NL2030813B1 - Method for Strengthening Aluminum Alloy Surface Coating - Google Patents

Method for Strengthening Aluminum Alloy Surface Coating Download PDF

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NL2030813B1
NL2030813B1 NL2030813A NL2030813A NL2030813B1 NL 2030813 B1 NL2030813 B1 NL 2030813B1 NL 2030813 A NL2030813 A NL 2030813A NL 2030813 A NL2030813 A NL 2030813A NL 2030813 B1 NL2030813 B1 NL 2030813B1
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aluminum alloy
coating
reinforcing
aluminium alloy
fluoride
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NL2030813A
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Li Cong
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Univ Changsha Sci & Tech
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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
    • C25D3/04—Electroplating: Baths therefor from solutions of chromium
    • C25D3/08—Deposition of black chromium, e.g. hexavalent chromium, CrVI
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
    • 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
    • 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
    • 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
    • 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
    • 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
    • C23C28/3455—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 with a refractory ceramic layer, e.g. refractory metal oxide, ZrO2, rare earth oxides or a thermal barrier system comprising at least one refractory oxide layer
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C25D5/42—Pretreatment of metallic surfaces to be electroplated of light metals
    • C25D5/44—Aluminium
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F4/00—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00

Abstract

Disclosed is an aluminium alloy surface coating strengthening method, which belongs to the technical field of metal material processing. The method comprises the following steps: firstly, immersing the aluminium alloy in titanium fluoride/zirconium fluoride solution to form an Ales - ZrOZ - TlOz transition film, then carrying out chromium plating treatment, carrying out microwave plasma etching after completion, then taking AlCrN target as a target material, continuously depositing PVD hard film on the surface and carrying out low - temperature aging treatment; According to the invention, firstly, the Ales - ZrOZ - TlOz transition film is formed on the surface of the aluminium alloy, then chromium plating, microwave plasma etching, and then PVD hard film is deposited, so that not only the wear resistance of the aluminium alloy is significantly improved, but also the bonding strength between the PVD hard film and the substrate is improved, and the service life of the PVD hard film is effectively prolonged.

Description

Method for Strengthening Aluminium Alloy Surface Coating
TECHNICAL FIELD The invention belongs to the technical field of metal material processing, and in particular relates to an aluminium alloy surface coating strengthening method.
BACKGROUND Aluminium alloy is an alloy based on aluminium and added with a certain amount of other alloying elements. It is one of the light metal materials. In addition to the general characteristics of aluminium, aluminium alloys have some specific characteristics of alloys due to different kinds and amounts of alloying elements. The density of aluminium alloy is 2.63 - 2.85 g/cm? which has high strength, the specific strength is close to that of high alloy steel, and the specific rigidity is higher than that of steel. It has good castability and plastic workability, good electrical and thermal conductivity, good corrosion resistance and weldability. It can be used as structural materials and is widely used in aerospace, aviation, transportation, construction, electromechanical, light industry and daily necessities. However, aluminium alloy parts have low surface hardness and poor wear resistance, which are prone to wear, crack, fatigue and so on during service, leading to parts failure and economic losses. Therefore, it is necessary to improve the surface mechanical properties, hardness and wear resistance of aluminium alloy parts. Physical vapor deposition (PVD) hard coating has high surface hardness, stable chemical inertness, good thermal stability and corrosion resistance, which can effectively prolong the service life of aluminium alloy parts, reduce production costs and ensure the quality of processed products. However, PVD hard coating deposited directly on the surface of aluminium alloy has some problems, such as poor adhesion between film and substrate, and the coating is easy to crack under heavy load. Therefore, when PVD hard coating is deposited on the surface of aluminium alloy by physical vapor deposition to improve its hardness, how to improve the bonding strength between substrate and hard coating and its bearing capacity is an urgent technical problem to be solved.
SUMMARY Aiming at the above - mentioned shortcomings in the prior art, the invention provides a method for strengthening aluminium alloy surface coating.
To achieve the above purpose, the present invention provides the following technical scheme: The invention provides a method for strengthening coating on the surface of aluminium alloy, which comprises the following steps: firstly, immersing aluminium alloy in titanium fluoride/zirconium fluoride solution to form Al2O3 - ZrO; - TiO: transition film, then performing chromium plating treatment, performing microwave plasma etching after completion, and then taking AICrN target as target material, continuously depositing PVD hard film on the surface and performing low - temperature aging treatment. Further, the titanium fluoride/zirconium fluoride solution takes hydrofluoric acid as a solvent, the concentration of titanium fluoride is 40 - 45 mg 1, the concentration of zirconium fluoride is 15-20 mg/l, and the pH of the titanium fluoride/zirconium fluoride solution is 3 - 3.5; The immersion time of the aluminium alloy in the titanium fluoride/zirconium fluoride solution is 80 to 90 seconds. Furthermore, the electrolyte used in the chromium plating treatment includes 200 - 250 gl chromic anhydride, 2.0 - 2.5 g/l sulfuric acid and 3.0 - 6.0 g/l trivalent chromium. Further, the current density during the chromium plating treatment is 50 - 90 A/dm?, and the temperature is 50 - 70°C. Further, the plasma used in the microwave plasma etching is argon plasma, and the argon flow rate is 300 - 350 sccm. Further, the microwave plasma etching temperature is 450 - 500°C, the pressure is 13 - 15 kPa, and the time is 3 - 5 min. Furthermore, in the PVD hard film deposition process, the sample bias voltage is - 100 - - 150 V, and the deposition time is 4 - 5 hours under the nitrogen atmosphere, the pressure is 3 - 5 Pa, the temperature is 420 - 460°C, the target current is 70 - 110 A. Further, the temperature of the low - temperature aging treatment is 170 - 180°C and the timeis 24h. Further, the aluminium alloy includes 2000 series, 5000 series, 6000 series and 7000 series aluminium alloys. Compared with the prior art, the invention has the following beneficial effects: according to the invention, firstly, the Al:O3 - ZrO; - TiO; transition film is formed on the surface of the aluminium alloy, then chromium plating, microwave plasma etching, and then PVD hard film is deposited, so that not only the wear resistance of the aluminium alloy is significantly improved, but also the bonding strength between the PVD hard film and the substrate is improved, and the service life of the PVD hard film is effectively prolonged.
DESCRIPTION OF THE INVENTION Now, various exemplary embodiments of the present invention will be described in detail. This detailed description should not be considered as a limitation of the present invention, but should be understood as a more detailed description of some aspects, characteristics and embodiments of the present invention. It should be understood that the terms used in this invention are only for describing specific embodiments, and are not used to limit the invention. In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper limit and the lower limit of the range is also specifically disclosed. Any stated value or intermediate value within the stated range and any other stated value or every smaller range between intermediate values within the stated range are also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded from the range. Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by the ordinary technicians in the field of this invention.
Although the present invention only describes the preferred methods and materials, any methods and materials similar or equivalent to those described herein can also be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and/or materials related to the documents. In case of conflict with any incorporated documents, the contents of this specification shall prevail. Without departing from the scope or spirit of the present invention, it is obvious to those skilled in the art that many modifications and changes can be made to the specific embodiments of the present invention. Other embodiments obtained from the description of the present invention will be obvious to the skilled person. The description and example of that present invention are exemplary only.
The words “including”, "comprising", "having" and "containing" used in this paper are all open terms, that is, they mean including but not limited to. Embodiment 1 The surface of 6061 aluminium alloy is coated and strengthened, including the following steps: (1) preparing a hydrofluoric acid solution of titanium fluoride/zirconium fluoride, wherein the concentration of titanium fluoride is 43 mg /I, the concentration of zirconium fluoride is 18 mg /l, and the pH of the solution is 3.2; (2) immersing the aluminium alloy sample in the hydrofluoric acid solution of titanium fluoride/zirconium fluoride prepared in step (1) for 75 s to form an Al;O: - ZrO; - TiO» transition film on the surface of the sample; (3) chromium plating is carried out on the sample obtained in step (2), the electroplating solution includes 220 g /l chromic anhydride, 2.2 g/l sulfuric acid and 4.5 g /l trivalent chromium, and electroplating is carried out at the current density of 70 A/dm? and the temperature of 60°C to obtain chromium - plated aluminium alloy; (4) placing the chromium - plated aluminium alloy obtained in step (3) in a microwave chemical vapor deposition system, sealing the cavity, vacuumizing to 0.1 Pa, then introducing argon at a flow rate of 320 sccm, turning on the microwave when the pressure reaches 2 Kpa, generating argon plasma, then adjusting the pressure to 14 KPa and the temperature to 470°C, and etching with argon plasma for 4 min; (5) depositing a PVD hard film on the surface of the sample obtained by argon plasma etching in step (4): putting the sample into a PVD furnace with a vacuum degree of 2Pa and an
AICrN target as the target, opening the target, introducing nitrogen to make the pressure 4 Pa, controlling the sample temperature at 440°C and the target current 90 A, and depositing for 4.5 h hours to obtain the PVD hard film; after that, low - temperature aging treatment is carried out at 175°C for 24 hours, and 8061 aluminium alloy with enhanced surface coating is obtained.
Its surface hardness is 3,120 HV, and its wear resistance is significantly improved.
Embodiment 2 The surface of 5083 aluminium alloy is coated and strengthened, including the following steps: (1) preparing a hydrofluoric acid solution of titanium fluoride/zirconium fluoride, wherein the concentration of titanium fluoride is 40 mg /I, the concentration of zirconium fluoride is 15 mg /l, and the pH of the solution is 3; (2) immersing the aluminium alloy sample in the hydrofluoric acid solution of titanium fluoride/zirconium fluoride prepared in step (1) for 60s to form an Al,Os - ZrO; - TiO: transition film on the surface of the sample; (3) chromium plating is carried out on the sample obtained in step (2), wherein the electroplating solution comprises 200 g /I chromic anhydride, 2.0 g /I sulfuric acid and 3.0 g /I trivalent chromium, and electroplating is carried out under the conditions of current density of 50 A/dm? and temperature of 50°C to obtain chromium - plated aluminium alloy; (4) placing the chromium - plated aluminium alloy obtained in step (3) in a microwave chemical vapor deposition system, sealing the cavity, vacuumizing to 0.1 Pa, then introducing argon at a flow rate of 300 sccm, turning on the microwave when the pressure reaches 2 Kpa, generating argon plasma, then adjusting the pressure to 13 KPa and the temperature to 450°C, and etching with argon plasma for 5 minutes; (5) depositing a PVD hard film on the surface of the sample obtained by argon plasma etching in step (4): putting the sample into a PVD furnace with a vacuum degree of 0.5 Pa and an AICrN target as the target, turning on the target, introducing nitrogen, controlling the pressure at 3 Pa, controlling the sample temperature at 420°C and the target current at 70 A, and depositing for 5 hours to obtain the PVD hard film; After that, low - temperature aging treatment is carried out at 170°C for 24 hours, and 5083 aluminium alloy with enhanced surface coating is obtained.
Its surface hardness is 3,110 HV, and its wear resistance is significantly improved.
Embodiment 3 The surface of 7075 aluminium alloy is coated and strengthened, including the following steps:
(1) preparing a hydrofluoric acid solution of titanium fluoride/zirconium fluoride, wherein the concentration of titanium fluoride is 45 mg /l, the concentration of zirconium fluoride is 20 mg /l, and the pH of the solution is 3.5; (2) immersing the aluminium alloy sample in the hydrofluoric acid solution of titanium 5 fluoride/zirconium fluoride prepared in step (1) for 90 seconds to form an Al2O3 - ZrO: - TiO: transition film on the surface of the sample; (3) chromium plating treatment is carried out on the sample obtained in step (2), wherein the electroplating solution comprises 250 g /I chromic anhydride, 2.5 g /I sulfuric acid and 6.0 g fl trivalent chromium, and electroplating is carried out at the current density of 90 A/dm? and the temperature of 70°C to obtain chromium - plated aluminium alloy; (4) placing the chromium - plated aluminium alloy obtained in step (3) in a microwave chemical vapor deposition system, sealing the cavity, vacuumizing to 0.1 Pa, then introducing argon at a flow rate of 350 sccm, turning on the microwave when the pressure reaches 2 Kpa, generating argon plasma, then adjusting the pressure to 15 KPa and the temperature to 500°C, and etching with argon plasma for 3 minutes; (5) depositing a PVD hard film on the surface of the sample obtained by argon plasma etching in step (4): putting the sample into a PVD furnace with a vacuum of 3 Pa and an AICrN target as the target, opening the target, introducing nitrogen to make the pressure 5Pa, controlling the sample temperature at 460°C and the target current 110 A, and depositing for 4 hours to obtain the PVD hard film; after that, low - temperature aging treatment is carried out at 180°C for 24 hours, and 7075 aluminium alloy with enhanced surface coating is obtained. Its surface hardness is 3,140 HV, and its wear resistance is significantly improved.
According to GB5933 - 1986 - Adhesion Testing Method of the Metal Deposits for The Light Industrial Products”, the bonding strength between the coating and the substrate of the products prepared in Embodiments 1 - 3 is tested. In bending test, file test and thermal shock test, no peeling, even cracking and peeling phenomenon occurred in the coating of each embodiment. It can be seen that the bonding strength between the coating and the substrate obtained by the method of the present invention is high.
What has been described above is only a preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto. Any person familiar with the technical field who makes equivalent replacement or change within the technical scope disclosed by the present invention according to the technical scheme and inventive concept of the present invention should be covered within the scope of protection of the present invention.

Claims (9)

CONCLUSIESCONCLUSIONS 1. Een werkwijze voor het versterken van de deklaag op het oppervlak van een aluminiumlegering, welke werkwijze de volgende stappen omvat: — eerst het onderdompelen van een aluminiumlegering in een oplossing van titaanfluoride en zirkoniumfluoride om een Al2O3 - ZrO2 - TiO2 overgangsfilm te vormen, — vervolgens het uitvoeren van een verchromingsbehandeling, — na voltooing het uitvoeren van microgolf plasma etsen, en vervolgens — het nemen van AICrN als doelwitmateriaal, — het door fysieke dampafzetting (PVD) continu aanbrengen van een harde film op het oppervlak en — het uitvoeren van een verouderingsbehandeling bij lage temperatuur.A method for reinforcing the coating on the surface of an aluminum alloy, the method comprising the steps of: — first immersing an aluminum alloy in a solution of titanium fluoride and zirconium fluoride to form an Al2O3 - ZrO2 - TiO2 transition film, — then performing a chromium plating treatment, — after completion, performing microwave plasma etching, and then — taking AICrN as target material, — continuously applying a hard film to the surface by physical vapor deposition (PVD), and — performing a low temperature aging treatment. 2. De werkwijze voor het versterken van de deklaag op het oppervlak van een aluminiumlegering volgens conclusie 1, met het kenmerk dat de titaanfluoride/zirkoniumfluoride-oplossing fluorwaterstofzuur als oplosmiddel neemt, de concentratie van titaanfluoride 40 - 45 mg/l is, de concentratie van zirkoniumfluoride 15 - 20 mg/l is, en de pH van de titaanfluoride/zirkoniumfluoride-oplossing 3 - 3 is. 5; de onderdompeltijd van de aluminiumlegering in de titaanfluoride/zirkoniumfluoride-oplossing bedraagt 60 tot 90 seconden.The method for reinforcing the coating on the surface of an aluminum alloy according to claim 1, characterized in that the titanium fluoride/zirconium fluoride solution takes hydrofluoric acid as a solvent, the concentration of titanium fluoride is 40-45 mg/l, the concentration of zirconium fluoride is 15-20 mg/l, and the pH of the titanium fluoride/zirconium fluoride solution is 3-3. 5; the immersion time of the aluminum alloy in the titanium fluoride/zirconium fluoride solution is 60 to 90 seconds. 3. De werkwijze voor het versterken van de deklaag op het oppervlak van een aluminiumlegering volgens conclusie 1, met het kenmerk dat de elektrolyt die bij de verchroomingsbehandeling wordt toegepast: 200 - 250 g/l chroomzuuranhydride, 2,0 - 2,5 g/l zwavelzuur en 3,0 - 6,0 g/l driewaardig chroom omvat.The method for reinforcing the coating on the surface of an aluminum alloy according to claim 1, characterized in that the electrolyte used in the chrome plating treatment is: 200 - 250 g/l chromic anhydride, 2.0 - 2.5 g/l l sulfuric acid and 3.0 - 6.0 g/l trivalent chromium. 4. De werkwijze voor het versterken van de deklaag op het oppervlak van een aluminiumlegering volgens conclusie 3, met het kenmerk dat de stroomdichtheid tijdens het verchromen 50 - 90 A/dm2 bedraagt en de temperatuur 50 - 70°C bedraagt.The method for reinforcing the coating on the surface of an aluminum alloy according to claim 3, characterized in that the current density during chrome plating is 50 - 90 A/dm 2 and the temperature is 50 - 70°C. 5. De werkwijze voor het versterken van de deklaag op het oppervlak van een aluminiumlegering volgens conclusie 1, met het kenmerk dat het plasma dat voor het etsen in microgolfplasma wordt gebruikt argonplasma is en dat het argondebiet 300 - 350 sccm bedraagt.The method for reinforcing the coating on the surface of an aluminum alloy according to claim 1, characterized in that the plasma used for the microwave plasma etching is argon plasma and the argon flow rate is 300-350 sccm. 6. De werkwijze voor het versterken van de deklaag op het oppervlak van een aluminiumlegering volgens conclusie 5, met het kenmerk dat bij het microgolfplasma etsen de temperatuur 450 - 500°C bedraagt, de druk 13 - 15 kPa bedraagt, en de tijd 3 - 5 min. bedraagt.The method for reinforcing the coating on the surface of an aluminum alloy according to claim 5, characterized in that in the microwave plasma etching, the temperature is 450 - 500°C, the pressure is 13 - 15 kPa, and the time is 3 - 5 minutes. 7. De werkwijze voor het versterken van de deklaag op het oppervlak van een aluminiumlegering volgens conclusie 1, met het kenmerk dat in het PVD-depositieproces van de harde film de voorspanning van het monster -100 tot -150 V is, en de depositietijd 4 - 5 uur bedraagt bij een druk van 3 - 5 Pa, een temperatuur van 420 - 460°C en een doelstroom van 70 - 110 A.The method for reinforcing the coating on the surface of an aluminum alloy according to claim 1, characterized in that in the PVD deposition process of the hard film, the bias voltage of the sample is -100 to -150 V, and the deposition time is 4 - 5 hours at a pressure of 3 - 5 Pa, a temperature of 420 - 460°C and a target current of 70 - 110 A. 8. De werkwijze voor het versterken van de deklaag op het oppervlak van een aluminiumlegering volgens conclusie 1, met het kenmerk dat de temperatuur van de verouderingsbehandeling bij lage temperatuur 170 - 180°C bedraagt en de tijdsduur 24 uur bedraagt.The method for reinforcing the coating on the surface of an aluminum alloy according to claim 1, characterized in that the temperature of the low-temperature aging treatment is 170-180°C and the time is 24 hours. 9. De werkwijze voor het versterken van de deklaag op het oppervlak van een aluminiumlegering conclusie 1, met het kenmerk dat de aluminiumlegering aluminiumlegeringen omvat van de 2000 reeks, de 5000 reeks, de 6000 reeks en de 7000 reeks.The method for reinforcing the coating on the surface of an aluminum alloy, characterized in that the aluminum alloy includes aluminum alloys of 2000 series, 5000 series, 6000 series and 7000 series.
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