CN107176604B - A kind of method that carbon materials surface in situ generates nano-carbide coating - Google Patents
A kind of method that carbon materials surface in situ generates nano-carbide coating Download PDFInfo
- Publication number
- CN107176604B CN107176604B CN201610133960.4A CN201610133960A CN107176604B CN 107176604 B CN107176604 B CN 107176604B CN 201610133960 A CN201610133960 A CN 201610133960A CN 107176604 B CN107176604 B CN 107176604B
- Authority
- CN
- China
- Prior art keywords
- carbon
- carbon materials
- coating
- carbide
- oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000000576 coating method Methods 0.000 title claims abstract description 80
- 239000011248 coating agent Substances 0.000 title claims abstract description 78
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 61
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000005255 carburizing Methods 0.000 claims abstract description 16
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 8
- 238000003980 solgel method Methods 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 47
- 229910003460 diamond Inorganic materials 0.000 claims description 46
- 239000010432 diamond Substances 0.000 claims description 46
- 229910052799 carbon Inorganic materials 0.000 claims description 43
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 23
- 239000004917 carbon fiber Substances 0.000 claims description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 22
- 238000010792 warming Methods 0.000 claims description 11
- 239000003638 chemical reducing agent Substances 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 229930006000 Sucrose Natural products 0.000 claims description 8
- 239000005720 sucrose Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 150000001721 carbon Chemical group 0.000 claims description 6
- 229910003470 tongbaite Inorganic materials 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 239000002048 multi walled nanotube Substances 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- 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
- 238000003763 carbonization Methods 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- -1 polyethylene Polymers 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 2
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 claims description 2
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 claims description 2
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 2
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 2
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 2
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229910052702 rhenium Inorganic materials 0.000 claims description 2
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 229910003468 tantalcarbide Inorganic materials 0.000 claims description 2
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 2
- 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 claims description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 2
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims 1
- 239000004698 Polyethylene Substances 0.000 claims 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims 1
- 229910000423 chromium oxide Inorganic materials 0.000 claims 1
- 239000004615 ingredient Substances 0.000 claims 1
- 229910052750 molybdenum Inorganic materials 0.000 claims 1
- 239000011733 molybdenum Substances 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims 1
- 229910010271 silicon carbide Inorganic materials 0.000 claims 1
- 125000000185 sucrose group Chemical group 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 23
- 239000002131 composite material Substances 0.000 abstract description 12
- 229920002521 macromolecule Polymers 0.000 abstract description 11
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 8
- 239000000919 ceramic Substances 0.000 abstract description 6
- 239000011230 binding agent Substances 0.000 abstract description 2
- 150000001722 carbon compounds Chemical class 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 abstract 1
- 239000002103 nanocoating Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 239000010936 titanium Substances 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 9
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 8
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 7
- 229960000935 dehydrated alcohol Drugs 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 229910052719 titanium Inorganic materials 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 229920002593 Polyethylene Glycol 800 Polymers 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 239000011651 chromium Substances 0.000 description 5
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 238000007747 plating Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000000428 dust Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 238000005240 physical vapour deposition Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 239000000908 ammonium hydroxide Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 229910017985 Cu—Zr Inorganic materials 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 229910039444 MoC Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 238000003483 aging Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of methods that carbon materials surface in situ generates nano-carbide coating, belong to the technical field of material such as high-strength, superhard, wear-resisting and heat management.This method is that oxide sol or gel are prepared using sol-gel method, after being uniformly coated to carbon materials surface, handled after drying, sintering process, then through vacuum high-temperature, it realizes in-situ reducing-carburizing reagent, forms in-situ carbon compound nano coating on carbon materials surface.The present invention overcomes carbon materials surface free energy is low between the binders/matrix such as metal, ceramics and macromolecule poor compatibility, interface cohesion is bad the problems such as, the binding force between matrixes and carbon materials such as metal, ceramics and macromolecule is improved, the thermal impedance at interface between carbon materials and metal is reduced.The present invention can effectively improve the mechanics of composite materials such as carbon materials enhancing metal, ceramics and macromolecule, thermally conductive, conductive and wear-resisting etc. performances.
Description
Technical field
The present invention relates to the technical field of material such as high-strength, superhard, wear-resisting and heat management, and in particular to a kind of carbon material
Expect the method that surface in situ generates nano-carbide coating.
Background technique
Carbon possesses a variety of C-C bonding modes and crystal structure, can form the carbon material of a variety of configurations and excellent combination property
Material, such as carbon fiber, diamond, crystalline flake graphite and multi-walled carbon nanotube, with density is low, thermal expansion coefficient is low, intensity is high, mould
It measures the advantages that big, it is especially thermally conductive, electric conductivity is extremely excellent.Carbon materials are not only the important former material in traditional industry field
The fields such as material and photoelectricity, national defence and aerospace are the grand strategy goods and materials of the high-tech industry of representative.
Although carbon materials possess many excellent performances, carbon materials are mostly particle or threadiness, are difficult individually to make
With.Composite material is a kind of multiphase solid material being composed of two or more physics substance different with chemical property
The advantages of expecting, can integrating different materials is learnt from other's strong points to offset one's weaknesses, and is one of important development direction of Material Field.Therefore, carbon materials
It is considered as the ideal reinforcement of composite material.But between the other materials such as carbon materials and metal, ceramics, carbon, macromolecule
Interface compatibility it is poor, such as wetability, chemical stability and mechanical compatibility between carbon materials and metallic aluminium etc. is all
It is poor.In addition, the heat-conducting mode of the materials such as carbon materials and metal, ceramics and macromolecule is also completely different, this leads to carbon material
Interface resistance between material and other materials is anti-higher, is unfavorable for giving full play to the characteristic of carbon material high thermal conductivity.
Research shows that can be effectively improved or improve carbon materials and other materials in the modification of carbon material surface alloying coating
Compatibility between material.Currently, carrying out the coating modified technology of surface alloying to carbon materials has chemical vapor deposition
(CVD), the micro- evaporation plating of physical vapour deposition (PVD) (PVD), magnetron sputtering, vacuum, chemical plating and elements diffusion method etc..Wherein, PVD and
The methods of magnetron sputtering is relatively suitable for coating in the outer surface of smooth workpiece or material, and can not be in the inner surface of porous material
Uniformly coating is formed, therefore is difficult to apply to the carbon materials such as diamond, carbon fiber, crystalline flake graphite；Chemical vapour deposition technique
The process is more complicated, the unfavorable factors such as at high cost also greatly limit its industrial applications.Although in addition, Electroless Cu Plating and Ni
Technology is highly developed, but belongs to chemical inertness between Cu, Ni and carbon, is hardly produced metallic compound, can not be fundamentally
Solve the problems, such as poor compatibility between the materials such as carbon materials and metal, and the preparation process of the coatings such as chemical plating Ti, Al it is complicated,
Cost is also higher, and is easily guided into impurity element, therefore is not also used widely.
" the diamond plating for 25-28 pages of the phase of the academic journal " diamond and grinding materials and grinding tool engineering " the 128th published for 2002
In the relationship of a technique and using effect " text, Wang Yanhui et al. is coated with using the micro- evaporation electroplating method of vacuum in diamond surface
The diamond drop-off rate in diamond saw blade can be effectively reduced in Ti coating, improves the efficiency and service life of tool.This method
Be by diamond and the pioneer containing titanium elements after mixing, can be in short distance using Ti atom under vacuum, hot conditions
The principle of interior migration finally deposits Ti coating in diamond surface.However, theoretically the thickness of diamond surface titanium coating divides
Cloth Normal Distribution, the i.e. titanium coating apart from titanium elements precursor more near position are thicker.In addition, the academic phase published in 2006
" vacuum slowly vapor deposition parameters on coating quality and the gold of 17-19 pages of the phase of periodical " diamond and grinding materials and grinding tool engineering " the 155th
In the influence of a hard rock performance " text, Zhao Yucheng et al. has inquired into influence of the temperature to diamond, finds the condition at 1100 DEG C
Under, excessively high temperature, which will increase the extension of diamond internal flaw and the expansion of Ti wrapping layer, leads to the chance of crystal cleavage, leads to gold
The impact flexibility of hard rock sharply declines.
22-26 pages of volume 68 of the academic journal " Composites Part B:Engineering " of publication in 2015
“Thermal conductivity of Cu-Zr/diamond composites produced by high
In a temperature-high pressure method " text, He etc. is under conditions of 1500 DEG C, 5GPa using infiltration legal system
677W/mK is reached for diamond/Cu-Zr composite material, the thermal conductivity of composite material, this is mainly due to Zr element and exists
Being diffused into diamond surface and foring ZrC layers of nanoscale in Cu.
603-609 pages of volume 265 of the academic journal " Applied Surface Science " of publication in 2013
“Preparation of anti-oxidative SiC/SiO2coating on carbon fibers from
In a vinyltriethoxysilane by sol-gel method " text, Xia et al. is using sol-gel method in carbon fiber
Surface is coated with SiO2Coating, and under the protection of high-purity argon gas 1500 DEG C sintering 2 hours after, obtain SiC/SiO2Compound painting
Layer, research shows that the coating can effectively improve the inoxidizability of carbon fiber.The experimental program is using the carbon in carbon fiber as also
Former agent, but since there is carbon fiber good thermal stability and the SiC layer being initially formed to hinder the diffusion of carbon atom, even if 1500
DEG C, under conditions of sintering 2 hours still cannot provide raw material of the sufficient free carbon atom as reducing agent and carburizing reagent, lead
It causes still to remain part SiO in coating2。
Summary of the invention
The object of the present invention is to provide a kind of method that carbon materials surface in situ generates nano-carbide coating, this method
Generated in-situ nano-sized carbon can be prepared on the carbon materials such as carbon fiber, diamond, crystalline flake graphite and multi-walled carbon nanotube surface
The thickness of compound coating, the coating can be controlled in 10~20nm, and with coating, complete, coating uniform, chemical component are controllable, technique
It is simple and reliable, low in cost, preparation temperature is low, is coated the small, carburizing reagent of carbon materials damage completely and has wide range of applications
The advantages that.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of method that carbon materials surface in situ generates nano-carbide coating, this method comprises the following steps:
(1) single or doping oxide sol or gel, concentration 0.05 are prepared using traditional sol-gel method
~1.5 mol/Ls；
(2) carbon materials removing surface is clean；The carbon materials are that carbon fiber, graphite, diamond and multi wall carbon are received
One or more of mitron；
(3) surface coating processing: according to the difference of coating object, the side such as ultrasonic oscillation, lifting, stirring or spraying is utilized
Colloidal sol or gel are uniformly coated to carbon materials surface by method；
(4) be dried: by the carbon materials after the coating processing of surface be placed on 10~80 DEG C of drying, in clean room into
Row is dried, and being dried the time is 1 hour~mono- week；
(5) pre-sintering is handled: under the conditions of atmosphere or protective atmosphere, by the carbon materials after coating and drying process
It is put into resistance furnace, is warming up to 240-700 DEG C with the rate less than 10 DEG C/min, 20-300 minutes is kept the temperature, in carbon materials table
Face forms coating；
(6) operating process of step (3)-step (5) is repeated, until the coating on carbon materials surface reaches required thickness；
(7) in-situ reducing-carburizing reagent: the carbon materials after sintering processes are put into vacuum drying oven, are evacuated in furnace
Vacuum degree is less than 5 × 10-1After Pa, after being warming up to 700~1450 DEG C with the rate lower than 20 DEG C/min and keep the temperature 2~48 hours,
It is furnace-cooled to room temperature under vacuum condition, completes in-situ reducing-carburizing reagent, finally obtains receiving for growth in situ on carbon materials surface
Rice carbide coating.
In above-mentioned steps (1), the single oxide sol or gel, which refer to, has contained only titanium oxide, silica, oxidation
The colloidal sol of one or more of chromium, vanadium oxide, zirconium oxide, niobium oxide, tantalum oxide, molybdenum oxide, tungsten oxide and rheium oxide is solidifying
Glue；The oxide sol or gel of the doping refer to that addition is as reducing agent in single oxide sol (or gel)
The colloidal sol (or gel) formed after the precursor of (carbon), wherein carbon atom in the precursor as reducing agent (carbon) of addition
Mole is 0.1 to 10 times of oxide molar amount in colloidal sol or gel, and the precursor as reducing agent (carbon) is sucrose, poly- second
The organic matters such as alkene, polyvinyl alcohol.It wherein, is undersaturation as the content of the precursor of reducing agent residual carbon after Pintsch process,
Crack total amount of the content lower than carbon required for reduction-carburizing reagent of residual carbon.In addition, the addition of macromolecule organic is also
The viscosity that colloidal sol or gel can be improved is conducive to increase coating layer thickness, and the repeatedly processes such as coating are reduced or avoided.
It is described that carbon materials removing surface is clean in above-mentioned steps (2), mainly according to the residual of carbon materials surface
Excess or impurity the methods such as burn by pickling, alkali cleaning, organic solvent washing and/or high temperature.The residue on carbon materials surface
Or impurity refers to the pollutant etc. introduced during the remaining catalyst of carbon material surface, organic matter etc. and production and storage,
The gluing of remaining catalyst, carbon fiber surface on such as multi-walled carbon nanotube.
In above-mentioned steps (7), reducing agent used in the in-situ reducing-carburizing reagent is carbon, and the source of carbon is wrapped
The organic matter for including doping in the carbon and/or colloidal sol (or gel) of coated object carbon materials itself cracks under the high temperature conditions to be remained
Remaining carbon.
Become titanium carbide, carbonization in the group that carbon materials surface in situ generates nano-carbide coating using the above method
One of silicon, chromium carbide, vanadium carbide, zirconium carbide, niobium carbide, tantalum carbide, molybdenum carbide, tungsten carbide and carbonization carbide such as rhenium or
Several (as (Ta, Nb) C), nano-carbide coating with a thickness of 10~20nm.
It design principle of the present invention and has the beneficial effect that:
1, by the reaction equation of carbon reduced oxide it is found that its reaction product is gaseous CO, the present invention uses vacuum
Method, the CO for generating reaction quickly taken away, leads to the concentration dramatic decrease of reaction product, it is anti-that reduction will be greatly improved in this
The speed answered, and ensure that the irreversible of reaction.
2, according to thermodynamic principles, the chemical reaction of carbon reduced oxide needs to be more than that certain reaction temperature just can be into
Row must satisfy the Gibbs free energy decline of reaction system, and Gibbs free energy is before a standard atmospheric pressure
It puts and carrys out evaluation response maximum system energy.Under vacuum conditions, reaction product CO, which is pumped, is equivalent to reaction system and externally does work,
Compared with conventional argon gas protective condition, this will be substantially reduced the reaction temperature of carbon reduced oxide.
3, the temperature of superelevation will lead to diamond graphitization and energy cost and rise, and C-C key is highly stable covalent
Key, the constraint that lower temperature cannot allow more carbon atoms to be detached from C-C key become free state carbon atom, furthermore carbon material surface
The carbide lamella formed in advance can also hinder carbon atom to spread on the outside of coating, these cause carbon materials and oxide coating it
Between reduction and carburizing reagent cannot thoroughly carry out.The present invention is used to mix in the precursor (sol-gel) of oxide coating
Miscellaneous sucrose etc. contains carbon macromolecule, cracks remaining carbon as supplementary carbon source using macromolecule under hot conditions, ensure that in situ go back
Original-carburizing reagent progress.
4, the viscosity that sol-gel is improved using the addition of macromolecule organic is conducive to increase coating layer thickness, be reduced
Or avoid the repeatedly processes such as coating.
5, for unsaturated state, (i.e. the content of cracking residual carbon is lower than reduction-carburizing reagent institute to the macromolecule carbon source adulterated
The total amount of the carbon needed), thus in situ in reduction-carbonation reaction carbon concentration in gradient distribution, i.e., closer to carbon
The concentration of material surface carbon is higher, the atom (i.e. oxide reduzate) being reduced can to carbon material surface spread and in turn
In-situ preparation carbide.
6, the oxide coating of sol-gel method coating is nano particle composition, utilizes heredity principle, in-situ preparation carbon
Compound coating is similarly nanostructure.
7, the method for the present invention can effectively solve phase between nanocarbon/metal, carbon/ceramics, carbon/macromolecule and carbon/carbon interface
The problem of capacitive difference improves bond strength, thermal conductivity and the wear-resisting property at interface between carbon and multiple material.In addition, should
The in-situ nano carbide coating of technique preparation can also effectively improve the antioxygenic property of carbon materials.
Detailed description of the invention
Fig. 1 is the generated in-situ TiC coating of diamond surface prepared by embodiment 1；Wherein: (a) electron scanning Electronic Speculum
(SEM) observe TiC coating cladding diamond grind after pattern, (b) and (c) be respectively TiC/ diamond low power and
High power high-resolution atomic response.
Fig. 2 is the SEM pattern of SiC coating cladding diamond broken material prepared by embodiment 2.
Fig. 3 is the generated in-situ nanometer Cr of carbon fiber surface prepared by embodiment 33C2Coating；Wherein: (a) carbon fiber surface
In-situ preparation nanometer Cr3C2SEM pattern after coating, the SEM photograph of the carbon fiber surface coating after (b) artificially poking.
Specific embodiment
The present invention can prepare in-situ nano carbide coating on the carbon materials surface of various configuration, below by way of implementation
The present invention is further described for example.
Embodiment 1:
The coating object selected in the present embodiment is the bortz powder of 25 μm of commercially available partial sizes, the specific steps are as follows:
(1) the present embodiment is with butyl titanate (Ti (OC4H9)4) it is presoma, and use dehydrated alcohol, deionized water, second
Acyl acetone, nitric acid (concentration 69wt.%, analyze pure) and PEG-800 as raw material, wherein butyl titanate, dehydrated alcohol, go
The volume ratio of ionized water, acetylacetone,2,4-pentanedione and PEG-800 is 1:9:0.7:0.15:0.25；Dehydrated alcohol is first pressed the 1/3 of total dosage
It is two parts with 2/3 point；It is with deionized water that 69wt.% nitric acid is dilute by deionized water and 1/3 dehydrated alcohol mixing wiring solution-forming
It is interpreted into the dust technology that concentration is 2.5wt.%, then the pH value for adjusting solution with dust technology is made into solution A to 3.0；By the titanium of weighing
Sour four butyl esters, acetylacetone,2,4-pentanedione, are slowly added in remaining 2/3 dehydrated alcohol under rapid stirring, are made into B solution；So
Afterwards under fast stirring, solution A is slowly dropped into B solution with buret, then instills PEG-800 (polyethylene glycol), stirring is equal
The TiO for the homogeneous transparent that concentration is 0.3 mol/L is obtained after even2Colloidal sol；The colloidal sol of acquisition still aging 24 hours stand-by.
(2) diamond of clean surface is poured into the colloidal sol of step (1) acquisition, after mixing evenly, in 360rpm revolving speed
Under conditions of centrifugal filtration after five minutes, take out diamond and be placed in 50 DEG C of drying box and be dried, it is small to be dried 48
When.
(3) after the diamond that step (2) obtain being put into cover and closed preferable graphite crucible, it is placed in resistance furnace
In, 1 hour is kept the temperature after being warming up to 350 DEG C under atmospheric environment with the rate of 5 DEG C/min, carries out pre-sintering processing；
(4) finally the graphite crucible for filling diamond is put into vacuum drying oven, be evacuated in furnace vacuum degree less than 1 ×
10-1After Pa, after being warming up to 1250 DEG C with the rate of 10 DEG C/min and keep the temperature 4 hours, it is furnace-cooled to room temperature under vacuum condition, completes former
Position reduction-carburizing reagent, the final diamond for obtaining surface and being coated with in-situ nano TiC coating.
Fig. 1 show the pattern and microstructure of 40~50 μm of diamond surface coating TiC coatings in the present embodiment,
The TiC coating tight that diamond surface is about 10nm by thickness, and be tightly combined between diamond and TiC layer and (pass through SEM
Pattern is difficult to distinguish diamond initial surface and TiC coating, to the diamond of TiC coating cladding, after grinding known to observation
(such as Fig. 1 (a): black portions are conductive preferable TiC coating, and brilliant white part is that the diamond of conductive insulation destroys cleavage
Face)；50vol.% diamond/6061Al composite material is prepared for using powder metallurgic method, performance test shows in diamond table
After the coated carbide coating of face, the bending strength and thermal conductivity of the composite material of preparation have significantly promotion (such as table 1).
Embodiment 2:
The coating object selected in the present embodiment is 40~50 μm of commercially available diamond broken materials, the specific steps are as follows:
(1) the present embodiment with ethyl orthosilicate (TEOS) be presoma, and using nitric acid (concentration 69wt.%, analysis
It is pure), deionized water, dehydrated alcohol and sucrose as raw material, the wherein molar ratio of TEOS, deionized water, dehydrated alcohol and sucrose
For 1:6:25:0.25；Nitric acid is first diluted to the dust technology that concentration is 2.5wt.% with deionized water, then with dust technology distillation
Water pH value is adjusted to 3, then TEOS weighing and ethyl alcohol are add to deionized water, and airtight heating is to 70 DEG C and stirs 24 hours,
Then sucrose is added and stops stirring to after being completely dissolved, obtains the SiO that concentration is about the homogeneous transparent of 0.15 mol/L2Colloidal sol
Stand 48 hours for use.
(2) diamond of clean surface is poured into the SiO of step (1) acquisition2In colloidal sol, after mixing evenly, in 300rpm
After five minutes, taking-up single-crystal diamond, which is placed in 50 DEG C of drying box, to be dried, dry for centrifugal filtration under conditions of revolving speed
Processing 48 hours.
(3) after the diamond that step (2) obtain being put into cover and closed preferable graphite crucible, it is placed in resistance furnace
In, 1 hour is kept the temperature after being warming up to 350 DEG C under atmospheric environment with the rate of 5 DEG C/min, carries out pre-sintering processing；
(4) finally the graphite crucible for filling single-crystal diamond is put into vacuum drying oven, is evacuated in furnace vacuum degree less than 1
×10-1After Pa, after being warming up to 1350 DEG C with the rate of 10 DEG C/min and keep the temperature 4 hours, it is furnace-cooled to room temperature under vacuum condition, completes
In-situ reducing-carburizing reagent, the final diamond for obtaining surface and being coated with in-situ nano SiC coating.
As shown in Fig. 2, diamond broken material is coated completely by generated in-situ nano SiC coating, and SiC coating uniform,
It is fine and close；50vol.% diamond/6061Al composite material is prepared for using powder metallurgic method, performance test shows in coating SiC
After coating, the thermal conductivity of composite material is promoted (such as table 1) by a relatively large margin.
1 50vol.% diamond of table/6061Al composite material performance characteristic
Embodiment 3:
The coating object selected in the present embodiment is domestic T300 carbon fiber, the specific steps are as follows:
(1) the present embodiment is with chromic nitrate (Cr (NO3)3·9H2It O) is presoma, and (concentration is using deionized water, ammonium hydroxide
25wt.%), sucrose (analysis pure) and PEG-800 be as raw material, wherein the weight of chromic nitrate, deionized water, sucrose and PEG-800
Amount is than being 1:9:0.5:0.5.Under agitation, first chromic nitrate is dissolved into deionized water, then with deionized water by ammonium hydroxide
Concentration adjust to 5wt.%, diluted ammonium hydroxide is slowly dropped in chromium nitrate solution, pH to 3.5 is adjusted, and is kept stirring
Form within 0.5 hour the Cr for the transparent and stable that concentration is 0.25 mol/L2O3Colloidal sol, 60 DEG C of water-bath agings 1 are small under conditions of stirring
When, stand 48 hours it is stand-by.
(2) carbon fiber is put into vacuum drying oven, is evacuated to 1 × 10-1After Pa or more, it is warming up to 400 DEG C and heat preservation 1 is small
When, remove the organic binder of carbon fiber surface.
(3) Cr will be housed2O3The container of colloidal sol is placed in ultrasonic oscillation sink, and then the carbon fiber handled well is soaked
Enter into colloidal sol, carbon fiber is pulled out from colloidal sol with the speed of 1.6mm/s after ultrasonic oscillation 5 minutes, it is clean to be placed in drying
Net place is dried.
(4) after the carbon fiber that step (3) obtain being put into cover and closed preferable graphite crucible, it is placed in resistance furnace
In, 1 hour is kept the temperature after being warming up to 350 DEG C with the rate of 5 DEG C/min, carries out pre-sintering processing；
(5) finally the carbon fiber that step (4) obtain is put into vacuum drying oven, is evacuated in furnace vacuum degree less than 1 × 10- 1After Pa, after being warming up to 1000 DEG C with the rate of 10 DEG C/min and keep the temperature 4 hours, it is furnace-cooled to room temperature under vacuum condition, completes in situ
Reduction-carburizing reagent, the final surface that obtains are coated with in-situ nano Cr3C2The carbon fiber of coating.
As shown in figure 3, carbon fiber surface in-situ preparation nanometer Cr3C2After coating, coating is evenly distributed, wraps up tightly；Through
After artificially poking, it can be observed that Cr3C2Coating layer thickness is about tens nanometers.
Claims (3)
1. a kind of method that carbon materials surface in situ generates nano-carbide coating, it is characterised in that: this method includes as follows
Step:
(1) using the oxide sol or gel of sol-gel method preparation doping, concentration is 0.05~1.5 mol/L；Institute
The oxide sol or gel for stating doping are after adding in single oxide sol or gel as the precursor of reducing agent
It is formed, the added precursor as reducing agent is sucrose, polyethylene or polyvinyl alcohol；The single oxide sol or
Gel, which refers to, has contained only titanium oxide, silica, chromium oxide, vanadium oxide, zirconium oxide, niobium oxide, tantalum oxide, molybdenum oxide, tungsten oxide
With the colloidal sol or gel of one or more of rheium oxide ingredient；It is added in the oxide sol or gel of the doping
Mole as carbon atom in the precursor of reducing agent is 0.1 to 10 times of oxide molar amount in colloidal sol or gel；
(2) carbon materials removing surface is clean；
(3) surface coating processing:, will be molten using ultrasonic oscillation, lifting, stirring or spraying method according to the difference of coating object
Glue or gel are uniformly coated to carbon materials surface；
(4) it is dried: the carbon materials after the coating processing of surface being placed on 10~80 DEG C of drying, are done in clean room
Dry processing；
(5) pre-sintering is handled: under the conditions of atmosphere or protective atmosphere, the carbon materials after coating and drying process being put into
In resistance furnace, it is warming up to 240-700 DEG C with the rate less than 10 DEG C/min, 20-300 minutes are kept the temperature, in carbon materials surface shape
At coating；
(6) operating process of step (3)-step (5) is repeated, until the coating on carbon materials surface reaches required thickness；
(7) in-situ reducing-carburizing reagent: will be pre-sintered that treated that carbon materials are put into vacuum drying oven, be evacuated in furnace true
Reciprocal of duty cycle is less than 5 × 10-1After Pa, after being warming up to 1000~1450 DEG C with the rate lower than 20 DEG C/min and keep the temperature 2~48 hours, very
It is furnace-cooled to room temperature under empty condition, completes in-situ reducing-carburizing reagent, the nanometer of growth in situ is finally obtained on carbon materials surface
Carbide coating；
Reducing agent used in the in-situ reducing-carburizing reagent is carbon, and the source of carbon is to adulterate in colloidal sol or gel
Organic matter cracks remaining carbon under the high temperature conditions；
The nano-carbide coating with a thickness of 10~20nm.
2. the method that carbon materials surface in situ according to claim 1 generates nano-carbide coating, it is characterised in that:
Carbon materials described in step (2) are one or more of carbon fiber, graphite, diamond and multi-walled carbon nanotube.
3. the method that carbon materials surface in situ according to claim 1 generates nano-carbide coating, it is characterised in that:
The group of the nano-carbide coating becomes titanium carbide, silicon carbide, chromium carbide, vanadium carbide, zirconium carbide, niobium carbide, tantalum carbide, carbon
Change one or more of molybdenum, tungsten carbide and carbonization rhenium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610133960.4A CN107176604B (en) | 2016-03-10 | 2016-03-10 | A kind of method that carbon materials surface in situ generates nano-carbide coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610133960.4A CN107176604B (en) | 2016-03-10 | 2016-03-10 | A kind of method that carbon materials surface in situ generates nano-carbide coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107176604A CN107176604A (en) | 2017-09-19 |
| CN107176604B true CN107176604B (en) | 2019-08-02 |
Family
ID=59829995
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610133960.4A Active CN107176604B (en) | 2016-03-10 | 2016-03-10 | A kind of method that carbon materials surface in situ generates nano-carbide coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107176604B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217629B (en) * | 2017-12-29 | 2019-07-23 | 西安理工大学 | A kind of preparation method of the compound CNTs of surface in situ generation nano SiC |
| CN109940162B (en) * | 2019-04-30 | 2020-05-22 | 西安理工大学 | Preparation method of titanium carbide in-situ reinforced titanium and titanium alloy stent |
| CN110304628A (en) * | 2019-08-12 | 2019-10-08 | 南昌航空大学 | A method of controllable nano silica is prepared in diamond surface |
| CN111732448A (en) * | 2020-06-16 | 2020-10-02 | 璨隆科技发展有限公司 | Graphite crucible and preparation method thereof |
| TWI824212B (en) * | 2020-12-18 | 2023-12-01 | 遠東科技大學 | Method for forming carbide film on surface of graphite substrate |
| CN112661507A (en) * | 2021-01-11 | 2021-04-16 | 湖南省美程陶瓷科技有限公司 | Alumina ceramic material for dual-function pressure sensor and preparation method thereof |
| CN114455586B (en) * | 2022-02-22 | 2024-03-19 | 合肥工业大学 | W (W) 2 Rapid preparation method of C nano-particles |
| CN114907144B (en) * | 2022-06-06 | 2023-04-18 | 吉林联科特种石墨材料有限公司 | Method for preparing SiC-C composite high-temperature coating by one-step method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1435503A (en) * | 2002-01-28 | 2003-08-13 | 西北工业大学 | Carbide coating of enhancing carbon/copper interface binding characteristic, and process thereof |
| CN101585534A (en) * | 2009-06-18 | 2009-11-25 | 西安交通大学 | Sol-gel method-based method for preparing composite nano diamond thin films |
| CN101792331A (en) * | 2010-01-04 | 2010-08-04 | 北京科技大学 | Microwave preparation method of anti-oxidation coating made of carbon-based material |
| CN102560291A (en) * | 2010-12-17 | 2012-07-11 | 中国科学院金属研究所 | Preparation method of metal-based composite material reinforcement surface nano coating |
| CN102677031A (en) * | 2012-05-18 | 2012-09-19 | 中国科学院上海硅酸盐研究所 | Metal/carbon nano composite porous membrane and preparation method thereof |
| CN103643481A (en) * | 2013-10-24 | 2014-03-19 | 上海交通大学 | Preparation method of alumina coating layer on carbon fiber surface |
-
2016
- 2016-03-10 CN CN201610133960.4A patent/CN107176604B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1435503A (en) * | 2002-01-28 | 2003-08-13 | 西北工业大学 | Carbide coating of enhancing carbon/copper interface binding characteristic, and process thereof |
| CN101585534A (en) * | 2009-06-18 | 2009-11-25 | 西安交通大学 | Sol-gel method-based method for preparing composite nano diamond thin films |
| CN101792331A (en) * | 2010-01-04 | 2010-08-04 | 北京科技大学 | Microwave preparation method of anti-oxidation coating made of carbon-based material |
| CN102560291A (en) * | 2010-12-17 | 2012-07-11 | 中国科学院金属研究所 | Preparation method of metal-based composite material reinforcement surface nano coating |
| CN102677031A (en) * | 2012-05-18 | 2012-09-19 | 中国科学院上海硅酸盐研究所 | Metal/carbon nano composite porous membrane and preparation method thereof |
| CN103643481A (en) * | 2013-10-24 | 2014-03-19 | 上海交通大学 | Preparation method of alumina coating layer on carbon fiber surface |
Non-Patent Citations (2)
| Title |
|---|
| "Improvement of interface between Al and short carbon fibers by a-Al2O3 coatings deposited by sol–gel technology";Yiping Tang et al;《Ceramics International》;20070810;第34卷;第1787–1790页 * |
| Preparation of anti-oxidative SiC/SiO2 coating on carbon fibers from vinyltriethoxysilane by sol–gel method;Kedong Xia et al;《Applied Surface Science》;20121123;第265卷;第603-609页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107176604A (en) | 2017-09-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107176604B (en) | A kind of method that carbon materials surface in situ generates nano-carbide coating | |
| JP6954685B2 (en) | Silicon Carbide Fiber Reinforced Silicon Carbide Composite | |
| AU2010321534B2 (en) | Ceramic composite materials containing carbon nanotube-infused fiber materials and methods for production thereof | |
| CN110256082B (en) | Method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite material by reaction sintering | |
| Cheng et al. | A SiCnw/PyC-toughened ZrB2-SiC coating for protecting Si-SiC coated C/C composites against oxidation | |
| CN108484190B (en) | Preparation method of carbon fiber reinforced multiphase carbide ceramic matrix composite | |
| Jiang et al. | Oxidation protective ZrB2-MoSi2-SiC-Si coating for graphite materials prepared by slurry dipping and vapor silicon infiltration | |
| EP2470472B1 (en) | Composite materials containing aligned nanotubes and the production thereof | |
| CN104975201A (en) | Nanocarbon-reinforced aluminium composite materials and method for manufacturing the same | |
| Li et al. | In situ synthesis of SiC nanowire porous layer on carbon/carbon composites | |
| CN110304932B (en) | Preparation method of Cf/SiC composite material with HfB2 interface | |
| Xin et al. | Anti-oxidation behavior of chemical vapor reaction SiC coatings on different carbon materials at high temperatures | |
| Tian et al. | Preparation and ablation properties of SiC nanowire-reinforced ZrC–SiC coating-matrix integrated C/C composites | |
| Abdollahi et al. | High temperature anti‐oxidation behavior of in situ and ex situ nanostructured C/SiC/ZrB2‐SiC gradient coatings: Thermodynamical evolution, microstructural characterization, and residual stress analysis | |
| JPH10505053A (en) | Boron nitride | |
| Xu et al. | High-quality SiC-HfC coating with interpenetrating structure based on a two-step low temperature molten salt method | |
| Vilatela et al. | A spray pyrolysis method to grow carbon nanotubes on carbon fibres, steel and ceramic bricks | |
| CN106631161A (en) | Method for preparing high-temperature oxidation resistant composite coating on surface of carbon-based material | |
| CN112299882B (en) | In-situ preparation method of HfC-based ternary carbide gradient coating on surface of carbon material | |
| CN117534495A (en) | Method for preparing ceramic matrix composite by combining precursor dipping, cracking and reaction infiltration | |
| JP5263980B2 (en) | REINFORCING FIBER MATERIAL, FIBER-REINFORCED CERAMIC COMPOSITE MATERIAL USING THE SAME, AND METHOD FOR PRODUCING THEM. | |
| CN107311685A (en) | The preparation method of electrophoresis and thermal evaporation techniques fabricated in situ refractory carbide nano wire | |
| CN105669231A (en) | Preparation method of carbon fiber reinforced MoSi2-SiC ceramic matrix composite | |
| Kenawy | Synthesis and characterization of aluminum borate ceramic whiskers | |
| CN111850498B (en) | Carbon nanofiber reinforced nickel-based composite coating and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |