CN111826687A - 一种不锈钢mim产品表面镀层的加工工艺 - Google Patents
一种不锈钢mim产品表面镀层的加工工艺 Download PDFInfo
- Publication number
- CN111826687A CN111826687A CN202010644344.1A CN202010644344A CN111826687A CN 111826687 A CN111826687 A CN 111826687A CN 202010644344 A CN202010644344 A CN 202010644344A CN 111826687 A CN111826687 A CN 111826687A
- Authority
- CN
- China
- Prior art keywords
- mim product
- product
- mim
- coating
- electroplating
- 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.)
- Pending
Links
- 239000011248 coating agent Substances 0.000 title claims abstract description 94
- 238000000576 coating method Methods 0.000 title claims abstract description 94
- 238000012545 processing Methods 0.000 title claims abstract description 16
- 239000010935 stainless steel Substances 0.000 title claims abstract description 16
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 16
- 238000005516 engineering process Methods 0.000 title claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 121
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 58
- 238000007747 plating Methods 0.000 claims abstract description 53
- 238000009713 electroplating Methods 0.000 claims abstract description 48
- 230000003213 activating effect Effects 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 238000002791 soaking Methods 0.000 claims abstract description 15
- 238000007789 sealing Methods 0.000 claims abstract description 14
- 238000007598 dipping method Methods 0.000 claims abstract description 12
- 238000007605 air drying Methods 0.000 claims abstract description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 6
- 239000010410 layer Substances 0.000 claims description 40
- -1 hydroxypropyl Chemical group 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 31
- 229910021389 graphene Inorganic materials 0.000 claims description 31
- 239000002270 dispersing agent Substances 0.000 claims description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 238000005406 washing Methods 0.000 claims description 26
- 239000003921 oil Substances 0.000 claims description 24
- 238000005240 physical vapour deposition Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 16
- 239000013527 degreasing agent Substances 0.000 claims description 15
- 238000005237 degreasing agent Methods 0.000 claims description 15
- 150000007522 mineralic acids Chemical class 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 238000006073 displacement reaction Methods 0.000 claims description 14
- 239000000565 sealant Substances 0.000 claims description 14
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 11
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims description 11
- 239000001509 sodium citrate Substances 0.000 claims description 11
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 239000004698 Polyethylene Substances 0.000 claims description 10
- 229920000573 polyethylene Polymers 0.000 claims description 10
- 150000004756 silanes Chemical class 0.000 claims description 10
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 10
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 8
- 239000004115 Sodium Silicate Substances 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 8
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 8
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 8
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 claims description 8
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 8
- 238000007664 blowing Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 7
- BSWXAWQTMPECAK-UHFFFAOYSA-N 6,6-diethyloctyl dihydrogen phosphate Chemical class CCC(CC)(CC)CCCCCOP(O)(O)=O BSWXAWQTMPECAK-UHFFFAOYSA-N 0.000 claims description 5
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 5
- 229920000178 Acrylic resin Polymers 0.000 claims description 5
- 239000004925 Acrylic resin Substances 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 239000004743 Polypropylene Substances 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical class [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 239000001913 cellulose Chemical class 0.000 claims description 5
- 229920002678 cellulose Chemical class 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 5
- 230000005684 electric field Effects 0.000 claims description 5
- 239000000194 fatty acid Substances 0.000 claims description 5
- 229930195729 fatty acid Natural products 0.000 claims description 5
- 150000004665 fatty acids Chemical class 0.000 claims description 5
- QXLPXWSKPNOQLE-UHFFFAOYSA-N methylpentynol Chemical class CCC(C)(O)C#C QXLPXWSKPNOQLE-UHFFFAOYSA-N 0.000 claims description 5
- 230000000737 periodic effect Effects 0.000 claims description 5
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 5
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 229920001522 polyglycol ester Polymers 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 5
- 239000002356 single layer Substances 0.000 claims description 5
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 5
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 5
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 5
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 5
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 5
- 235000019794 sodium silicate Nutrition 0.000 claims description 5
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 239000013077 target material Substances 0.000 claims description 5
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims description 2
- 230000003014 reinforcing effect Effects 0.000 claims description 2
- 238000004659 sterilization and disinfection Methods 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 17
- 230000007797 corrosion Effects 0.000 abstract description 17
- 238000005238 degreasing Methods 0.000 abstract description 5
- 238000005868 electrolysis reaction Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 130
- 230000004913 activation Effects 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 9
- 238000005086 pumping Methods 0.000 description 7
- 239000007921 spray Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000007888 film coating Substances 0.000 description 3
- 238000009501 film coating Methods 0.000 description 3
- 238000007373 indentation Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 230000010358 mechanical oscillation Effects 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000003595 mist Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 230000010355 oscillation Effects 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 239000001488 sodium phosphate Substances 0.000 description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 3
- 238000013022 venting Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/085—Oxides of iron group metals
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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Abstract
本发明公开了一种不锈钢MIM产品表面镀层的加工工艺，包括以下工艺步骤:⑴热浸除油；⑵超声波清洗；⑶电解除油；⑷风干处理；⑸活化处理：将MIM产品放入到质量分数为15～20%的活化液中进行活化处理，活化处理的时间为60～120s；⑹预镀镍：将MIM产品放入到8～12波美度的镀镍溶液中，浸泡1～2min；⑺电镀镍：将MIM产品放入到4～6波美度的镀镍溶液中，在80～90℃的温度下进行电镀；⑻PVD镀膜：将MIM产品放入到镀膜室中，在真空度达到1～1.5MPa，温度达到160～165℃条件下进行PVD镀膜；⑼纳米封闭：将MIM产品放入封闭剂中浸泡3～5min。本发明能够在MIM产品的表面形成一层附着能力更大的高致密性PVD镀膜，让MIM产品具有较好的抗水、耐磨和耐腐蚀性能。
Description
技术领域
本发明属于粉末冶金表面处理技术领域，具体涉及一种不锈钢MIM产品表面镀层的加工工艺。
背景技术
MIM是一种将金属粉末与其粘结剂的增塑混合料注射于模型中的一种成形方法，其工艺步骤是选取符合要求的金属粉末和粘结剂，然后在一定温度下用适当的方法将粉末和粘结剂混合成均匀的喂料，经制粒后再通过模具注射成半成品，获得的半成品经脱脂、烧结后再经过后续的整形、钻孔和热处理等工序获得最终产品。采用上述方法制得的MIM产品具有组织均匀、致密度高、产品表面光洁度、尺寸精度高的优点，人们通常都采用MIM技术来制作结构复杂、体积小等薄型零部件。目前，采用上述方法制得的MIM产品在使用的过程中，因为与外界环境直接或者间接接触，其表面会存在腐蚀的现象，故在MIM产品整形后，需要在MIM产品的表面镀上一层保护膜。在现有的技术中，保护膜通常都是采用电镀的方式进行，电镀就是利用电解原理在MIM产品表面镀上一层其他金属或者合金的过程，理论上，电镀工艺可以提高MIM产品的耐磨性、抗腐蚀性和美观性，但在实际的操作过程中，由于电镀工艺的布置不合理，以及选用的电镀液等差异，使得电镀后的MIM产品保护膜容易脱落，耐磨性能差，尤其是在进行盐雾试验后，90%以上的产品盐雾试验能够达到24小时，抗腐蚀性能较差。因此，研制开发一种工艺简单、可操作性强、具体较好耐磨、耐腐蚀效果的不锈钢MIM产品表面镀层的加工工艺是客观需要的。
发明内容
为了解决背景技术中存在的问题，本发明的目的在于提供一种工艺简单、可操作性强、具有较好耐磨、耐腐蚀效果的不锈钢MIM产品表面镀层的加工工艺。
本发明所述的一种不锈钢MIM产品表面镀层的加工工艺，其特征在于,包括以下工艺步骤:
⑴热浸除油:将MIM产品放入温度为50～60℃的热浸除油剂中，浸泡170～200s；
⑵超声波清洗：将MIM产品从热浸除油剂中捞出后进行超声波水洗，超声清洗的水温为50～60℃，超声清洗的时间为150～200s，超声频率为30～40HZ；
⑶电解除油：将MIM产品放入温度为50～60℃的无机酸溶液中进行电解除油，无机酸溶液的质量浓度为50～80g/L，电解除油的时间为3～5min，电解除油的电压为3～5V；
⑷风干处理：将MIM产品放入用40～50℃的热水清洗30～60s，之后用压缩空气吹去MIM产品表面的水分，压缩空气的气压为0.1～0.2MPa；
⑸活化处理：将MIM产品放入到质量分数为15～20%的活化液中进行活化处理，活化处理的时间为60～120s；
⑹预镀镍：将MIM产品放入到8～12波美度的镀镍溶液中，浸泡1～2min；
⑺电镀镍：将MIM产品放入到4～6波美度的镀镍溶液中，在80～90℃的温度下进行电镀，让MIM产品的表面镀上一层镀镍层，镀镍层的厚度为0.1～0.2um，之后用压缩空气吹去MIM产品表面的水分，压缩空气的气压为0.1～0.2MPa；
⑻PVD镀膜：将MIM产品放入到镀膜室中，对镀膜室内进行抽真空和加热处理，使镀膜室内的真空度达到1～1.5MPa，镀膜室内的温度达到160～165℃之后，向镀膜室内通入氩气，然后开启靶源对MIM产品镀膜，靶源受电场和磁场的周期变化驱动，在磁控溅射与阴极电弧之间切换镀膜，待工件表面的PV镀膜厚度达到0.5～1.5μm后，停止镀膜，然后关闭靶源和所有电源，待镀膜室内的温度降至室温后，抽出室内的氩气，加强抽气5～10min，除去镀膜室内的残留的氩气后，将镀膜室内放空气至大气压，取出MIM产品；
⑼ 纳米封闭：将MIM产品放入封闭剂中浸泡3～5min，所述封闭剂包括以下重量份的原料：硅溶胶50～100份、改性硅烷10～20份、水溶性丙烯酸树脂25～60份、石墨烯3～5份、石墨烯分散剂3～5份和水30～70份，之后将MIM产品从封闭剂中取出后，置于烤箱中，在70～80℃的温度下烘烤30～40s，取出冷却至室温后即可得到MIM成品。
进一步的，在步骤⑸中，所述活化液包括以下质量百分比含量的组分：无机酸40～90%、氟化氢铵8～60%和过氧化氢1～3%。
进一步的，在步骤⑹和⑺中，所述镀镍溶液的配方为：氯化镍100～150g/L、氨基磺酸镍50～80 g/L、硼酸20～30 g/L、十二烷基苯磺酸钠0.01～0.02 g/L、柠檬酸钠20～30g/L、硫酸铵2～5 g/L、羟丙基走位剂0.1～0.15 g/L和PS试剂0.05～0.1 g/L。
进一步的，在步骤⑺中，电镀镍分三次进行，第一次电镀的电流密度为1～2A/dm2，第一次电镀的时间为1～2min，第二次电镀的电流密度3～5A/dm2，第二次电镀的时间为2～4min，第三次电镀的电流密度7～10A/dm2，第三次电镀的时间为3～4min，每次电镀结束后需采用喷淋的方式对MIM产品进行水洗，水洗的时间为2～3min。
进一步的，在步骤⑻中，靶源选用的靶材为Ni、NiO、TiO2、Sn或SnO2。
进一步的，在步骤⑼中，所述石墨烯为单层氧化纳米石墨烯、少层氧化纳米石墨烯和多层氧化纳米石墨烯中的至少一种；所述石墨烯分散剂包括无机分散剂和有机分散剂，所述无机分散剂为硅酸钠、三聚磷酸钠、六偏磷酸钠和焦磷酸钠中的至少一种，所述有机分散剂为三乙基己基磷酸、十二烷基硫酸钠、甲基戊醇、纤维素衍生物、古尔胶、脂肪酸聚乙二醇酯、聚乙烯醇、聚乙烯吡咯烷酮、聚丙烯酸钠和聚丙烯酰胺中的至少一种；所述改性硅烷为聚乙二醇-14二甲基硅氧烷、聚乙二醇/聚丙二醇-14/4-二甲基硅氧烷、聚乙二醇-6醋酸酯硅氧烷中的至少一种。
与现有技术相比，本发明的优点在于：一是本发明利用热浸、超声波和电解除油后能够彻底的去除产品表面的油污、锈渍等污物，二是在镀镍前利用活化液对产品进行活化处理，利用活化液的还原性，对除油的产品氧化层进行活化和清润，使氧化层松动，便于后续的镀镍处理，活化处理工序能在活化产品表面氧化层的同时，还可以修复产品表面的凹痕和损伤；三是利用镀镍溶液在产品的表面镀上一层镀镍层，镀镍层可以防止产品表面氧化，从而可以提高镀镍层与PVD镀膜的结合能力，防止PVD镀膜脱落；四是通过优化PVD镀膜的真空度和温度等参数，可以进一步的提高镀镍层与PVD镀膜之间具有更强的结合力，同时能够让PVD镀膜的均匀性更好。本发明在MIM 产品的表面依次镀镍层和PVD膜，其工艺简单，可操作性强，在能够大幅提高产品表面平滑度的同时，还能够有效的提高产品的耐磨和耐腐蚀能力，采用本发明工艺处理后镀层的结合能力较强，在进行盐雾试验后，90%以上的产品能够达到60小时，抗腐蚀性能较好，易于推广使用。
具体实施方式
下面结合实施例对本发明作进一步的说明，但不以任何方式对本发明加以限制，基于本发明教导所作的任何变换或替换，均属于本发明的保护范围。
实施例1：
本实施例1所述不锈钢MIM产品表面镀层的加工工艺，包括以下工艺步骤:
⑴热浸除油:将MIM产品放入温度为50℃的热浸除油剂中，浸泡170s，热浸除油剂采用现有MIM产品使用的除油剂，除油剂包括以下质量百分比含量的组分，碳酸氢钠30～60%、氢氧化钠25～40%、磷酸钠10～20%和硅酸钠5～10%；
⑵超声波清洗：将MIM产品从热浸除油剂中捞出后进行超声波水洗，超声清洗的水温为50℃，超声清洗的时间为150s，超声频率为30HZ，采用超声波进行清洗，超声波发生器发出的高频振荡信号，通过超声波换能器转换成高频机械振荡而传播到清洗介质，从而将粘附在产品表面不易清除的固体离子等污物脱离；
⑶电解除油：将MIM产品放入温度为50℃的无机酸溶液中进行电解除油，无机酸溶液的质量浓度为50g/L，电解除油的时间为3min，电解除油的电压为3V；
⑷风干处理：将MIM产品放入用40℃的热水清洗30s，之后用压缩空气吹去MIM产品表面的水分，压缩空气的气压为0.1MPa；
⑸活化处理：将MIM产品放入到质量分数为1%的活化液中进行活化处理，活化处理的时间为60s，所所述活化液包括以下质量百分比含量的组分：无机酸40～90%、氟化氢铵8～60%和过氧化氢1～3%，利用活化液对产品进行活化处理，利用活化液的还原性，对除油的产品氧化层进行活化和清润，使氧化层松动，便于后续的镀镍处理，活化处理工序能在活化产品表面氧化层的同时，还可以修复产品表面的凹痕和损伤；
⑹预镀镍：将MIM产品放入到8波美度的镀镍溶液中，浸泡1min，所述镀镍溶液的配方为：氯化镍100～150g/L、氨基磺酸镍50～80 g/L、硼酸20～30 g/L、十二烷基苯磺酸钠0.01～0.02 g/L、柠檬酸钠20～30 g/L、硫酸铵2～5 g/L、羟丙基走位剂0.1～0.15 g/L和PS试剂0.05～0.1 g/L；
⑺电镀镍：将MIM产品放入到4波美度的镀镍溶液中，所述镀镍溶液的配方为：氯化镍100～150g/L、氨基磺酸镍50～80 g/L、硼酸20～30 g/L、十二烷基苯磺酸钠0.01～0.02 g/L、柠檬酸钠20～30 g/L、硫酸铵2～5 g/L、羟丙基走位剂0.1～0.15 g/L和PS试剂0.05～0.1 g/L，在传统镀镍液的基础上，添加了羟丙基走位剂，结合柠檬酸钠和硫酸铵，能够大幅的提高镀镍液的深镀能力，且通过添加羟丙基走位剂和P试剂能够使得到的镀镍层光亮平整，晶粒均匀致密，耐腐蚀性好，在80℃的温度下进行电镀，让MIM产品的表面镀上一层镀镍层，镀镍层的厚度为0.1um，电镀镍分三次进行，第一次电镀的电流密度为1A/dm2，第一次电镀的时间为1min，第二次电镀的电流密度3A/dm2，第二次电镀的时间为2min，第三次电镀的电流密度7A/dm2，第三次电镀的时间为3min，每次电镀结束后需采用喷淋的方式对MIM产品进行水洗，水洗的时间为2min，之后用压缩空气吹去MIM产品表面的水分，压缩空气的气压为0.1MPa；
⑻PVD镀膜：将MIM产品放入到镀膜室中，对镀膜室内进行抽真空和加热处理，使镀膜室内的真空度达到1MPa，镀膜室内的温度达到160℃之后，向镀膜室内通入氩气，然后开启靶源对MIM产品镀膜，靶源受电场和磁场的周期变化驱动，在磁控溅射与阴极电弧之间切换镀膜，待工件表面的PV镀膜厚度达到0.5μm后，停止镀膜，然后关闭靶源和所有电源，靶源选用的靶材为Ni、NiO、TiO2、Sn或SnO2，待镀膜室内的温度降至室温后，抽出室内的氩气，加强抽气5min，除去镀膜室内的残留的氩气后，将镀膜室内放空气至大气压，取出MIM产品；
⑼ 纳米封闭：将MIM产品放入封闭剂中浸泡3min，所述封闭剂包括以下重量份的原料：硅溶胶50份、改性硅烷10份、水溶性丙烯酸树脂25份、石墨烯3份、石墨烯分散剂3份和水30份，所述石墨烯为单层氧化纳米石墨烯、少层氧化纳米石墨烯和多层氧化纳米石墨烯中的至少一种；所述石墨烯分散剂包括无机分散剂和有机分散剂，所述无机分散剂为硅酸钠、三聚磷酸钠、六偏磷酸钠和焦磷酸钠中的至少一种，所述有机分散剂为三乙基己基磷酸、十二烷基硫酸钠、甲基戊醇、纤维素衍生物、古尔胶、脂肪酸聚乙二醇酯、聚乙烯醇、聚乙烯吡咯烷酮、聚丙烯酸钠和聚丙烯酰胺中的至少一种；所述改性硅烷为聚乙二醇-14二甲基硅氧烷、聚乙二醇/聚丙二醇-14/4-二甲基硅氧烷、聚乙二醇-6醋酸酯硅氧烷中的至少一种；MIM产品经过封闭剂浸泡处理，能够在其表面形成抗水、耐湿、耐盐雾的防水层，具有非常好的耐腐蚀性能，之后将MIM产品从封闭剂中取出后，置于烤箱中，在70℃的温度下烘烤30s，取出冷却至室温后即可得到MIM成品。
本实施例1对MIM产品进行除油、镀镍后，再经过PVD镀膜和封闭处理后，能够在MIM产品的表面形成一层附着能力更大的高致密性PVD镀膜，让MIM产品具有较好的抗水、耐磨和耐腐蚀性能，完全能够满足3C行业结构外观件48小时的中性盐雾性测试的需求，经试验证明，本发明处理后的膜层与MIM产品的结合能力较强，90%以上的镀层抗中性盐雾试验能高达68h，具有较好的耐磨和耐腐蚀能力。
实施例2：
本实施例2所述不锈钢MIM产品表面镀层的加工工艺，包括以下工艺步骤:
⑴热浸除油:将MIM产品放入温度为55℃的热浸除油剂中，浸泡185s，热浸除油剂采用现有MIM产品使用的除油剂，除油剂包括以下质量百分比含量的组分，碳酸氢钠30～60%、氢氧化钠25～40%、磷酸钠10～20%和硅酸钠5～10%；
⑵超声波清洗：将MIM产品从热浸除油剂中捞出后进行超声波水洗，超声清洗的水温为55℃，超声清洗的时间为175s，超声频率为35HZ，采用超声波进行清洗，超声波发生器发出的高频振荡信号，通过超声波换能器转换成高频机械振荡而传播到清洗介质，从而将粘附在产品表面不易清除的固体离子等污物脱离；
⑶电解除油：将MIM产品放入温度为55℃的无机酸溶液中进行电解除油，无机酸溶液的质量浓度为65g/L，电解除油的时间为4min，电解除油的电压为4V；
⑷风干处理：将MIM产品放入用45℃的热水清洗45s，之后用压缩空气吹去MIM产品表面的水分，压缩空气的气压为0.15MPa；
⑸活化处理：将MIM产品放入到质量分数为13%的活化液中进行活化处理，活化处理的时间为90s，所述活化液包括以下质量百分比含量的组分：无机酸40～90%、氟化氢铵8～60%和过氧化氢1～3%，利用活化液对产品进行活化处理，利用活化液的还原性，对除油的产品氧化层进行活化和清润，使氧化层松动，便于后续的镀镍处理，活化处理工序能在活化产品表面氧化层的同时，还可以修复产品表面的凹痕和损伤；
⑹预镀镍：将MIM产品放入到10波美度的镀镍溶液中，浸泡1.5min，所述镀镍溶液的配方为：氯化镍100～150g/L、氨基磺酸镍50～80 g/L、硼酸20～30 g/L、十二烷基苯磺酸钠0.01～0.02 g/L、柠檬酸钠20～30 g/L、硫酸铵2～5 g/L、羟丙基走位剂0.1～0.15 g/L和PS试剂0.05～0.1 g/L；
⑺电镀镍：将MIM产品放入到5波美度的镀镍溶液中，所述镀镍溶液的配方为：氯化镍100～150g/L、氨基磺酸镍50～80 g/L、硼酸20～30 g/L、十二烷基苯磺酸钠0.01～0.02 g/L、柠檬酸钠20～30 g/L、硫酸铵2～5 g/L、羟丙基走位剂0.1～0.15 g/L和PS试剂0.05～0.1 g/L，在传统镀镍液的基础上，添加了羟丙基走位剂，结合柠檬酸钠和硫酸铵，能够大幅的提高镀镍液的深镀能力，且通过添加羟丙基走位剂和P试剂能够使得到的镀镍层光亮平整，晶粒均匀致密，耐腐蚀性好，在80～90℃的温度下进行电镀，让MIM产品的表面镀上一层镀镍层，镀镍层的厚度为0.2um，电镀镍分三次进行，第一次电镀的电流密度为1.5A/dm2，第一次电镀的时间为1.5min，第二次电镀的电流密度4A/dm2，第二次电镀的时间为3min，第三次电镀的电流密度9A/dm2，第三次电镀的时间为4min，每次电镀结束后需采用喷淋的方式对MIM产品进行水洗，水洗的时间为3min，之后用压缩空气吹去MIM产品表面的水分，压缩空气的气压为0.15MPa；
⑻PVD镀膜：将MIM产品放入到镀膜室中，对镀膜室内进行抽真空和加热处理，使镀膜室内的真空度达到1.2MPa，镀膜室内的温度达到162℃之后，向镀膜室内通入氩气，然后开启靶源对MIM产品镀膜，靶源受电场和磁场的周期变化驱动，在磁控溅射与阴极电弧之间切换镀膜，待工件表面的PV镀膜厚度达到1μm后，停止镀膜，然后关闭靶源和所有电源，靶源选用的靶材为Ni、NiO、TiO2、Sn或SnO2，待镀膜室内的温度降至室温后，抽出室内的氩气，加强抽气8min，除去镀膜室内的残留的氩气后，将镀膜室内放空气至大气压，取出MIM产品；
⑼ 纳米封闭：将MIM产品放入封闭剂中浸泡4min，所述封闭剂包括以下重量份的原料：硅溶胶80份、改性硅烷15份、水溶性丙烯酸树脂35份、石墨烯4份、石墨烯分散剂4份和水50份，所述石墨烯为单层氧化纳米石墨烯、少层氧化纳米石墨烯和多层氧化纳米石墨烯中的至少一种；所述石墨烯分散剂包括无机分散剂和有机分散剂，所述无机分散剂为硅酸钠、三聚磷酸钠、六偏磷酸钠和焦磷酸钠中的至少一种，所述有机分散剂为三乙基己基磷酸、十二烷基硫酸钠、甲基戊醇、纤维素衍生物、古尔胶、脂肪酸聚乙二醇酯、聚乙烯醇、聚乙烯吡咯烷酮、聚丙烯酸钠和聚丙烯酰胺中的至少一种；所述改性硅烷为聚乙二醇-14二甲基硅氧烷、聚乙二醇/聚丙二醇-14/4-二甲基硅氧烷、聚乙二醇-6醋酸酯硅氧烷中的至少一种；MIM产品经过封闭剂浸泡处理，能够在其表面形成抗水、耐湿、耐盐雾的防水层，具有非常好的耐腐蚀性能，之后将MIM产品从封闭剂中取出后，置于烤箱中，在75℃的温度下烘烤35s，取出冷却至室温后即可得到MIM成品。
本实施例2对MIM产品进行除油、镀镍后，再经过PVD镀膜和封闭处理后，能够在MIM产品的表面形成一层附着能力更大的高致密性PVD镀膜，让MIM产品具有较好的抗水、耐磨和耐腐蚀性能，完全能够满足3C行业结构外观件48小时的中性盐雾性测试的需求，经试验证明，本发明处理后的膜层与MIM产品的结合能力较强，90%以上的镀层抗中性盐雾试验能高达72h，具有较好的耐磨和耐腐蚀能力。
实施例3：
本实施例3所述不锈钢MIM产品表面镀层的加工工艺，包括以下工艺步骤:
⑴热浸除油:将MIM产品放入温度为60℃的热浸除油剂中，浸泡200s，热浸除油剂采用现有MIM产品使用的除油剂，除油剂包括以下质量百分比含量的组分，碳酸氢钠30～60%、氢氧化钠25～40%、磷酸钠10～20%和硅酸钠5～10%；
⑵超声波清洗：将MIM产品从热浸除油剂中捞出后进行超声波水洗，超声清洗的水温为60℃，超声清洗的时间为200s，超声频率为40HZ，采用超声波进行清洗，超声波发生器发出的高频振荡信号，通过超声波换能器转换成高频机械振荡而传播到清洗介质，从而将粘附在产品表面不易清除的固体离子等污物脱离；
⑶电解除油：将MIM产品放入温度为60℃的无机酸溶液中进行电解除油，无机酸溶液的质量浓度为80g/L，电解除油的时间为5min，电解除油的电压为5V；
⑷风干处理：将MIM产品放入用50℃的热水清洗60s，之后用压缩空气吹去MIM产品表面的水分，压缩空气的气压为0.2MPa；
⑸活化处理：将MIM产品放入到质量分数为20%的活化液中进行活化处理，活化处理的时间为60～120s，所述活化液包括以下质量百分比含量的组分：无机酸40～90%、氟化氢铵8～60%和过氧化氢1～3%，利用活化液对产品进行活化处理，利用活化液的还原性，对除油的产品氧化层进行活化和清润，使氧化层松动，便于后续的镀镍处理，活化处理工序能在活化产品表面氧化层的同时，还可以修复产品表面的凹痕和损伤；
⑹预镀镍：将MIM产品放入到8～12波美度的镀镍溶液中，浸泡2min，所述镀镍溶液的配方为：氯化镍100～150g/L、氨基磺酸镍50～80 g/L、硼酸20～30 g/L、十二烷基苯磺酸钠0.01～0.02 g/L、柠檬酸钠20～30 g/L、硫酸铵2～5 g/L、羟丙基走位剂0.1～0.15 g/L和PS试剂0.05～0.1 g/L；
⑺电镀镍：将MIM产品放入到4～6波美度的镀镍溶液中，所述镀镍溶液的配方为：氯化镍100～150g/L、氨基磺酸镍50～80 g/L、硼酸20～30 g/L、十二烷基苯磺酸钠0.01～0.02g/L、柠檬酸钠20～30 g/L、硫酸铵2～5 g/L、羟丙基走位剂0.1～0.15 g/L和PS试剂0.05～0.1 g/L，在传统镀镍液的基础上，添加了羟丙基走位剂，结合柠檬酸钠和硫酸铵，能够大幅的提高镀镍液的深镀能力，且通过添加羟丙基走位剂和P试剂能够使得到的镀镍层光亮平整，晶粒均匀致密，耐腐蚀性好，在90℃的温度下进行电镀，让MIM产品的表面镀上一层镀镍层，镀镍层的厚度为0.2um，电镀镍分三次进行，第一次电镀的电流密度为2A/dm2，第一次电镀的时间为2min，第二次电镀的电流密度5A/dm2，第二次电镀的时间为4min，第三次电镀的电流密度10A/dm2，第三次电镀的时间为4min，每次电镀结束后需采用喷淋的方式对MIM产品进行水洗，水洗的时间为3min，之后用压缩空气吹去MIM产品表面的水分，压缩空气的气压为0.2MPa；
⑻PVD镀膜：将MIM产品放入到镀膜室中，对镀膜室内进行抽真空和加热处理，使镀膜室内的真空度达到1.5MPa，镀膜室内的温度达到165℃之后，向镀膜室内通入氩气，然后开启靶源对MIM产品镀膜，靶源受电场和磁场的周期变化驱动，在磁控溅射与阴极电弧之间切换镀膜，待工件表面的PV镀膜厚度达到1.5μm后，停止镀膜，然后关闭靶源和所有电源，靶源选用的靶材为Ni、NiO、TiO2、Sn或SnO2，待镀膜室内的温度降至室温后，抽出室内的氩气，加强抽气10min，除去镀膜室内的残留的氩气后，将镀膜室内放空气至大气压，取出MIM产品；
⑼ 纳米封闭：将MIM产品放入封闭剂中浸泡5min，所述封闭剂包括以下重量份的原料：硅溶胶100份、改性硅烷20份、水溶性丙烯酸树脂60份、石墨烯5份、石墨烯分散剂5份和水70份，所述石墨烯为单层氧化纳米石墨烯、少层氧化纳米石墨烯和多层氧化纳米石墨烯中的至少一种；所述石墨烯分散剂包括无机分散剂和有机分散剂，所述无机分散剂为硅酸钠、三聚磷酸钠、六偏磷酸钠和焦磷酸钠中的至少一种，所述有机分散剂为三乙基己基磷酸、十二烷基硫酸钠、甲基戊醇、纤维素衍生物、古尔胶、脂肪酸聚乙二醇酯、聚乙烯醇、聚乙烯吡咯烷酮、聚丙烯酸钠和聚丙烯酰胺中的至少一种；所述改性硅烷为聚乙二醇-14二甲基硅氧烷、聚乙二醇/聚丙二醇-14/4-二甲基硅氧烷、聚乙二醇-6醋酸酯硅氧烷中的至少一种；MIM产品经过封闭剂浸泡处理，能够在其表面形成抗水、耐湿、耐盐雾的防水层，具有非常好的耐腐蚀性能，之后将MIM产品从封闭剂中取出后，置于烤箱中，在80℃的温度下烘烤40s，取出冷却至室温后即可得到MIM成品。
本实施例3对MIM产品进行除油、镀镍后，再经过PVD镀膜和封闭处理后，能够在MIM产品的表面形成一层附着能力更大的高致密性PVD镀膜，让MIM产品具有较好的抗水、耐磨和耐腐蚀性能，完全能够满足3C行业结构外观件48小时的中性盐雾性测试的需求，经试验证明，本发明处理后的膜层与MIM产品的结合能力较强，90%以上的镀层抗中性盐雾试验能高达65h，具有较好的耐磨和耐腐蚀能力。
Claims (6)
1.一种不锈钢MIM产品表面镀层的加工工艺，其特征在于,包括以下工艺步骤:
⑴热浸除油:将MIM产品放入温度为50～60℃的热浸除油剂中，浸泡170～200s；
⑵超声波清洗：将MIM产品从热浸除油剂中捞出后进行超声波水洗，超声清洗的水温为50～60℃，超声清洗的时间为150～200s，超声频率为30～40HZ；
⑶电解除油：将MIM产品放入温度为50～60℃的无机酸溶液中进行电解除油，无机酸溶液的质量浓度为50～80g/L，电解除油的时间为3～5min，电解除油的电压为3～5V；
⑷风干处理：将MIM产品放入用40～50℃的热水清洗30～60s，之后用压缩空气吹去MIM产品表面的水分，压缩空气的气压为0.1～0.2MPa；
⑸活化处理：将MIM产品放入到质量分数为15～20%的活化液中进行活化处理，活化处理的时间为60～120s；
⑹预镀镍：将MIM产品放入到8～12波美度的镀镍溶液中，浸泡1～2min；
⑺电镀镍：将MIM产品放入到4～6波美度的镀镍溶液中，在80～90℃的温度下进行电镀，让MIM产品的表面镀上一层镀镍层，镀镍层的厚度为0.1～0.2um，之后用压缩空气吹去MIM产品表面的水分，压缩空气的气压为0.1～0.2MPa；
⑻PVD镀膜：将MIM产品放入到镀膜室中，对镀膜室内进行抽真空和加热处理，使镀膜室内的真空度达到1～1.5MPa，镀膜室内的温度达到160～165℃之后，向镀膜室内通入氩气，然后开启靶源对MIM产品镀膜，靶源受电场和磁场的周期变化驱动，在磁控溅射与阴极电弧之间切换镀膜，待工件表面的PV镀膜厚度达到0.5～1.5μm后，停止镀膜，然后关闭靶源和所有电源，待镀膜室内的温度降至室温后，抽出室内的氩气，加强抽气5～10min，除去镀膜室内的残留的氩气后，将镀膜室内放空气至大气压，取出MIM产品；
⑼ 纳米封闭：将MIM产品放入封闭剂中浸泡3～5min，所述封闭剂包括以下重量份的原料：硅溶胶50～100份、改性硅烷10～20份、水溶性丙烯酸树脂25～60份、石墨烯3～5份、石墨烯分散剂3～5份和水30～70份，之后将MIM产品从封闭剂中取出后，置于烤箱中，在70～80℃的温度下烘烤30～40s，取出冷却至室温后即可得到MIM成品。
2.根据权利要求1所述的一种不锈钢MIM产品表面镀层的加工工艺，其特征在于：在步骤⑸中，所述活化液包括无机酸、氟化氢铵和过氧化氢。
3.根据权利要求1所述的一种不锈钢MIM产品表面镀层的加工工艺，其特征在于：在步骤⑹和⑺中，所述镀镍溶液的配方为：氯化镍100～150g/L、氨基磺酸镍50～80 g/L、硼酸20～30 g/L、十二烷基苯磺酸钠0.01～0.02 g/L、柠檬酸钠20～30 g/L、硫酸铵2～5 g/L、羟丙基走位剂0.1～0.15 g/L和PS试剂0.05～0.1 g/L。
4.根据权利要求1所述的一种不锈钢MIM产品表面镀层的加工工艺，其特征在于：在步骤⑺中，电镀镍分三次进行，第一次电镀的电流密度为1～2A/dm2，第一次电镀的时间为1～2min，第二次电镀的电流密度3～5A/dm2，第二次电镀的时间为2～4min，第二次电镀的电流密度7～10A/dm2，第二次电镀的时间为3～4min，每次电镀结束后需采用喷淋的方式对MIM产品进行水洗，水洗的时间为2～3min。
5.根据权利要求1所述的一种不锈钢MIM产品表面镀层的加工工艺，其特征在于：在步骤⑻中，靶源选用的靶材为Ni、NiO、TiO2、Sn或SnO2。
6.根据权利要求1所述的一种不锈钢MIM产品表面镀层的加工工艺，其特征在于：在步骤⑼中，所述石墨烯为单层氧化纳米石墨烯、少层氧化纳米石墨烯和多层氧化纳米石墨烯中的至少一种；所述石墨烯分散剂包括无机分散剂和有机分散剂，所述无机分散剂为硅酸钠、三聚磷酸钠、六偏磷酸钠和焦磷酸钠中的至少一种，所述有机分散剂为三乙基己基磷酸、十二烷基硫酸钠、甲基戊醇、纤维素衍生物、古尔胶、脂肪酸聚乙二醇酯、聚乙烯醇、聚乙烯吡咯烷酮、聚丙烯酸钠和聚丙烯酰胺中的至少一种；所述改性硅烷为聚乙二醇-14二甲基硅氧烷、聚乙二醇/聚丙二醇-14/4-二甲基硅氧烷、聚乙二醇-6醋酸酯硅氧烷中的至少一种。
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