aluminiumoxid eller carbon.
31. Fremgangsmåde til fremstilling af én eller flere i det væsentlige cylindriske carbonfibriler ifølge krav 9, kendetegnet ved, at én eller flere metalholdige 15 partikler bringes i kontakt med en gasformig, carbonholdig forbindelse, og den metalholdige partikel opvarmes uafhængigt til en temperatur på mellem ca. 850°C og ca. 1800°C, idet temperaturen af partiklen er højere end temperaturen af den gasformige, carbonholdige forbindelse.
32. Fremgangsmåde ifølge krav 31, kendetegnet ved, at partiklen opvaru^s ved elektromagnetisk bestråling.
33. Fremgangsmåde ifølge krav 9, kendetegnet ved, at hver af fibrilerne har en 25 diameter, der i det væsentlige er den samme som diameteren af enhver anden fibril.
34. Fremgangsmåde ifølge krav 9, kendetegnet ved, at de metalholdige partikler er præformede. DK 170841 B1
35. Kompositmateriale, kendetegnet ved, at det omfatter en mængde carbon-fibriler ifølge krav 1.
36. Kompositmateriale ifølge krav 35, 5 kendetegnet ved, at det omfatter en matrix af en organisk polymer.
37. Kompositmateriale ifølge krav 35, kendetegnet ved, at det omfatter en matrix af en uorganisk polymer.
38. Kompositmateriale ifølge krav 35, kendetegnet ved, at det omfatter en matrix af et metal.
39. Anvendelse af carbonfibrilerne til armering af et strukturmateriale , 15 kendetegnet ved, at der i materialet inkorporeres en virksom armerende mængde carbonfibriler ifølge krav 1.
40. Fremgangsmåde til forøgelse af et materiales elektriske ledningsevne, kendetegnet ved, at der i materialet inkorporeres 20 en til forøgelse af den elektriske ledningsevne virksom mængde carbonfibriler ifølge krav 1.
41. Fremgangsmåde til forøgelse af et materiales varmeled-ningsevne, kendetegnet ved, at der i materialet inkorporeres 25 en til forøgelse af varmeledningsevnen virksom mængde carbon-fibriler ifølge krav 1.
42. Fremgangsmåde til forøgelse af overfladearealet af en elektrode eller en elektrolytisk kondensatorplade, kendetegnet ved, at der til elektroden eller 30 pladen fastgøres én eller flere fibriler ifølge krav 1. DK 170841 B1
43. Fremgangsmåde til understøtning af en katalysator, kendetegnet ved, at der fastgøres en katalysator til en fibril ifølge krav 1.
44. Fremgangsmåde ifølge krav 43, 5 kendetegnet ved, at katalysatoren er en elektrokemisk katalysator.
45. Fremgangsmåde til beskyttelse af en genstand mod elektromagnetisk bestråling, kendetegnet ved, at der i genstanden inkorporeres 10 en virksom beskyttende mængde carbonfibriler ifølge krav 1.
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US06/678,701 US4663230A (en) | 1984-12-06 | 1984-12-06 | Carbon fibrils, method for producing same and compositions containing same |
US67870184 | 1984-12-06 | ||
PCT/US1985/002390 WO1986003455A1 (en) | 1984-12-06 | 1985-12-04 | Carbon fibrils, method for producing same, and compositions containing same |
US8502390 | 1985-12-04 |
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DK376286D0 DK376286D0 (da) | 1986-08-06 |
DK376286A DK376286A (da) | 1986-08-06 |
DK170841B1 true DK170841B1 (da) | 1996-02-05 |
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Application Number | Title | Priority Date | Filing Date |
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DK376286A DK170841B1 (da) | 1984-12-06 | 1986-08-06 | Carbonfibriller, fremgangsmåde til fremstilling deraf, kompositioner indeholdende dem samt anvendelse deraf |
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US (1) | US4663230A (da) |
EP (1) | EP0205556B1 (da) |
JP (3) | JPS62500943A (da) |
KR (1) | KR900008329B1 (da) |
AT (1) | ATE122406T1 (da) |
AU (1) | AU590239B2 (da) |
BR (1) | BR8507114A (da) |
CA (1) | CA1284857C (da) |
DE (1) | DE3588016T2 (da) |
DK (1) | DK170841B1 (da) |
FI (1) | FI87938C (da) |
IL (1) | IL77210A (da) |
NO (1) | NO173514C (da) |
WO (1) | WO1986003455A1 (da) |
ZA (1) | ZA859293B (da) |
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- 1985-12-04 KR KR1019860700536A patent/KR900008329B1/ko not_active IP Right Cessation
- 1985-12-04 EP EP86900426A patent/EP0205556B1/en not_active Expired - Lifetime
- 1985-12-04 WO PCT/US1985/002390 patent/WO1986003455A1/en active IP Right Grant
- 1985-12-04 JP JP61500094A patent/JPS62500943A/ja active Granted
- 1985-12-04 AU AU52058/86A patent/AU590239B2/en not_active Ceased
- 1985-12-04 AT AT86900426T patent/ATE122406T1/de not_active IP Right Cessation
- 1985-12-04 DE DE3588016T patent/DE3588016T2/de not_active Expired - Lifetime
- 1985-12-04 CA CA000496810A patent/CA1284857C/en not_active Expired - Lifetime
- 1985-12-04 ZA ZA859293A patent/ZA859293B/xx unknown
- 1985-12-04 BR BR8507114A patent/BR8507114A/pt not_active IP Right Cessation
-
1986
- 1986-08-05 NO NO863163A patent/NO173514C/no not_active IP Right Cessation
- 1986-08-05 FI FI863200A patent/FI87938C/fi not_active IP Right Cessation
- 1986-08-06 DK DK376286A patent/DK170841B1/da not_active IP Right Cessation
-
1990
- 1990-03-26 JP JP2076556A patent/JP2588626B2/ja not_active Expired - Lifetime
-
1995
- 1995-05-15 JP JP7115971A patent/JP2641712B2/ja not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
FI863200A (fi) | 1986-08-05 |
DK376286D0 (da) | 1986-08-06 |
JPH0364606B2 (da) | 1991-10-07 |
JPS62500943A (ja) | 1987-04-16 |
EP0205556A4 (en) | 1989-04-24 |
NO173514B (no) | 1993-09-13 |
EP0205556B1 (en) | 1995-05-10 |
ZA859293B (en) | 1986-08-27 |
FI863200A0 (fi) | 1986-08-05 |
NO863163D0 (no) | 1986-08-05 |
FI87938C (fi) | 1993-03-10 |
NO173514C (no) | 1993-12-22 |
FI87938B (fi) | 1992-11-30 |
NO863163L (no) | 1986-08-05 |
DE3588016D1 (de) | 1995-06-14 |
ATE122406T1 (de) | 1995-05-15 |
EP0205556A1 (en) | 1986-12-30 |
BR8507114A (pt) | 1987-03-31 |
JP2588626B2 (ja) | 1997-03-05 |
AU590239B2 (en) | 1989-11-02 |
JPH0827279A (ja) | 1996-01-30 |
KR900008329B1 (ko) | 1990-11-15 |
CA1284857C (en) | 1991-06-18 |
US4663230A (en) | 1987-05-05 |
JP2641712B2 (ja) | 1997-08-20 |
IL77210A (en) | 1990-11-05 |
DK376286A (da) | 1986-08-06 |
DE3588016T2 (de) | 1995-11-02 |
KR870700043A (ko) | 1987-02-28 |
AU5205886A (en) | 1986-07-01 |
WO1986003455A1 (en) | 1986-06-19 |
JPH03174018A (ja) | 1991-07-29 |
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