CN116770245B - Method for preparing metal surface protective coating by vacuum coating process - Google Patents
Method for preparing metal surface protective coating by vacuum coating process Download PDFInfo
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- CN116770245B CN116770245B CN202310693097.8A CN202310693097A CN116770245B CN 116770245 B CN116770245 B CN 116770245B CN 202310693097 A CN202310693097 A CN 202310693097A CN 116770245 B CN116770245 B CN 116770245B
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- 238000000034 method Methods 0.000 title claims abstract description 70
- 239000011253 protective coating Substances 0.000 title claims abstract description 40
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 37
- 239000002184 metal Substances 0.000 title claims abstract description 37
- 230000008569 process Effects 0.000 title claims abstract description 22
- 238000001771 vacuum deposition Methods 0.000 title claims abstract description 20
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 51
- 239000011651 chromium Substances 0.000 claims abstract description 48
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 46
- 238000000576 coating method Methods 0.000 claims abstract description 38
- 239000011248 coating agent Substances 0.000 claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 33
- 230000007704 transition Effects 0.000 claims abstract description 32
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 31
- 239000010703 silicon Substances 0.000 claims abstract description 31
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 27
- QQHSIRTYSFLSRM-UHFFFAOYSA-N alumanylidynechromium Chemical compound [Al].[Cr] QQHSIRTYSFLSRM-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229920000728 polyester Polymers 0.000 claims abstract description 24
- 229910017758 Cu-Si Inorganic materials 0.000 claims abstract description 14
- 229910017931 Cu—Si Inorganic materials 0.000 claims abstract description 14
- 238000007590 electrostatic spraying Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims description 46
- 229920001225 polyester resin Polymers 0.000 claims description 35
- 239000004645 polyester resin Substances 0.000 claims description 35
- 239000011261 inert gas Substances 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 23
- 229910052782 aluminium Inorganic materials 0.000 claims description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 21
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 19
- 229910052802 copper Inorganic materials 0.000 claims description 19
- 239000010949 copper Substances 0.000 claims description 19
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 238000005086 pumping Methods 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000011159 matrix material Substances 0.000 claims description 16
- 238000000151 deposition Methods 0.000 claims description 11
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 10
- 239000002518 antifoaming agent Substances 0.000 claims description 9
- 239000003963 antioxidant agent Substances 0.000 claims description 9
- 230000003078 antioxidant effect Effects 0.000 claims description 9
- DIJRHOZMLZRNLM-UHFFFAOYSA-N dimethoxy-methyl-(3,3,3-trifluoropropyl)silane Chemical compound CO[Si](C)(OC)CCC(F)(F)F DIJRHOZMLZRNLM-UHFFFAOYSA-N 0.000 claims description 9
- 239000003365 glass fiber Substances 0.000 claims description 9
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 9
- 239000003921 oil Substances 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- BVFSYZFXJYAPQJ-UHFFFAOYSA-N butyl(oxo)tin Chemical compound CCCC[Sn]=O BVFSYZFXJYAPQJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 230000007423 decrease Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 7
- 239000000853 adhesive Substances 0.000 abstract description 5
- 230000001070 adhesive effect Effects 0.000 abstract description 5
- 230000006750 UV protection Effects 0.000 abstract description 4
- 238000005034 decoration Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 230000008859 change Effects 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 6
- 238000005240 physical vapour deposition Methods 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- GOWYWDDPOBCVFH-UHFFFAOYSA-N methoxy-methyl-propyl-(trifluoromethoxy)silane Chemical compound FC(O[Si](OC)(C)CCC)(F)F GOWYWDDPOBCVFH-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
- B05D1/04—Processes for applying liquids or other fluent materials performed by spraying involving the use of an electrostatic field
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0218—Pretreatment, e.g. heating the substrate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
-
- 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
- C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the 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
- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
-
- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/028—Physical treatment to alter the texture of the substrate surface, e.g. grinding, polishing
-
- 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
- C23C14/54—Controlling or regulating the coating process
- C23C14/548—Controlling the composition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2508/00—Polyesters
Abstract
The invention relates to a method for preparing a metal surface protective coating by adopting a vacuum coating process, and belongs to the technical field of metal surface coatings. Pretreating aluminum alloy, then adopting a magnetron sputtering method to deposit a layer of Al-Cr transition layer, then adopting the magnetron sputtering method to prepare a layer of Cr-Cu-Si color decorative layer, finally carrying out electrostatic spraying on organosilicon modified polyester transparent powder coating, and curing to obtain the protective coating with the transparent layer on the surface. According to the invention, the Al-Cr transition layer is deposited on the surface of the aluminum alloy, so that the binding force between the coating and the aluminum alloy is improved, the chromium target current is controlled to be gradually reduced, the silicon target current is controlled to be gradually increased in the preparation process of the color decorative layer, the color decorative layer has the color gradient effect, and the transparent layer prepared from the organic silicon modified polyester transparent powder coating has a good surface highlight effect on the color decorative layer, and also has good high temperature resistance, ultraviolet resistance, hydrophobicity and high adhesive force.
Description
Technical Field
The invention belongs to the technical field of metal surface coatings, and relates to a method for preparing a metal surface protective coating by adopting a vacuum coating process.
Background
With the development of automobiles, hardware, household appliances, electronics, buildings and corresponding decoration industries, the aluminum alloy has higher and higher requirements on the appearance and functions of various internal and external decoration products, has light weight and other excellent properties, and is widely applied to the automobiles, hardware, household appliances, electronics, buildings and corresponding decoration industries, and the aluminum alloy is relatively poor in stability, easy to oxidize and single in color, and needs to be treated on the surface of the aluminum alloy to improve the surface decoration property, weather resistance and other properties.
The conventional electroplating method is faced with the problems of rearranging and technical innovation due to the large amount of discharged polluted wastewater. Vacuum coating refers to a method of forming a thin film by heating a metal or non-metal material under high vacuum conditions to evaporate and condense the material on the surface of a plated article (metal, semiconductor or insulator), and the vacuum coating technique is generally classified into two main types, namely, physical Vapor Deposition (PVD) technique and Chemical Vapor Deposition (CVD) technique. The chemical vapor deposition technology is a method for preparing a metal or compound film on a substrate by supplying simple substance gas or compound containing film elements to the substrate and adopting the gas phase action or chemical reaction on the surface of the substrate, and mainly comprises normal pressure chemical vapor deposition, low pressure chemical vapor deposition, plasma chemical vapor deposition and the like with the characteristics of CVD and PVD; physical vapor deposition refers to a method of directly depositing plating materials onto a substrate surface by vaporizing atoms, molecules or ionizing them into ions using various physical methods under vacuum conditions, including vacuum evaporation, arc plasma plating, magnetron sputtering, and the like.
The technology for preparing the protective decorative coating on the surface of the aluminum alloy by adopting magnetron sputtering is more, but the problems of lower binding force between the decorative coating and the aluminum alloy matrix, single decorative color, low glossiness and the like exist.
Disclosure of Invention
The invention aims to provide a method for preparing a metal surface protective coating by adopting a vacuum coating process, and belongs to the technical field of metal surface coatings. The invention polishes, cleans, glows and cleans the aluminum alloy, then adopts magnetron sputtering method to deposit a layer of Al-Cr transition layer by aluminum target and chromium target, then adopts magnetron sputtering method to prepare a Cr-Cu-Si color decorative layer with gradually changed components from inside to outside by chromium target, copper target and silicon target, finally electrostatic spraying organosilicon modified polyester transparent powder coating, and the protective coating with transparent layer on the surface is obtained after curing treatment. According to the invention, the Al-Cr transition layer is deposited on the surface of the aluminum alloy, so that the binding force between the coating and the aluminum alloy is improved, the chromium target current is controlled to be gradually reduced, the silicon target current is controlled to be gradually increased in the preparation process of the color decorative layer, the color decorative layer has the effect of gradually changing colors, and the transparent layer prepared from the organic silicon modified polyester transparent powder coating has a better surface highlight effect on the color decorative layer, and also has better high-temperature resistance, hydrophobic performance and higher adhesive force; the organosilicon modified polyester resin in the organosilicon modified polyester transparent powder coating contains C-F bonds, so that the ultraviolet resistance, the weather resistance, the hydrophobic property and the high temperature resistance of the surface of the coating are improved, and the binding force between the transparent layer and the color decorative layer is enhanced.
The aim of the invention can be achieved by the following technical scheme:
a method for preparing a protective coating on a metal surface by adopting a vacuum coating process, comprising the following steps:
(1) Polishing the aluminum alloy matrix;
(2) Cleaning the surface of the polished aluminum alloy matrix;
(3) Transferring the aluminum alloy with the surface cleaned into a vacuum furnace, and carrying out glow cleaning after exhausting to background vacuum;
(4) Depositing an Al-Cr transition layer on the surface of the aluminum alloy matrix subjected to glow cleaning by adopting a magnetron sputtering method from an aluminum target and a chromium target at the same time;
(5) A Cr-Cu-Si color decorative layer is deposited on the surface of the Al-Cr transition layer by a magnetron sputtering method from a chromium target, a copper target and a silicon target at the same time, so as to obtain a coated workpiece;
(6) Transferring the coated workpiece to a powder spraying line, heating and preserving heat;
(7) And (3) carrying out electrostatic spraying on the surface of the heat-preserving workpiece with an organosilicon modified polyester transparent powder coating, and heating and curing to form a transparent layer, thereby preparing the metal surface protective coating.
As a preferable technical scheme of the invention, the surface cleaning in the step (2) refers to the steps of wax removal, oil removal and rust removal cleaning of the aluminum alloy matrix.
As a preferable technical scheme of the invention, the glow cleaning process in the step (3) comprises the following steps: pumping the vacuum furnace to background vacuum with the vacuum degree of 6.5-9.5X10 -4 And during Pa, introducing inert gas, starting a bias power supply to carry out glow cleaning on the surface of the workpiece when the vacuum degree reaches 0.5-1.5Pa, wherein the bias voltage during glow cleaning is 800-1200V, the duty ratio is 45-70%, and the current is 1.5-4.8A.
As a preferable technical scheme of the invention, the conditions of the magnetron sputtering in the step (4) are as follows: pumping air in the vacuum furnace to background vacuum, and then introducing inert gas to enable the vacuum degree to reach 0.1-1Pa; the aluminum target current is 15-30A, the chromium target current is 10-20A, and the inert gas flow is 80-200sccm.
As a preferred embodiment of the present invention, the initial current of the chromium target in the step (5) is 35-45A and gradually decreases at a rate of 1-3A/min, the copper target current is 20-30A and remains unchanged, and the initial current of the silicon target is 10-20A and gradually increases at a rate of 2-3A/min.
As a preferable technical scheme of the invention, the heating temperature in the step (6) is 90-120 ℃.
As a preferable technical scheme of the invention, the organosilicon modified polyester transparent powder coating in the step (7) comprises 60-80 parts by weight of organosilicon modified polyester resin, 10-30 parts by weight of curing agent, 15-25 parts by weight of glass fiber, 2-3 parts by weight of leveling agent, 0.5-1.5 parts by weight of defoaming agent and 0.5-1 part by weight of antioxidant.
As a preferred technical scheme of the invention, the preparation method of the organosilicon modified polyester resin comprises the following steps:
39 parts by weight of neopentyl glycol and 0.05 part by weight of monobutyl tin oxide are put into a reaction kettle, nitrogen is introduced, 32 parts by weight of trifluoropropyl methyl dimethoxy silane is dropwise added while stirring, the temperature is raised, when the temperature is raised to 190 ℃, the temperature is kept for 2.5 hours, 45 parts by weight of terephthalic acid is added after the temperature is lowered to 150 ℃, then the temperature is raised to 240 ℃ and the temperature is kept for 3 hours, and the organosilicon modified polyester resin is obtained after the temperature is lowered.
As a preferable technical scheme of the invention, the thickness of the Al-Cr transition layer is 80-120um, the thickness of the Cr-Cu-Si color decorative layer is 100-200um, and the thickness of the transparent layer is 60-80um.
As a preferable technical scheme of the invention, the heating temperature in the step (7) is 200-220 ℃.
The invention has the beneficial effects that:
(1) According to the invention, after polishing, cleaning and glow cleaning of the aluminum alloy, a layer of Al-Cr transition layer is deposited on the aluminum target and the chromium target simultaneously by adopting a magnetron sputtering method, and parameters such as current of the aluminum target and the chromium target are controlled by adopting a mode of simultaneous deposition of the aluminum target and the chromium target, so that the transition layer contains a certain content of aluminum, and the binding force of the Al-Cr transition layer and an aluminum alloy substrate is improved;
(2) In the preparation process of the color decorative layer, the chromium target current is controlled to be gradually reduced, the silicon target current is gradually increased, so that the chromium content in the Cr-Cu-Si color decorative layer is gradually reduced from inside to outside, and the silicon content is gradually increased from inside to outside, and the color decorative layer shows the effect of color gradual change;
(3) The color decoration layer has higher chromium content at one side close to the transition layer, so that the stress difference between the transition layer and the color decoration layer can be reduced, and the binding force between the color decoration layer and the transition layer is enhanced; the silicon content of one side of the color decoration layer close to the transparent layer is higher, so that the stress difference between the color decoration layer and the transparent layer can be reduced, and the binding force between the color decoration layer and the transparent layer is enhanced;
(4) According to the invention, the transparent layer is prepared by adopting an electrostatic spraying mode to spray the organosilicon modified polyester transparent powder coating, the polyester resin is modified by the organosilicon, so that the high temperature resistance, the hydrophobicity, the ultraviolet resistance and the glossiness of the transparent layer are improved, the adhesive force of the transparent layer can be improved by adopting the organosilicon modified polyester resin as the matrix resin of the coating, and meanwhile, the adhesive force of the transparent layer is further improved by introducing a benzene ring structure into the organosilicon modified polyester resin; the trifluoropropyl methyl dimethoxy silane and neopentyl glycol are added in the process of synthesizing the organosilicon modified polyester resin to carry out dealcoholization reaction, and then the trifluoropropyl methyl dimethoxy silane and neopentyl glycol are subjected to polycondensation reaction with terephthalic acid, so that fluorine is introduced into the organosilicon modified polyester resin, the high temperature resistance, the hydrophobicity and the ultraviolet resistance of the transparent layer are further enhanced, meanwhile, the polarity of C-F bonds is larger, the acting force between the transparent layer and the color decorative layer can be improved, and the adhesive force of the transparent layer is further improved.
Detailed Description
In order to further describe the technical means and effects adopted by the present invention for achieving the intended purpose, the following detailed description is given below with reference to the embodiments, structures, features and effects according to the present invention.
Example 1
A method for preparing a protective coating on a metal surface by adopting a vacuum coating process, comprising the following steps:
(1) Polishing the aluminum alloy matrix;
(2) Performing wax removal, oil removal and rust removal cleaning on the polished aluminum alloy substrate;
(3) Transferring the aluminum alloy with the surface cleaned into a vacuum furnace, pumping the vacuum furnace to background vacuum, wherein the vacuum degree is 6.5-9.5X10% -4 During Pa, inert gas is introduced, a bias power supply is started to carry out glow cleaning on the surface of the workpiece when the vacuum degree reaches 0.5-1.5Pa, the bias voltage during glow cleaning is 900V, the duty ratio is 50%, and the current is 2A;
(4) Pumping air in a vacuum furnace to background vacuum, then introducing inert gas to enable the vacuum degree to reach 0.1-1Pa, controlling the current of an aluminum target to be 22A, controlling the current of a chromium target to be 15A, enabling the flow of the inert gas to be 120sccm, and simultaneously depositing an Al-Cr transition layer with the thickness of 80um on the surface of an aluminum alloy substrate subjected to glow cleaning by adopting a magnetron sputtering method from the aluminum target and the chromium target;
(5) A chromium target, a copper target and a silicon target are simultaneously deposited on the surface of an Al-Cr transition layer by adopting a magnetron sputtering method to form a Cr-Cu-Si color decorative layer with the thickness of 185um, the initial current of the chromium target is controlled to be 42A and gradually reduced at the speed of 2A/min, the current of the copper target is 22A and kept unchanged, the initial current of the silicon target is 12A and gradually increased at the speed of 2A/min, and a coated workpiece is obtained;
(6) Transferring the coated workpiece to a powder spraying line, heating to 100 ℃, and preserving heat;
(7) And (3) carrying out electrostatic spraying on the surface of the heat-preserving workpiece with an organosilicon modified polyester transparent powder coating, heating to 210 ℃ and curing to form a transparent layer with the thickness of 65um, so as to prepare the metal surface protective coating, wherein the protective coating presents gradual change color.
The organic silicon modified polyester transparent powder coating comprises 68 parts by weight of organic silicon modified polyester resin, 22 parts by weight of curing agent, 19 parts by weight of glass fiber, 2.2 parts by weight of leveling agent, 0.9 part by weight of defoaming agent and 0.7 part by weight of antioxidant.
The preparation method of the organosilicon modified polyester resin comprises the following steps:
39 parts by weight of neopentyl glycol and 0.05 part by weight of monobutyl tin oxide are put into a reaction kettle, nitrogen is introduced, 32 parts by weight of trifluoropropyl methyl dimethoxy silane is dropwise added while stirring, the temperature is raised, when the temperature is raised to 190 ℃, the temperature is kept for 2.5 hours, 45 parts by weight of terephthalic acid is added after the temperature is lowered to 150 ℃, then the temperature is raised to 240 ℃ and the temperature is kept for 3 hours, and the organosilicon modified polyester resin is obtained after the temperature is lowered.
Example 2
A method for preparing a protective coating on a metal surface by adopting a vacuum coating process, comprising the following steps:
(1) Polishing the aluminum alloy matrix;
(2) Performing wax removal, oil removal and rust removal cleaning on the polished aluminum alloy substrate;
(3) Transferring the aluminum alloy with the surface cleaned into a vacuum furnace, pumping the vacuum furnace to background vacuum, wherein the vacuum degree is 6.5-9.5X10% -4 During Pa, inert gas is introduced, a bias power supply is started to carry out glow cleaning on the surface of the workpiece when the vacuum degree reaches 0.5-1.5Pa, the bias voltage during glow cleaning is 800V, the duty ratio is 60%, and the current is 4A;
(4) Pumping air in a vacuum furnace to background vacuum, then introducing inert gas to enable the vacuum degree to reach 0.1-1Pa, controlling the current of an aluminum target to be 18A, controlling the current of a chromium target to be 14A, enabling the flow of the inert gas to be 100sccm, and simultaneously depositing an Al-Cr transition layer with the thickness of 100um on the surface of an aluminum alloy substrate subjected to glow cleaning by adopting a magnetron sputtering method from the aluminum target and the chromium target;
(5) A Cr-Cu-Si color decorative layer with the thickness of 150um is deposited on the surface of an Al-Cr transition layer by adopting a magnetron sputtering method from a chromium target, a copper target and a silicon target, the initial current of the chromium target is controlled to be 39A and gradually reduced at the speed of 1.2A/min, the current of the copper target is 25A and kept unchanged, the initial current of the silicon target is 18A and gradually increased at the speed of 1A/min, and a coated workpiece is obtained;
(6) Transferring the coated workpiece to a powder spraying line, heating to 110 ℃ and then preserving heat;
(7) And (3) carrying out electrostatic spraying on the surface of the heat-preserving workpiece with an organosilicon modified polyester transparent powder coating, heating to 200 ℃ and curing to form a transparent layer with the thickness of 70 mu m, so as to prepare the metal surface protective coating, wherein the protective coating presents gradual change color.
The silicone modified polyester transparent powder coating comprises 75 parts by weight of silicone modified polyester resin, 25 parts by weight of curing agent, 22 parts by weight of glass fiber, 3 parts by weight of leveling agent, 1.1 parts by weight of defoaming agent and 0.6 part by weight of antioxidant.
The preparation method of the organosilicon modified polyester resin comprises the following steps:
39 parts by weight of neopentyl glycol and 0.05 part by weight of monobutyl tin oxide are put into a reaction kettle, nitrogen is introduced, 32 parts by weight of trifluoropropyl methyl dimethoxy silane is dropwise added while stirring, the temperature is raised, when the temperature is raised to 190 ℃, the temperature is kept for 2.5 hours, 45 parts by weight of terephthalic acid is added after the temperature is lowered to 150 ℃, then the temperature is raised to 240 ℃ and the temperature is kept for 3 hours, and the organosilicon modified polyester resin is obtained after the temperature is lowered.
Example 3
A method for preparing a protective coating on a metal surface by adopting a vacuum coating process, comprising the following steps:
(1) Polishing the aluminum alloy matrix;
(2) Performing wax removal, oil removal and rust removal cleaning on the polished aluminum alloy substrate;
(3) Transferring the aluminum alloy with the surface cleaned into a vacuum furnace, pumping the vacuum furnace to background vacuum, wherein the vacuum degree is 6.5-9.5X10% -4 During Pa, inert gas is introduced, a bias power supply is started to carry out glow cleaning on the surface of the workpiece when the vacuum degree reaches 0.5-1.5Pa, the bias voltage during glow cleaning is 1200V, the duty ratio is 48%, and the current is 3A;
(4) Pumping air in a vacuum furnace to background vacuum, then introducing inert gas to enable the vacuum degree to reach 0.1-1Pa, controlling the current of an aluminum target to be 30A, controlling the current of a chromium target to be 20A, enabling the flow of the inert gas to be 200sccm, and simultaneously depositing an Al-Cr transition layer with the thickness of 120um on the surface of an aluminum alloy substrate subjected to glow cleaning by adopting a magnetron sputtering method from the aluminum target and the chromium target;
(5) A chromium target, a copper target and a silicon target are simultaneously deposited on the surface of an Al-Cr transition layer by adopting a magnetron sputtering method to form a Cr-Cu-Si color decorative layer with the thickness of 200um, the initial current of the chromium target is controlled to be 45A and gradually reduced at the speed of 3A/min, the current of the copper target is 26A and kept unchanged, the initial current of the silicon target is 10A and gradually increased at the speed of 3A/min, and a coated workpiece is obtained;
(6) Transferring the coated workpiece to a powder spraying line, heating to 120 ℃ and then preserving heat;
(7) And (3) carrying out electrostatic spraying on the surface of the heat-preserving workpiece with an organosilicon modified polyester transparent powder coating, heating to 220 ℃ and curing to form a transparent layer with the thickness of 80um, so as to prepare the metal surface protective coating, wherein the protective coating presents gradual change color.
The organosilicon modified polyester transparent powder coating comprises 80 parts by weight of organosilicon modified polyester resin, 28 parts by weight of curing agent, 25 parts by weight of glass fiber, 2.6 parts by weight of leveling agent, 1.5 parts by weight of defoaming agent and 1 part by weight of antioxidant.
The preparation method of the organosilicon modified polyester resin comprises the following steps:
39 parts by weight of neopentyl glycol and 0.05 part by weight of monobutyl tin oxide are put into a reaction kettle, nitrogen is introduced, 32 parts by weight of trifluoropropyl methyl dimethoxy silane is dropwise added while stirring, the temperature is raised, when the temperature is raised to 190 ℃, the temperature is kept for 2.5 hours, 45 parts by weight of terephthalic acid is added after the temperature is lowered to 150 ℃, then the temperature is raised to 240 ℃ and the temperature is kept for 3 hours, and the organosilicon modified polyester resin is obtained after the temperature is lowered.
Comparative example 1
A method for preparing a protective coating on a metal surface by adopting a vacuum coating process, comprising the following steps:
(1) Polishing the aluminum alloy matrix;
(2) Performing wax removal, oil removal and rust removal cleaning on the polished aluminum alloy substrate;
(3) Transferring the aluminum alloy with the surface cleaned into a vacuum furnace, pumping the vacuum furnace to background vacuum, wherein the vacuum degree is 6.5-9.5X10% -4 During Pa, inert gas is introduced, a bias power supply is started to carry out glow cleaning on the surface of the workpiece when the vacuum degree reaches 0.5-1.5Pa, the bias voltage during glow cleaning is 1200V, the duty ratio is 48%, and the current is 3A;
(4) Pumping air in a vacuum furnace to background vacuum, then introducing inert gas to enable the vacuum degree to reach 0.1-1Pa, controlling the current of a chromium target to be 20A, wherein the flow of the inert gas is 200sccm, and depositing a Cr transition layer with the thickness of 120um on the surface of the aluminum alloy substrate subjected to glow cleaning by adopting a magnetron sputtering method;
(5) A chromium target, a copper target and a silicon target are simultaneously deposited on the surface of an Al-Cr transition layer by adopting a magnetron sputtering method to form a Cr-Cu-Si color decorative layer with the thickness of 200um, the initial current of the chromium target is controlled to be 45A and gradually reduced at the speed of 3A/min, the current of the copper target is 26A and kept unchanged, the initial current of the silicon target is 10A and gradually increased at the speed of 3A/min, and a coated workpiece is obtained;
(6) Transferring the coated workpiece to a powder spraying line, heating to 120 ℃ and then preserving heat;
(7) And (3) carrying out electrostatic spraying on the surface of the heat-preserving workpiece with an organosilicon modified polyester transparent powder coating, heating to 220 ℃ and curing to form a transparent layer with the thickness of 80um, so as to prepare the metal surface protective coating, wherein the protective coating presents gradual change color.
The organosilicon modified polyester transparent powder coating comprises 80 parts by weight of organosilicon modified polyester resin, 28 parts by weight of curing agent, 25 parts by weight of glass fiber, 2.6 parts by weight of leveling agent, 1.5 parts by weight of defoaming agent and 1 part by weight of antioxidant.
The preparation method of the organosilicon modified polyester resin comprises the following steps:
39 parts by weight of neopentyl glycol and 0.05 part by weight of monobutyl tin oxide are put into a reaction kettle, nitrogen is introduced, 32 parts by weight of trifluoropropyl methyl dimethoxy silane is dropwise added while stirring, the temperature is raised, when the temperature is raised to 190 ℃, the temperature is kept for 2.5 hours, 45 parts by weight of terephthalic acid is added after the temperature is lowered to 150 ℃, then the temperature is raised to 240 ℃ and the temperature is kept for 3 hours, and the organosilicon modified polyester resin is obtained after the temperature is lowered.
Comparative example 2
A method for preparing a protective coating on a metal surface by adopting a vacuum coating process, comprising the following steps:
(1) Polishing the aluminum alloy matrix;
(2) Performing wax removal, oil removal and rust removal cleaning on the polished aluminum alloy substrate;
(3) Transferring the aluminum alloy with the surface cleaned into a vacuum furnace, pumping the vacuum furnace to background vacuum, wherein the vacuum degree is 6.5-9.5X10% -4 During Pa, inert gas is introduced, a bias power supply is started to carry out glow cleaning on the surface of the workpiece when the vacuum degree reaches 0.5-1.5Pa, the bias voltage during glow cleaning is 1200V, the duty ratio is 48%, and the current is 3A;
(4) Pumping air in a vacuum furnace to background vacuum, then introducing inert gas to enable the vacuum degree to reach 0.1-1Pa, controlling the current of an aluminum target to be 30A, controlling the current of a chromium target to be 20A, enabling the flow of the inert gas to be 200sccm, and simultaneously depositing an Al-Cr transition layer with the thickness of 120um on the surface of an aluminum alloy substrate subjected to glow cleaning by adopting a magnetron sputtering method from the aluminum target and the chromium target;
(5) A chromium target, a copper target and a silicon target are simultaneously deposited on the surface of an Al-Cr transition layer by adopting a magnetron sputtering method to form a Cr-Cu-Si color decorative layer with the thickness of 200 mu m, the current of the chromium target is controlled to be 20A, the current of the copper target is controlled to be 26A, and the current of the silicon target is controlled to be 25A, so that a coated workpiece is obtained;
(6) Transferring the coated workpiece to a powder spraying line, heating to 120 ℃ and then preserving heat;
(7) And (3) carrying out electrostatic spraying on the surface of the heat-preserving workpiece to obtain an organosilicon modified polyester transparent powder coating, heating to 220 ℃ and curing to form a transparent layer with the thickness of 80um, so as to prepare the metal surface protective coating, wherein the protective coating has single color and does not show gradual change.
The organosilicon modified polyester transparent powder coating comprises 80 parts by weight of organosilicon modified polyester resin, 28 parts by weight of curing agent, 25 parts by weight of glass fiber, 2.6 parts by weight of leveling agent, 1.5 parts by weight of defoaming agent and 1 part by weight of antioxidant.
The preparation method of the organosilicon modified polyester resin comprises the following steps:
39 parts by weight of neopentyl glycol and 0.05 part by weight of monobutyl tin oxide are put into a reaction kettle, nitrogen is introduced, 32 parts by weight of trifluoropropyl methyl dimethoxy silane is dropwise added while stirring, the temperature is raised, when the temperature is raised to 190 ℃, the temperature is kept for 2.5 hours, 45 parts by weight of terephthalic acid is added after the temperature is lowered to 150 ℃, then the temperature is raised to 240 ℃ and the temperature is kept for 3 hours, and the organosilicon modified polyester resin is obtained after the temperature is lowered.
Comparative example 3
A method for preparing a protective coating on a metal surface by adopting a vacuum coating process, comprising the following steps:
(1) Polishing the aluminum alloy matrix;
(2) Performing wax removal, oil removal and rust removal cleaning on the polished aluminum alloy substrate;
(3) Transferring the aluminum alloy with the surface cleaned into a vacuum furnace, pumping the vacuum furnace to background vacuum, wherein the vacuum degree is 6.5-9.5X10% -4 During Pa, inert gas is introduced, a bias power supply is started to carry out glow cleaning on the surface of the workpiece when the vacuum degree reaches 0.5-1.5Pa, the bias voltage during glow cleaning is 1200V, the duty ratio is 48%, and the current is 3A;
(4) Pumping air in a vacuum furnace to background vacuum, then introducing inert gas to enable the vacuum degree to reach 0.1-1Pa, controlling the current of an aluminum target to be 30A, controlling the current of a chromium target to be 20A, enabling the flow of the inert gas to be 200sccm, and simultaneously depositing an Al-Cr transition layer with the thickness of 120um on the surface of an aluminum alloy substrate subjected to glow cleaning by adopting a magnetron sputtering method from the aluminum target and the chromium target;
(5) A chromium target, a copper target and a silicon target are simultaneously deposited on the surface of an Al-Cr transition layer by adopting a magnetron sputtering method to form a Cr-Cu-Si color decorative layer with the thickness of 200um, the initial current of the chromium target is controlled to be 45A and gradually reduced at the speed of 3A/min, the current of the copper target is 26A and kept unchanged, the initial current of the silicon target is 10A and gradually increased at the speed of 3A/min, and a coated workpiece is obtained;
(6) Transferring the coated workpiece to a powder spraying line, heating to 120 ℃ and then preserving heat;
(7) And (3) carrying out electrostatic spraying on the surface of the workpiece in heat preservation to obtain a polyester transparent powder coating, heating to 220 ℃ and curing to form a transparent layer with the thickness of 80 mu m, so as to prepare the metal surface protective coating, wherein the protective coating presents gradual change color.
The polyester transparent powder coating comprises 80 parts by weight of polyester resin, 28 parts by weight of curing agent, 25 parts by weight of glass fiber, 2.6 parts by weight of leveling agent, 1.5 parts by weight of defoaming agent and 1 part by weight of antioxidant.
The polyester resin is obtained by polycondensation of neopentyl glycol and terephthalic acid.
Comparative example 4
A method for preparing a protective coating on a metal surface by adopting a vacuum coating process, comprising the following steps:
(1) Polishing the aluminum alloy matrix;
(2) Performing wax removal, oil removal and rust removal cleaning on the polished aluminum alloy substrate;
(3) Transferring the aluminum alloy with the surface cleaned into a vacuum furnace, pumping the vacuum furnace to background vacuum, wherein the vacuum degree is 6.5-9.5X10% -4 During Pa, inert gas is introduced, a bias power supply is started to carry out glow cleaning on the surface of the workpiece when the vacuum degree reaches 0.5-1.5Pa, the bias voltage during glow cleaning is 1200V, the duty ratio is 48%, and the current is 3A;
(4) Pumping air in a vacuum furnace to background vacuum, then introducing inert gas to enable the vacuum degree to reach 0.1-1Pa, controlling the current of an aluminum target to be 30A, controlling the current of a chromium target to be 20A, enabling the flow of the inert gas to be 200sccm, and simultaneously depositing an Al-Cr transition layer with the thickness of 120um on the surface of an aluminum alloy substrate subjected to glow cleaning by adopting a magnetron sputtering method from the aluminum target and the chromium target;
(5) A chromium target, a copper target and a silicon target are simultaneously deposited on the surface of an Al-Cr transition layer by adopting a magnetron sputtering method to form a Cr-Cu-Si color decorative layer with the thickness of 200um, the initial current of the chromium target is controlled to be 45A and gradually reduced at the speed of 3A/min, the current of the copper target is 26A and kept unchanged, the initial current of the silicon target is 10A and gradually increased at the speed of 3A/min, and a coated workpiece is obtained;
(6) Transferring the coated workpiece to a powder spraying line, heating to 120 ℃ and then preserving heat;
(7) And (3) carrying out electrostatic spraying on the surface of the heat-preserving workpiece with an organosilicon modified polyester transparent powder coating, heating to 220 ℃ and curing to form a transparent layer with the thickness of 80um, so as to prepare the metal surface protective coating, wherein the protective coating presents gradual change color.
The organosilicon modified polyester transparent powder coating comprises 80 parts by weight of organosilicon modified polyester resin, 28 parts by weight of curing agent, 25 parts by weight of glass fiber, 2.6 parts by weight of leveling agent, 1.5 parts by weight of defoaming agent and 1 part by weight of antioxidant.
The preparation method of the organosilicon modified polyester resin comprises the following steps:
39 parts by weight of neopentyl glycol and 0.05 part by weight of monobutyl tin oxide are put into a reaction kettle, nitrogen is introduced, 32 parts by weight of dimethyl dimethoxy silane is dropwise added while stirring, meanwhile, the temperature is raised, when the temperature is raised to 190 ℃, the temperature is kept for 2.5 hours, 45 parts by weight of terephthalic acid is added after the temperature is lowered to 150 ℃, then the temperature is raised to 240 ℃ and the temperature is kept for 3 hours, and the organosilicon modified polyester resin is obtained after the temperature is lowered.
Performance testing
The metal surface protective coatings obtained in examples 1 to 3 and comparative examples 1 to 4 were tested for water contact angle according to GB/T30693-2014, adhesion according to GB/T9286-2021, fluorescent ultraviolet aging resistance according to GB/T14522-2008, gloss of the coating surface according to ASTM D523, and gloss retention calculated according to ASTM D523 after baking the metal surface protective coating at 380℃for 4 hours, and the test results are shown in Table 1 below.
TABLE 1
From the above test results, it is known that the adhesion of the coating is obviously reduced when the al—cr transition layer is changed to the Cr transition layer in comparative example 1 based on example 3, the adhesion of the coating is obviously reduced when the chromium target and the silicon target are fixed during the preparation of the color decorative layer in comparative example 2 based on example 3, the water contact angle of the coating is obviously reduced when the silicone modified polyester resin is changed to the common polyester resin in comparative example 3 based on example 3, the anti-fluorescent ultraviolet aging performance is obviously reduced, the glossiness is obviously reduced, the light retention after baking is also obviously reduced, and the water contact angle of the coating is reduced, the anti-fluorescent ultraviolet aging performance is reduced and the light retention after baking is reduced after the trifluoro propyl methyl dimethoxy silane in the synthetic process of the silicone modified polyester resin is changed to the dimethyl dimethoxy silane in comparative example 4 based on example 3.
The present invention is not limited to the above embodiments, but is capable of modification and variation in detail, and other modifications and variations can be made by those skilled in the art without departing from the scope of the present invention.
Claims (7)
1. A method for preparing a metal surface protective coating by adopting a vacuum coating process, which is characterized by comprising the following steps:
(1) Polishing the aluminum alloy matrix;
(2) Cleaning the surface of the polished aluminum alloy matrix;
(3) Transferring the aluminum alloy with the surface cleaned into a vacuum furnace, and carrying out glow cleaning after exhausting to background vacuum;
(4) Depositing an Al-Cr transition layer on the surface of the aluminum alloy matrix subjected to glow cleaning by adopting a magnetron sputtering method from an aluminum target and a chromium target at the same time;
(5) A Cr-Cu-Si color decorative layer is deposited on the surface of the Al-Cr transition layer by a magnetron sputtering method from a chromium target, a copper target and a silicon target at the same time, so as to obtain a coated workpiece;
(6) Transferring the coated workpiece to a powder spraying line, heating and preserving heat;
(7) Electrostatic spraying of organosilicon modified polyester transparent powder coating on the surface of the heat-preserving workpiece, heating and curing to form a transparent layer, and preparing the metal surface protective coating;
the initial current of the chromium target in the step (5) is 35-45A and gradually decreases at a speed of 1-3A/min, the copper target current is 20-30A and remains unchanged, and the initial current of the silicon target is 10-20A and gradually increases at a speed of 2-3A/min;
the organic silicon modified polyester transparent powder coating in the step (7) comprises 60-80 parts by weight of organic silicon modified polyester resin, 10-30 parts by weight of curing agent, 15-25 parts by weight of glass fiber, 2-3 parts by weight of leveling agent, 0.5-1.5 parts by weight of defoaming agent and 0.5-1 part by weight of antioxidant;
the preparation method of the organosilicon modified polyester resin comprises the following steps:
39 parts by weight of neopentyl glycol and 0.05 part by weight of monobutyl tin oxide are put into a reaction kettle, nitrogen is introduced, 32 parts by weight of trifluoropropyl methyl dimethoxy silane is dropwise added while stirring, the temperature is raised, when the temperature is raised to 190 ℃, the temperature is kept for 2.5 hours, 45 parts by weight of terephthalic acid is added after the temperature is lowered to 150 ℃, then the temperature is raised to 240 ℃ and the temperature is kept for 3 hours, and the organosilicon modified polyester resin is obtained after the temperature is lowered.
2. The method for preparing a metal surface protective coating by a vacuum coating process according to claim 1, wherein the surface cleaning in the step (2) is to perform wax removal, oil removal and rust removal cleaning on an aluminum alloy substrate.
3. The method for preparing a protective coating on a metal surface by a vacuum coating process according to claim 1, wherein the glow cleaning process in step (3) is as follows: pumping the vacuum furnace to background vacuum with the vacuum degree of 6.5-9.5X10 -4 And during Pa, introducing inert gas, starting a bias power supply to carry out glow cleaning on the surface of the workpiece when the vacuum degree reaches 0.5-1.5Pa, wherein the bias voltage during glow cleaning is 800-1200V, the duty ratio is 45-70%, and the current is 1.5-4.8A.
4. The method for preparing a metal surface protective coating by vacuum coating process according to claim 1, wherein the conditions of the magnetron sputtering in the step (4) are: pumping air in the vacuum furnace to background vacuum, and then introducing inert gas to enable the vacuum degree to reach 0.1-1Pa; the aluminum target current is 15-30A, the chromium target current is 10-20A, and the inert gas flow is 80-200sccm.
5. The method for producing a protective coating on a metal surface according to claim 1, wherein the heating temperature in step (6) is 90-120 ℃.
6. The method for preparing the metal surface protective coating by adopting the vacuum coating process according to claim 1, wherein the thickness of the Al-Cr transition layer is 80-120um, the thickness of the Cr-Cu-Si color decorative layer is 100-200um, and the thickness of the transparent layer is 60-80um.
7. The method for producing a protective coating on a metal surface according to claim 1, wherein the heating temperature in step (7) is 200-220 ℃.
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| JPH07166370A (en) * | 1993-12-15 | 1995-06-27 | Kobe Steel Ltd | Al based plated steel sheet excellent in high temperature discoloration resistance and production thereof |
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| TW201413018A (en) * | 2012-09-27 | 2014-04-01 | Toshima Mfg Company Ltd | Sputtering target for optical medium recording layer |
| CN103774100A (en) * | 2012-10-22 | 2014-05-07 | 中环股份有限公司 | Sputtering target and recordable optical recording media |
| KR101467120B1 (en) * | 2013-11-15 | 2014-12-03 | 유흥상 | decorating material product method method of shoe outsole |
| CN110004412A (en) * | 2019-05-09 | 2019-07-12 | 宁波威霖住宅设施有限公司 | A kind of allumen process of surface treatment |
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| JP3143605U (en) * | 2008-05-01 | 2008-07-31 | 株式会社浜野メッキ | Surface decoration structure of articles |
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| JPH07166370A (en) * | 1993-12-15 | 1995-06-27 | Kobe Steel Ltd | Al based plated steel sheet excellent in high temperature discoloration resistance and production thereof |
| KR20070096105A (en) * | 2005-12-24 | 2007-10-02 | 키스타 주식회사 | Coloring method of electronic part |
| TW201413018A (en) * | 2012-09-27 | 2014-04-01 | Toshima Mfg Company Ltd | Sputtering target for optical medium recording layer |
| CN103774100A (en) * | 2012-10-22 | 2014-05-07 | 中环股份有限公司 | Sputtering target and recordable optical recording media |
| KR101467120B1 (en) * | 2013-11-15 | 2014-12-03 | 유흥상 | decorating material product method method of shoe outsole |
| CN110004412A (en) * | 2019-05-09 | 2019-07-12 | 宁波威霖住宅设施有限公司 | A kind of allumen process of surface treatment |
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