CN113430613A - Method for preparing ceramic coating on inner surface and outer surface of complex special-shaped component - Google Patents
Method for preparing ceramic coating on inner surface and outer surface of complex special-shaped component Download PDFInfo
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- CN113430613A CN113430613A CN202110673450.7A CN202110673450A CN113430613A CN 113430613 A CN113430613 A CN 113430613A CN 202110673450 A CN202110673450 A CN 202110673450A CN 113430613 A CN113430613 A CN 113430613A
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- 238000005524 ceramic coating Methods 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000003792 electrolyte Substances 0.000 claims abstract description 58
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 31
- 239000010439 graphite Substances 0.000 claims abstract description 31
- 230000008569 process Effects 0.000 claims abstract description 12
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 73
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- 238000001035 drying Methods 0.000 claims description 36
- 238000004140 cleaning Methods 0.000 claims description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 229910052751 metal Inorganic materials 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 20
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 13
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-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
- 239000002105 nanoparticle Substances 0.000 claims description 12
- 150000003839 salts Chemical class 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 9
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 9
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 8
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical group [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 7
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 239000002923 metal particle Substances 0.000 claims description 7
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 7
- 229910003470 tongbaite Inorganic materials 0.000 claims description 7
- 229910001297 Zn alloy Inorganic materials 0.000 claims description 6
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 6
- GVEHJMMRQRRJPM-UHFFFAOYSA-N chromium(2+);methanidylidynechromium Chemical compound [Cr+2].[Cr]#[C-].[Cr]#[C-] GVEHJMMRQRRJPM-UHFFFAOYSA-N 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 4
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 4
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 4
- 229910001093 Zr alloy Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 4
- 229910000347 yttrium sulfate Inorganic materials 0.000 claims description 4
- RTAYJOCWVUTQHB-UHFFFAOYSA-H yttrium(3+);trisulfate Chemical compound [Y+3].[Y+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RTAYJOCWVUTQHB-UHFFFAOYSA-H 0.000 claims description 4
- 229910000599 Cr alloy Inorganic materials 0.000 claims description 3
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 3
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000788 chromium alloy Substances 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 2
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 2
- 238000005536 corrosion prevention Methods 0.000 abstract 1
- 238000000576 coating method Methods 0.000 description 20
- 239000011248 coating agent Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 14
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 239000002131 composite material Substances 0.000 description 10
- 239000000758 substrate Substances 0.000 description 8
- 238000007664 blowing Methods 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 7
- 238000004506 ultrasonic cleaning Methods 0.000 description 7
- 229910052593 corundum Inorganic materials 0.000 description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 description 6
- 229910000619 316 stainless steel Inorganic materials 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052961 molybdenite Inorganic materials 0.000 description 2
- 229910052574 oxide ceramic Inorganic materials 0.000 description 2
- 239000011224 oxide ceramic Substances 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910010038 TiAl Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910000711 U alloy Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- 238000000231 atomic layer deposition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
- C25D9/10—Electrolytic coating other than with metals with inorganic materials by cathodic processes on iron or steel
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/02—Electrophoretic coating characterised by the process with inorganic material
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/12—Electrophoretic coating characterised by the process characterised by the article coated
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/42—Electroplating: Baths therefor from solutions of light metals
- C25D3/44—Aluminium
Abstract
A method for preparing ceramic coatings on the inner surface and the outer surface of a complex special-shaped component is characterized in that the complex special-shaped component is placed into electrolyte, a graphite plate is used as a positive electrode, the complex special-shaped component is used as a negative electrode, electrolysis is carried out for 5-120 min in the electrolyte at 10-70 ℃ under the conditions that the pulse voltage is 200-1000V, the working frequency is 50-2000 Hz, and the duty ratio is 5-50%, and a ceramic coating is formed on the surface of the complex special-shaped component. The method has the advantages of low equipment cost, easy adjustment of process parameters, good corrosion resistance and wear resistance of the prepared ceramic coating, short required time, good repeatability and easy realization of automation and mass production. The invention is applied to the field of wear resistance, friction reduction and corrosion prevention.
Description
Technical Field
The invention relates to the field of metal surface modification, in particular to a method for preparing a ceramic coating on the inner surface and the outer surface of a complex special-shaped component.
Background
The functional protection of the complex special-shaped component is always a difficult point and a hot point problem in the field of surface science and engineering. The ceramic coating has extremely high hardness and good wear resistance and corrosion resistance, so that the member can be well protected if a layer of ceramic coating is prepared on the surface of the member.
At present, a plurality of methods for preparing ceramic coatings exist, but the coating preparation of some special-shaped parts and components with complex structures is difficult. The traditional physical vapor deposition has the advantages that the number of particles which can enter the inner surface of a complex cavity is limited, and the film is difficult to form; the chemical vapor deposition has poor plating property and is only suitable for components with low complexity; the deposition period of the film layer prepared by atomic layer deposition is too long, and the internal stress between layers is large, so that the deposition of the film layer with the micron-scale or above is difficult to realize. Although the traditional micro-arc oxidation can prepare ceramic coatings on special-shaped pieces, the traditional micro-arc oxidation is limited by base materials, is only suitable for valve metals such as aluminum, magnesium, titanium and the like and alloys thereof, and has no effect on materials such as iron, iron alloys and the like which are not valve metals. Although the sol-gel method can also form an integral ceramic layer in the cavity, the solvent evaporation of the film layer in the later heat treatment drying process can generate residual stress, which easily causes a large amount of microcracks to appear on the coating, and leads to poor coating quality.
Chinese patent CN107557836A discloses a method for preparing CeO by cathode micro-arc plasma electrolytic deposition on the surface of TiAl alloy2-Al2O3The method for compounding the ceramic coating needs micro-arc oxidation of a substrate, has complex process, and is not suitable for materials which are not valve metals, such as steel materials and the like.
Chinese patent CN1327091A discloses a cathode micro-arc electrodeposition method for preparing oxide ceramic coating, but the method needs to prefabricate film in advance, the process is complex, and in addition, the preparation time is long, and it takes several hours.
Chinese patent CN105132982A discloses a preparation method of a ceramic coating on the surface of uranium and uranium alloy, but the method has poor repeatability of the prepared coating by controlling current density. Moreover, the method is suitable for simple components, and the effect of preparing the ceramic coating by grafting the ceramic coating on the inner surface and the outer surface of the complex special-shaped component is not ideal, so that a method suitable for the complex special-shaped component needs to be searched in a targeted manner. In addition, the above methods can only produce oxide ceramics, and cannot produce composite coatings containing carbides, sulfides, graphite, metals, or the like.
Therefore, the existing method for preparing the ceramic coating on the inner surface and the outer surface of the complex special-shaped component has a plurality of problems. E.g., difficulty in producing thicker ceramic coatings, limitations on the substrate material, poor quality of the ceramic film layer produced, etc.
Disclosure of Invention
The invention aims to solve the problems that the existing method is difficult to prepare thicker ceramic coatings on the inner and outer surfaces of a complex special-shaped component, is limited by a base material, and the prepared ceramic film layer has poor quality, and the like, and provides a method for preparing ceramic coatings on the inner and outer surfaces of the complex special-shaped component.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing ceramic coatings on the inner and outer surfaces of a complex special-shaped component comprises the steps of putting the complex special-shaped component into electrolyte, connecting the component into a pulse power supply, electrolyzing the component for 5-120 min in the electrolyte at 10-70 ℃ under the conditions that pulse voltage is 200-1000V, working frequency is 50-2000 Hz and duty ratio is 5-50% and forming the ceramic coatings on the surface of the complex special-shaped component by taking a graphite plate as a positive electrode and taking the complex special-shaped component as a negative electrode.
The invention is further improved in that the following processes are carried out before the complex special-shaped component is put into the electrolyte: and ultrasonically cleaning the complex special-shaped component by using acetone and alcohol, and then drying.
The invention is further improved in that the complex special-shaped component is made of iron, iron alloy, copper alloy, nickel alloy, chromium alloy, aluminum alloy, titanium alloy, magnesium alloy, zinc alloy, zirconium or zirconium alloy.
In a further development of the invention, the electrolyte is prepared by the following process: adding a metal salt into an ethanol solution to obtain an electrolyte, wherein the concentration of the metal salt is 0.2-1.5 mol/L; the volume fraction of water in the ethanol solution is 0-100%.
The invention is further improved in that the metal salt is one or more of nitrate, carbonate, sulfate and chloride of Zr, Al, Ce and Y.
In a further development of the invention, the metal salt is zirconium nitrate, aluminum nitrate, cerium nitrate, yttrium nitrate, zirconium sulfate, aluminum sulfate, cerium sulfate, yttrium sulfate, zirconium chloride, cerium chloride or yttrium chloride.
The further improvement of the invention is that the electrolyte also comprises oxide particles, carbide particles, sulfide particles, graphite particles or metal particles; the concentration of oxide particles, carbide particles, sulfide particles, graphite particles or metal particles in the electrolyte is 1 to 200 g/L.
The further improvement of the invention is that the oxide particles are micron-sized or nano-sized alumina, titanium oxide or zirconium oxide particles, the carbide particles are micron-sized or nano-sized silicon carbide, chromium carbide or tungsten carbide particles, the sulfide particles are micron-sized or nano-sized iron sulfide or molybdenum disulfide particles, the graphite particles are micron-sized or nano-sized graphite particles, and the metal particles are micron-sized or nano-sized silver, copper or aluminum particles.
The invention has the further improvement that the electrolysis is carried out for 10-100 min under the conditions that the pulse voltage is 250-800V, the working frequency is 200-1800 Hz and the duty ratio is 5-45%.
Compared with the prior art, the invention has the following beneficial effects:
the whole process of the method is carried out in the electrolyte environment, and the electrolyte is in a liquid phase environment, so that the ceramic coating can be formed on the inner surface and the outer surface of any complex special-shaped component. The invention has good universality to base materials, is almost suitable for all metals, requires simple main equipment, only needs one power supply, has very simple operation, does not need vacuum or atmosphere protection in the production process, and has low cost. The method is carried out under the high voltage with the pulse voltage of 200-1000V, plasma is generated on the surface of the component in the treatment process, the deposit on the surface of the cathode component can be sintered to form a ceramic film layer, and the participation of the plasma can enable the prepared ceramic coating to have excellent performance, such as Rockwell hardness up to thousands HV. The method of the invention has the advantages of easy adjustment of process parameters, capability of adjusting the process parameters (voltage, frequency, duty ratio, electrolysis time and the like) and conveniently controlling the structure and the thickness of the ceramic coating, simple equipment operation and easy realization of large-scale production and automation. The invention has the advantages of low equipment cost, easy adjustment of process parameters, good corrosion resistance and wear resistance of the prepared ceramic coating, short required time, good repeatability, easy realization of automation and mass production, and application in the fields of wear resistance, friction reduction and corrosion resistance.
Furthermore, the electrolyte of the method is easy to adjust, the components and concentration of metal salt and the mixture of a plurality of metal salts can be selected according to the required ceramic coating, and a plurality of solid particle modified coatings can be added according to the requirement, so that the components and the performance of the obtained coating can be conveniently controlled.
Furthermore, the silicon carbide particles are added in the invention, and because the silicon carbide is a semiconductor, the discharge behavior in the coating preparation process can be changed, so that the coating structure is compact, and the silicon carbide is a substance with high hardness, and the hardness and the wear resistance of the coating can be improved after entering the coating. Various solid particles have the characteristics, and the particles can be added according to the requirements to regulate and control the components and the performance of the coating.
Drawings
FIG. 1 shows Al prepared in example 12O3SEM image of the surface of the ceramic coating;
FIG. 2 shows Al prepared in example 12O3SEM image of the cross section of the ceramic coating;
FIG. 3 shows Al prepared in example 22O3Ceramic coating XRD pattern;
FIG. 4 is a graph showing the polarization of a 316 stainless steel substrate in example 2;
FIG. 5 shows Al prepared in example 22O3Polarization curve of ceramic coating.
FIG. 6 is an SEM image of the surface of a ceramic coating prepared by adding SiC particles in example 3.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
A method for preparing ceramic coatings on the inner and outer surfaces of a complex special-shaped component is carried out according to the following steps:
firstly, preprocessing a complex special-shaped component: and (3) putting the complex special-shaped component into an industrial ultrasonic machine, cleaning the complex special-shaped component completely, respectively adopting acetone and alcohol to carry out ultrasonic cleaning for 20min, and then putting the complex special-shaped component into a blowing type drying oven to dry. The complex special-shaped component is made of iron, iron alloy, copper alloy, nickel alloy, chromium alloy, aluminum alloy, titanium alloy, magnesium alloy, zinc alloy, zirconium or zirconium alloy and the like.
Secondly, preparing electrolyte: selecting corresponding metal salt as a solute for a ceramic coating to be prepared, adding a certain amount of other solid particles, and preparing an electrolyte by using an ethanol solution containing 0-100% of water by volume as a solvent, wherein the concentration of the metal salt in the electrolyte is 0.2-1.5 mol/L, and the concentration of the solid particles is 1-200 g/L; the electrolyte can be one or more of metal salt solutions or two or more of metal salt solutions mixed according to a certain proportion. The solid particles are micron-sized or nano-sized oxide particles of aluminum oxide, titanium oxide, zirconium oxide and the like, carbide particles of silicon carbide, chromium carbide, tungsten carbide and the like, sulfide particles of iron sulfide, molybdenum disulfide and the like, graphite particles or metal particles of silver, copper, aluminum and the like. .
Thirdly, electrolysis process parameters: putting the complex special-shaped component pretreated in the first step into electrolyte, connecting a pulse power supply, taking a graphite plate as a positive electrode and taking the complex special-shaped component as a negative electrode, and electrolyzing for 5-120 min under the conditions that the temperature of the electrolyte is 10-70 ℃, the pulse voltage is 200-1000V, the working frequency is 50-2000 Hz, and the duty ratio is 5-50%;
preferably, the electrolysis is carried out for 10-100 min under the conditions that the temperature of the electrolyte is 25-50 ℃, the pulse voltage is 250-800V, the working frequency is 200-1800 Hz, and the duty ratio is 5-45%.
And fourthly, taking the complex special-shaped component treated in the third step, washing the complex special-shaped component for 3-5 times by using deionized water, washing away residual electrolyte, and drying the complex special-shaped component by using a blower to obtain the ceramic coating.
Example 1
Firstly, putting a 45# steel complex special-shaped component into an industrial ultrasonic machine, cleaning the component cleanly, respectively ultrasonically cleaning the component for 20min by using acetone and alcohol, and then putting the component into a blast type drying oven for drying;
then, Al (NO) is added3)·9H2Adding O into an ethanol solution (absolute ethanol) with the water volume fraction of 0%, and adding micron-grade alumina particles to prepare an electrolyte; wherein Al (NO)3)·9H2The concentration of O was 0.8mol/L and the concentration of alumina fine particles was 15 g/L.
Putting the dried complex special-shaped component into electrolyte, taking the complex special-shaped component as a cathode and a graphite plate as an anode, electrolyzing the complex special-shaped component at the temperature of 20 ℃ for 50min by using the complex special-shaped component as a cathode and a graphite plate as an anode, cleaning the complex special-shaped component by using deionized water, and drying to obtain the Al2O3And (3) coating the ceramic.
As can be seen from FIG. 1, the surface morphology of the coating obtained by the present embodiment shows porosity and roughness, the surface has many dark holes, the size of the holes is micron, and there are many crater morphologies formed by the plasma action.
As can be seen from fig. 2, the cross-sectional thickness of the coating prepared was about 110 μm, and the coating and the substrate were canine-interdigitated and bonded very well. In addition, the spectral analysis found Al and OThe ratio is close to 2:3, which shows that the ceramic coating is mainly composed of Al2O3And (4) forming. Through a hardness test, Al is measured2O3The hardness of the ceramic coated specimens was 1350HV, while the stainless steel substrate was approximately 275 HV.
Example 2
Firstly, putting a complex special-shaped component made of 316 stainless steel into an industrial ultrasonic machine, cleaning the component cleanly, respectively ultrasonically cleaning the component for 20min by using acetone and alcohol, and then putting the component into a blast type drying oven for drying;
then, adding Al2(SO4)3Adding into ethanol solution with water volume fraction of 20%, and adding nanometer alumina particles to obtain electrolyte, wherein Al is2(SO4)3The concentration of (2) is 1mol/L and the concentration of the alumina fine particles is 5 g/L.
Putting the dried complex special-shaped component into electrolyte, taking the complex special-shaped component as a cathode and a graphite plate as an anode, electrolyzing for 80min in the electrolyte with the pulse voltage of 500V, the working frequency of 700Hz and the duty ratio of 10 percent, finally cleaning and drying by deionized water to obtain Al2O3And (3) coating the ceramic.
As can be seen from FIG. 3, the phase of the ceramic coating obtained in the present embodiment is alpha-Al2O3And gamma-Al2O3Two kinds of, wherein alpha-Al2O3Is the main phase.
As can be seen from a comparison of fig. 4 and 5, the corrosion current density of the coated coupon is less than that of the 316 stainless steel substrate, and the corrosion potential is higher than that of the 316 stainless steel substrate, indicating that the corrosion resistance of the resulting ceramic coating to the 316 stainless steel substrate is greatly improved.
Example 3
Firstly, putting a complex special-shaped component made of pure Al materials into an industrial ultrasonic machine, cleaning the component cleanly, respectively ultrasonically cleaning the component for 20min by using acetone and alcohol, and then putting the component into a blast type drying oven for drying;
then, Al (NO) is added3)·9H2Adding O into ethanol solution with water volume fraction of 35%, and adding micrometer-scale silicon carbide particles to obtain electrolyte, wherein Al (NO) is3)·9H2The concentration of O is 0.5mol/L, and the concentration of silicon carbide particles is 35 g/L;
putting the dried complex special-shaped component into electrolyte, taking the complex special-shaped component as a cathode and a graphite plate as an anode, electrolyzing for 30min in the electrolyte with the pulse voltage of 550V, the working frequency of 700Hz and the duty ratio of 18 percent, finally cleaning and drying by deionized water to obtain Al2O3+ SiC composite ceramic coating.
As can be seen from fig. 6, the surface appearance of the coating obtained in the present example was relatively flat, and SiC particles were observed on the surface of the coating. The roughness of the coating was found to be 10.2 μm in surface roughness Ra without the addition of SiC particles and 2.78 μm in surface roughness Ra after the addition of SiC particles, and the surface state was significantly improved.
Example 4
Firstly, putting a complex special-shaped component made of TC4 titanium alloy material into an industrial ultrasonic machine, cleaning the complex special-shaped component by ultrasonic cleaning for 20min respectively by acetone and alcohol, and then putting the complex special-shaped component into a blowing type drying oven for drying;
then, Al (NO) is added3)·9H2O and Zr (NO)3)4·6H2Adding O into ethanol solution with water volume fraction of 35%, and adding nanometer molybdenum disulfide particles to obtain electrolyte, wherein Al (NO)3)·9H2Concentration of O is 0.5mol/L, Zr (NO)3)4·6H2The concentration of O is 0.2mol/L, and the concentration of molybdenum disulfide particles is 5 g/L;
putting the dried complex special-shaped component into electrolyte, taking the complex special-shaped component as a cathode and a graphite plate as an anode, electrolyzing for 30min in the electrolyte with the pulse voltage of 550V, the working frequency of 700Hz and the duty ratio of 18 percent, finally cleaning and drying by deionized water to obtain Al2O3+ZrO2+MoS2And (3) composite ceramic coating.
Example 5
Firstly, putting a complex special-shaped component made of Zr4 zirconium alloy into an industrial ultrasonic machine, cleaning the component cleanly, respectively ultrasonically cleaning the component for 20min by using acetone and alcohol, and then putting the component into a blowing type drying oven for drying;
then, Zr (NO)3)4·6H2Adding O into water, and adding micron-sized silver particles to obtain electrolyte, wherein Zr (NO)3)4·6H2The concentration of O was 0.8mol/L and the concentration of silver particles was 10 g/L.
Putting the dried complex special-shaped component into electrolyte, taking the complex special-shaped component as a cathode and a graphite plate as an anode, electrolyzing for 90min in the electrolyte with the pulse voltage of 550V, the working frequency of 650Hz and the duty ratio of 35 percent, finally cleaning and drying by deionized water to obtain ZrO2+ Ag composite ceramic coating.
Example 6
Firstly, putting a complex special-shaped component made of a pure copper material into an industrial ultrasonic machine, cleaning the complex special-shaped component cleanly, respectively ultrasonically cleaning the complex special-shaped component for 20min by adopting acetone and alcohol, and then putting the complex special-shaped component into a blast type drying box for drying;
then, adding zirconium nitrate into an ethanol solution with the water volume fraction of 10%, and adding micron-sized titanium oxide particles to prepare an electrolyte; wherein the concentration of zirconium nitrate is 0.2mol/L and the concentration of titanium oxide fine particles is 1 g/L.
Putting the dried complex special-shaped component into electrolyte, taking the complex special-shaped component as a cathode and a graphite plate as an anode, electrolyzing the complex special-shaped component at 25 ℃ for 120min by using the complex special-shaped component as a cathode and a graphite plate as an anode under the conditions that the pulse voltage is 250V, the working frequency is 1000Hz and the duty ratio is 5 percent, and finally cleaning and drying the complex special-shaped component by using deionized water to obtain ZrO2+TiO2And (3) composite ceramic coating.
Example 7
Firstly, putting a nickel alloy Ni7N material complex special-shaped component into an industrial ultrasonic machine, cleaning the component cleanly, respectively adopting acetone and alcohol to carry out ultrasonic cleaning for 20min, and then putting the component into a blowing type drying oven to dry;
then, adding cerium nitrate into an ethanol solution with the water volume fraction of 70%, and adding micron-sized chromium carbide particles to prepare an electrolyte; wherein the concentration of the cerium nitrate is 0.5mol/L, and the concentration of the chromium carbide particles is 200 g/L.
Putting the dried complex special-shaped component into electrolyteIn the method, a complex special-shaped structural member is used as a cathode, a graphite plate is used as an anode, the pulse voltage is 200V, the working frequency is 1800Hz, the duty ratio is 40%, electrolysis is carried out for 100min in an electrolyte at 50 ℃, and finally, deionized water is used for cleaning and drying to obtain CeO2+Cr3C2And (3) composite ceramic coating.
Example 8
Firstly, putting a complex special-shaped component made of an aluminum alloy 7A04 material into an industrial ultrasonic machine, cleaning the component cleanly, respectively adopting acetone and alcohol to carry out ultrasonic cleaning for 20min, and then putting the component into a blowing type drying oven to dry;
then, adding yttrium nitrate into an ethanol solution (absolute ethanol) with the water volume fraction of 0%, and adding micron-sized iron sulfide particles to prepare an electrolyte; wherein the concentration of yttrium nitrate is 0.7mol/L, and the concentration of iron sulfide particles is 50 g/L.
Putting the dried complex special-shaped component into electrolyte, taking the complex special-shaped component as a cathode and a graphite plate as an anode, electrolyzing the complex special-shaped component at 10 ℃ for 80min by using a pulse voltage of 1000V, a working frequency of 50Hz and a duty ratio of 50 percent, and finally cleaning and drying the complex special-shaped component by using deionized water to obtain Y2O3+Fe2S3And (3) composite ceramic coating.
Example 9
Firstly, putting a complex special-shaped component made of zinc alloy ZA27 into an industrial ultrasonic machine, cleaning the component by ultrasonic cleaning for 20min respectively by using acetone and alcohol, and then putting the component into a blowing type drying oven for drying;
then adding yttrium sulfate into an ethanol solution with the water volume fraction of 80%, and adding micron-sized molybdenum disulfide particles to prepare an electrolyte; wherein the concentration of the yttrium sulfate is 1mol/L, and the concentration of the molybdenum disulfide particles is 100 g/L.
Putting the dried complex special-shaped component into electrolyte, taking the complex special-shaped component as a cathode and a graphite plate as an anode, electrolyzing the complex special-shaped component at 30 ℃ for 50min by using the complex special-shaped component as a cathode and a graphite plate as an anode at a pulse voltage of 800V and a working frequency of 2000Hz with a duty ratio of 10 percent, and finally cleaning and drying the complex special-shaped component by using deionized water to obtain Y2O3+MoS2And (3) composite ceramic coating.
Example 10
Firstly, putting a complex special-shaped component made of zinc alloy ZA43 into an industrial ultrasonic machine, cleaning the component by ultrasonic cleaning for 20min respectively by using acetone and alcohol, and then putting the component into a blowing type drying oven for drying;
then, adding cerium chloride into an ethanol solution (absolute ethanol) with the water volume fraction of 60%, and adding micron-sized graphite particles to prepare an electrolyte; wherein the concentration of cerium chloride is 1.5mol/L, and the concentration of graphite particles is 150 g/L.
Putting the dried complex special-shaped component into electrolyte, taking the complex special-shaped component as a cathode and a graphite plate as an anode, electrolyzing the complex special-shaped component at 40 ℃ for 10min by using the electrolyte with the pulse voltage of 500V, the working frequency of 200Hz and the duty ratio of 20 percent, and finally cleaning and drying the complex special-shaped component by using deionized water to obtain CeO2+ C composite ceramic coating.
Example 11
The difference from the example 10 is that micron-sized chromium carbide particles are added to prepare the electrolyte.
Example 12
The difference from the example 10 is that micron-sized tungsten carbide particles are added to prepare the electrolyte.
Example 13
Firstly, putting a complex special-shaped component made of zinc alloy ZA303 into an industrial ultrasonic machine, cleaning the complex special-shaped component by ultrasonic cleaning for 20min respectively by using acetone and alcohol, and then putting the complex special-shaped component into a blast type drying oven for drying;
then, adding cerium chloride into an ethanol solution (absolute ethanol) with the water volume fraction of 60%, and adding nano-silver particles to prepare an electrolyte; wherein the concentration of cerium chloride is 1.3mol/L, and the concentration of silver particles is 70 g/L.
Putting the dried complex special-shaped component into electrolyte, taking the complex special-shaped component as a cathode and a graphite plate as an anode, electrolyzing the complex special-shaped component at the temperature of 20 ℃ for 5min by using the complex special-shaped component as a cathode and a graphite plate as an anode, and finally cleaning and drying the complex special-shaped component by using deionized water to obtain CeO2+ Ag composite ceramic coating.
Example 14
The difference from example 14 is that the electrolyte is prepared by adding nano-copper particles.
Example 15
The difference from example 14 is that the electrolyte is prepared by adding nano-sized aluminum particles.
Claims (9)
1. A method for preparing ceramic coatings on the inner surface and the outer surface of a complex special-shaped component is characterized in that the complex special-shaped component is placed in electrolyte, the component is connected with a pulse power supply, a graphite plate is used as a positive electrode, the complex special-shaped component is used as a negative electrode, electrolysis is carried out for 5-120 min in the electrolyte at the temperature of 10-70 ℃ under the conditions that the pulse voltage is 200-1000V, the working frequency is 50-2000 Hz, and the duty ratio is 5-50%, and a ceramic coating is formed on the surface of the complex special-shaped component.
2. A method for preparing ceramic coatings on the inner and outer surfaces of a complex shaped component according to claim 1, characterized in that the following processes are carried out before the complex shaped component is put into the electrolyte: and ultrasonically cleaning the complex special-shaped component by using acetone and alcohol, and then drying.
3. The method of claim 1, wherein the complex shaped member is made of iron, iron alloy, copper alloy, nickel alloy, chromium alloy, aluminum alloy, titanium alloy, magnesium alloy, zinc alloy, zirconium or zirconium alloy.
4. The method for preparing the ceramic coating on the inner surface and the outer surface of the complex special-shaped component according to claim 1, wherein the electrolyte is prepared by the following steps: adding a metal salt into an ethanol solution to obtain an electrolyte, wherein the concentration of the metal salt is 0.2-1.5 mol/L; the volume fraction of water in the ethanol solution is 0-100%.
5. The method for preparing the ceramic coating on the inner surface and the outer surface of the complex special-shaped component according to claim 4, wherein the metal salt is one or more of nitrate, carbonate, sulfate and chloride of Zr, Al, Ce and Y.
6. The method of claim 4, wherein the metal salt is zirconium nitrate, aluminum nitrate, cerium nitrate, yttrium nitrate, zirconium sulfate, aluminum sulfate, cerium sulfate, yttrium sulfate, zirconium chloride, cerium chloride or yttrium chloride.
7. The method for preparing ceramic coating on inner and outer surfaces of complex special-shaped component according to claim 1, wherein the electrolyte further comprises oxide particles, carbide particles, sulfide particles, graphite particles or metal particles; the concentration of oxide particles, carbide particles, sulfide particles, graphite particles or metal particles in the electrolyte is 1 to 200 g/L.
8. The method of claim 7, wherein the oxide particles are micro-or nano-sized alumina, titania or zirconia particles, the carbide particles are micro-or nano-sized silicon carbide, chromium carbide or tungsten carbide particles, the sulfide particles are micro-or nano-sized iron sulfide or molybdenum disulfide particles, the graphite particles are micro-or nano-sized graphite particles, and the metal particles are micro-or nano-sized silver, copper or aluminum particles.
9. The method for preparing the ceramic coating on the inner surface and the outer surface of the complex special-shaped component according to claim 1, wherein the electrolysis is carried out for 10-100 min under the conditions that the pulse voltage is 250-800V, the working frequency is 200-1800 Hz, and the duty ratio is 5-45%.
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