CN113122845A - Preparation method of aluminum alloy metal plated part - Google Patents

Preparation method of aluminum alloy metal plated part Download PDF

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CN113122845A
CN113122845A CN202110364117.8A CN202110364117A CN113122845A CN 113122845 A CN113122845 A CN 113122845A CN 202110364117 A CN202110364117 A CN 202110364117A CN 113122845 A CN113122845 A CN 113122845A
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copper
nickel
solution
plating
temperature
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CN113122845B (en
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郑小宝
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Kunshan Luxin New Material Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/021—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal alloy layer
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
    • C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
    • C23C18/1837—Multistep pretreatment
    • C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
    • C23C18/1848—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by electrochemical pretreatment
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/48—Coating with alloys
    • C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
    • 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
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/20—Acidic compositions for etching aluminium or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/16—Pretreatment, e.g. desmutting
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/24—Chemical after-treatment
    • 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
    • C25D3/38—Electroplating: Baths therefor from solutions of copper
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00—Electrolytic etching or polishing
    • C25F3/16—Polishing
    • C25F3/18—Polishing of light metals
    • C25F3/20—Polishing of light metals of aluminium

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  • Thermal Sciences (AREA)
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  • Electroplating Methods And Accessories (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

The invention provides a preparation method of an aluminum alloy metal plated part, which can obviously improve the bonding force of an aluminum material and a copper layer, effectively improve the corrosion resistance of a plating layer, and has the advantages of bright, uniform and continuous surface, no peeling, shedding and local roughness.

Description

Preparation method of aluminum alloy metal plated part
Technical Field
The invention relates to a preparation method of an aluminum alloy metal plated part, in particular to a preparation method of electroplating copper alloy on an aluminum alloy.
Background
With the rapid development of electronic information technology, the Printed Circuit Board (PCB) industry develops rapidly. Copper electroplating is an important process in the manufacture of PCB boards. The purpose of the copper electroplating of the printed circuit board is to further electroplate and thicken the through holes or blind holes of the double-sided board or the multilayer board on the basis of hole metallization electroplating, so as to realize reliable interconnection between layers.
The metal-based copper-clad plate is divided according to different metal materials, and the types of the metal-based copper-clad plate mainly include three types: the copper-based copper-clad plate, the iron-based copper-clad plate and the aluminum-based copper-clad plate are low in density of aluminum alloy, good in corrosion resistance, high in fatigue resistance, high in specific strength and specific stiffness, equivalent to structural steel and even ultra-high strength steel, and widely applied to preparation of mobile phone components so as to reduce the weight of mobile phone structures. But the aluminum alloy has low hardness and poor wear resistance, and the surface hardness and the wear resistance can be greatly improved after chemical nickel plating. The plating on the aluminum alloy is more difficult and complicated than the plating on metal materials such as steel, iron, copper and the like, and because of the active property, the surface is easy to react with oxygen in the air to generate a layer of oxide film, and the existence of the oxide film hinders the further surface treatment of the aluminum alloy; meanwhile, the electrode potential of the aluminum is very negative, and the aluminum can perform a displacement reaction with various metal ions when immersed in the plating solution to generate a contact plating layer on the aluminum, so that the bonding strength of the plating layer and an aluminum substrate is reduced.
In order to improve the above technical problems, the prior art, such as CN108265281A vinca intelligent technology limited, provides a method for preparing an aluminum alloy composite material, comprising: and sequentially carrying out alkali washing, acid etching, first zinc dipping, zinc removing, second zinc dipping, chemical copper plating and chemical nickel and phosphorus alloy plating on the aluminum alloy to obtain the aluminum alloy composite material. The preparation method of the aluminum alloy composite material provided by the invention can better plate the nickel-phosphorus alloy on the surface of the aluminum alloy, and the obtained aluminum alloy plating layer has the advantages of bright, uniform and continuous surface, no peeling, falling off and local roughness. In addition, the aluminum alloy composite material provided by the invention contains the copper layer, so that the aluminum alloy composite material has good corrosion resistance. CN104213168A A magnesium alloy surface nickel electroplating process for notebook computer shells, which is characterized by comprising the following steps: the invention selects the plating solution of zinc immersion, cyanide-free copper electroplating and nickel electroplating and adjusts the content, so that the plating solution has stable performance and the chromium plating layer prepared finally has strong binding force. Cyanide is not adopted in the whole plating process, the amount of the selected fluoride is less than that of the fluoride used in the prior art, and the plating process is environment-friendly. Namely, zinc immersion is carried out to cause the displacement reaction of the aluminum material and zinc, and then the surface is galvanized.
The current relatively mature process for chemical nickel plating on the surface of aluminum alloy is a zinc dipping method, namely a process of chemical nickel plating after zinc dipping. The zinc dipping method forms a transition zinc layer on the surface of the aluminum, can prevent the surface of the aluminum from generating an oxide film again, can prevent the aluminum from contacting with a nickel plating solution, and improves the binding force of a plating layer. However, the zinc dipping method has the disadvantages of complex process, difficult treatment of the zinc dipping solution and the like, and the zinc dipping layer has a displacement reaction with nickel ions in the chemical nickel plating solution, so the generated zinc ions poison the plating solution, and the service life of the plating solution is shortened. The nickel pre-plating method has simple process and can overcome the defects brought by the zinc dipping method, but key process conditions such as the molar ratio of the complexing agent to nickel ions, the pH value of the plating solution and the like need to be strictly controlled to obtain excellent plating effect.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a plating piece processing method which can form a layer on the surface of the aluminum alloy, has high binding force and strong corrosion resistance, has high efficiency and simple operation, and can improve the quality of aluminum alloy products.
A preparation method of an aluminum alloy metal plated part comprises the following preparation methods:
(1) mechanical polishing, alkaline degreasing, heat treatment and electrochemical polishing;
(2) anodizing;
(3) removing the anodic oxide film;
(4) adsorption of nickel and copper ions
(5) Chemical nickel-phosphorus plating alloy
(6) And (4) electroplating copper.
In some embodiments, the mechanical polishing uses a white paste to polish to a mirror surface with a surface roughness Ra of 0.1-0.3 μm, and the alkaline degreasing is 7g/L trisodium phosphate and 20g/L aqueous sodium carbonate at a temperature of 75 deg.CoC。
In some embodiments of the present invention, the,the heat treatment temperature is 420 DEGoC, the time is 5h, the electrochemical polishing uses nitrogen atmosphere, the volume ratio of the electrochemical polishing used is perchloric acid and ethanol mixed solution, the current density is 700mA/cm2And the time is 3 min.
In some embodiments, the anode is oxidized to a 0.4-0.45M sulfuric acid solution in a solvent in a volume ratio of 2: (3-4) deionized water and ethylene glycol, wherein the voltage of anodic oxidation is 20V, and the time is 30-40 min.
In some embodiments, 6wt.% H is used for removing anodized film3PO4With 1.8wt.% of H2CrO4The mixed solution of (2) is at 60oAnd C, removing, washing with deionized water between the step (3) and the step (4) to be neutral, and drying in vacuum.
In some embodiments, the copper ion adsorption solution comprises 10-15g/L copper sulfate, 2-3g/L nickel sulfate, 5-6g/L citric acid complexing agent, 1-2g/L phytic acid stabilizer and deionized water, and the soaking time is 1-2 min.
In some embodiments, the solution of the electroless nickel-phosphorus alloy plating is 10-20g/L of nickel sulfate main salt, 10-15g/L of sodium hypophosphite reducing agent, 5-7g/L of hydroxyacetic acid complexing agent, 0.1-0.5g/L of mercaptobenzothiazole stabilizer, 1-2g/L of lanthanum chloride additive, and ammonia water is used for adjusting the pH to be 5.2 +/-0.2 and the temperature to be 50-60 DEGoC。
In some embodiments, the electroless nickel-phosphorous plating time is 10-20min and the thickness is 7-12 μm.
In some embodiments, the electrolytic solution for electroplating copper comprises 170g/L of 140-140 g/L of copper sulfate, 40-50g/L of sulfuric acid, and Cl-60-70ppm, 0.05-0.0.07 g/L of diazeniumphenyl black, 0.02-0.04g/L of polyethylene glycol and 0.01-0.04g/L of sodium polydithio dipropyl sulfonate.
In some embodiments, the electrolytic solution temperature of the electrolytic copper plating is 25 to 30 deg.CoC, current density 1-2A/dm2The thickness is 14-24 μm.
First, as known to those skilled in the art, aluminum has active chemical properties, negative standard electrode potential, and is easily reacted with oxygen in air to form a dense oxide film, and even after pretreatment such as degreasing and alkaline etching, the oxide film is rapidly formed at the moment of air contact when the aluminum is taken out, so that the bonding force between the copper plating layer obtained after copper electroplating and the aluminum substrate is affected, and thus, an appropriate aluminum material pretreatment means must be adopted.
The pretreatment means of the invention comprises mechanical polishing, alkaline degreasing, heat treatment and electrochemical polishing:
the polishing paste used for the mechanical polishing is white polishing paste polished to a mirror surface, and the surface roughness Ra is 0.1-0.3 mu m.
The alkaline oil removal is 7g/L trisodium phosphate and 20g/L sodium carbonate aqueous solution at the temperature of 75oC。
The heat treatment temperature is 420 DEGoAnd C, the time is 5 hours, and the atmosphere is nitrogen.
The electrochemical polishing is carried out by mixing perchloric acid and ethanol at a volume ratio of 1:10 and at a current density of 700mA/cm2And the time is 3 min.
The mechanical polishing is mainly used for removing non-good impurities and large-particle chips on the surface of the metal, improving the surface flatness of the metal aluminum material and obtaining the mirror surface effect.
The alkaline degreasing is mainly used for degreasing, the uniformity of subsequent anodic oxidation treatment is improved, and if grease on the metal surface cannot be effectively removed, the uniformity of anodic oxidation array pore channels is directly influenced.
The heat treatment is mainly used for removing internal stress of the metal aluminum material, and the internal stress directly influences the bonding force of the thickness coating and the aluminum material.
The chemical polishing is mainly to further improve the surface smoothness of the aluminum material and reduce the roughness, and meanwhile, although nitrogen is used for protection in the heat treatment process, oxygen or other oxides cannot react with active aluminum material through oxidation reaction, so that further surface expression is needed.
Secondly, carrying out anodic oxidation on the aluminum material, wherein the anodic oxidation is 0.4-0.45M sulfuric acid solution, and the volume ratio of the solvent is 2: (3-4) deionized water and ethylene glycol, wherein the voltage of anodic oxidation is 20V, and the time is 30-40 min. The main purpose of the anodic oxidation is not to obtain an anodic oxide film or an aluminum oxide layer, but to form uniform and tiny pores on the flat surface of the aluminum material, and after the anodic oxidation treatment, the anodic oxide film is formed on the surface of the aluminum material, wherein the pores of the oxide film are between 50 nm and 70nm, and the pores are uniformly distributed, as shown in schematic figure 1.
Although the oxide film is uniform, the anodic aluminum oxide and the subsequent electroless nickel plating solution cannot undergo a displacement reaction, a metal layer cannot be formed, and the subsequent conductive electrolytic copper plating is not facilitated, so that 6wt.% of H passes through3PO4With 1.8wt.% of H2CrO4The mixed solution of (2) is at 60oAnd C, removing an oxidation film, wherein the process removes the barrier layer alumina and the porous layer alumina on the surface of the aluminum material, but still obtains uniform pore-shaped aluminum metal on the surface of the aluminum material, as shown by the SEM in fig. 2 and the AFM in fig. 3, wherein the pore-shaped aluminum material surface is important for subsequent adsorption.
As known to those skilled in the art, when an aluminum substrate is placed in an electroplating solution, since the electroplating solution is acidic, aluminum reacts with sulfuric acid and also undergoes a displacement reaction with copper ions to form a displacement layer on the surface of the aluminum substrate, and the obtained film is rough and loose and has poor bonding strength with the aluminum substrate.
Therefore, in the prior art, copper can not be directly electroplated on the surface of the aluminum material, such as zinc dipping treatment, the invention adopts copper ion adsorption solution to treat the surface of the aluminum material, wherein the copper ion adsorption solution comprises 10-15g/L of copper sulfate, 2-3g/L of nickel sulfate, 5-6g/L of citric acid complexing agent, 1-2g/L of phytic acid stabilizer and deionized water, and the soaking time is 1-2 min.
During the soaking process, the following reactions occur: (1) cu2++Al→Cu+Al3+；Cu2++Al→Cu++Al3+
（2）Ni2++Al→Ni+Al3+；
Due to the restriction of the metal activity order table and the concentration of copper ions in the adsorption solution is significantly higher than that of nickel ions, only the chemical reaction formula (1) will occur during the adsorption process, i.e. the adsorption process will occurCopper particles can be formed on the surface of the aluminum material, and as known by the technical personnel in the field, when two metals with different reactivities exist simultaneously, a galvanic cell corrosion phenomenon can be formed due to potential difference, and the copper particles are used as positive electrodes in the process to obtain electrons; the aluminum substrate is used as a negative electrode, and electrons are lost, and the lost electrons are easy to be Ni2+Trapping thereby making Ni2++2e-→ Ni, the presence of the nickel ions as a catalyst is able to catalyze the subsequent electroless nickel phosphorous plating process.
It should be noted that, in the present invention, nano-pores are formed by anodic oxidation, and the anodic oxide film is removed to expose the aluminum material with pores, the micropores on the surface of the aluminum material can generate a significant acceleration effect on the corrosion process of the galvanic cell to accelerate the formation of catalytic nickel particles, and at the same time, the pores are beneficial to the subsequent bonding strength of the nickel-phosphorus alloy and the substrate, i.e. the control of the surface morphology of the aluminum material is indispensable.
As known to those skilled in the art, for electroless nickel plating, metals having catalytic activity for sodium hypophosphite include Pd and Ni, and Cu has no catalytic activity, and through the adsorption process, copper particles and nickel particles are simultaneously formed on the surface of the aluminum material, the nickel particles can continuously catalyze the sodium hypophosphite to chemically reduce nickel sulfate, and electroless nickel-phosphorus alloy is formed on the surface of the aluminum material, and the thickness of the electroless nickel-phosphorus alloy is 7-12 μm as shown in figure 6.
The technological parameters of the chemical nickel plating are as follows: the solution of the chemical nickel-phosphorus plating alloy is 10-20g/L of nickel sulfate main salt, 20-25g/L of sodium hypophosphite reducing agent, 5-7g/L of hydroxyacetic acid complexing agent, 0.1-0.5g/L of mercaptobenzothiazole stabilizer, 1-2g/L of lanthanum chloride additive, ammonia water is used for adjusting the pH to be 5.2 +/-0.2, and the temperature is 50-60oC。
The invention adopts nickel sulfate as main salt, the optional nickel salt is nickel sulfamate or nickel acetate, the use of nickel chloride is strictly forbidden, when the nickel chloride is used as metal main salt, obvious coating stress can be generated, and when nickel phosphorus is used as an intermediate layer, the binding force can be influenced when the coating stress exists.
The invention uses sodium hypophosphite as a reducing agent, the reaction process of chemical nickel plating known to those skilled in the art is an autocatalytic oxidation-reduction process, under the catalytic action of the nickel particles, the sodium hypophosphite can continuously reduce nickel sulfate, and it is clear that the concentration of the sodium hypophosphite is increased, the deposition speed of the plating layer is increased, the phosphorus content in the plating layer is also increased, the phosphorus enables the stable potential of the plating layer to be positive, and the higher the phosphorus content is, the more positive the stable potential is, that is, generally speaking, the corrosion resistance of the plating layer is enhanced along with the increase of the phosphorus content. However, the phosphorus content is not the only factor influencing the corrosion resistance of the coating, and the higher the phosphorus content is, the better the corrosion resistance can not be generally considered, so the dosage of the sodium hypophosphite should be properly controlled, and the dosage of the sodium hypophosphite reducing agent of the invention is 10-15 g/L.
In addition, the chemical nickel and phosphorus plating solution also contains 5-7g/L of hydroxyacetic acid complexing agent, 0.1-0.5g/L of mercaptobenzothiazole stabilizer and 1-2g/L of lanthanum chloride additive, for hydroxyacetic acid, phosphorous acid ion is accumulated in the solution and combined with free nickel ion to generate nickel phosphite precipitate, and in order to prevent the generation of the nickel phosphite ion, a proper complexing agent is required to be added to generate a complex ion beam of nickel to reduce the concentration of the free nickel ion, and in addition, the mercaptobenzothiazole stabilizer and rare earth element are both additives for improving nickel and phosphorus plating.
Finally, electroplating copper on the nickel-phosphorus intermediate layer, wherein the electrolyte of the electroplating copper comprises 140g/L of copper sulfate, 40-50g/L of sulfuric acid and Cl-60-70ppm, 0.05-0.0.07 g/L of diazeniumphenyl black, 0.02-0.04g/L of polyethylene glycol, 0.01-0.04g/L of sodium polydithio-dipropyl sulfonate, and the temperature of the electrolyte of the electrolytic copper plating is 25-30oC, current density 1-2A/dm2The thickness is 14-24 μm.
Copper sulfate and sulfuric acid are main components of sulfate plating solution, and both of them participate in the electrode process and have interdependence relationship in the plating solution. The concentration of copper sulfate is too low, and the coating in the high current area is easy to be burnt; the copper sulfate concentration is too high, and the dispersing ability and leveling ability of the plating solution are lowered. The sulfuric acid is used for improving the conductivity of the solution, preventing the copper salt from hydrolyzing and enabling the plating layer to be fine in crystallization. The sulfuric acid concentration is too low, the conductivity of the solution is poor, and the dispersion capability of the plating solution is poor; too high a concentration of sulfuric acid lowers the mobility of Cu2+, the plating efficiency is lowered, the ductility of the copper plated layer is lowered, and the brightness of the plated layer is lowered. The chloride ion is an anode activator and a stress relieving agent of the plating layer, can help the anode to dissolve, and can be used for brightening and leveling the plating layer under the synergistic action of the chloride ion and the additive, and can also reduce the tensile stress of the plating layer. Proper amount of Cl-can improve the brightness and leveling property of the coating and reduce the stress of the coating. In addition, an improvement additive needs to be added into the plating solution, wherein sodium polydithio-dipropyl sulfonate is used as a brightening agent, polyethylene glycol is used as an auxiliary brightening agent, diazobenzene black is used as a leveling agent, and the diazobenzene black and positively charged copper ions compete with each other, so that the copper ions are not easy to deposit at a high current density region, but the copper deposition in a low current density region is not influenced, and the originally fluctuant and uneven surface is flatter, so that the leveling effect on the plating layer is achieved, and the effect of copper electroplating is shown in the right diagram of figure 4 and figure 7.
The beneficial technical effects are as follows:
through the treatment, the bonding force of the aluminum material and the copper layer can be obviously improved, the corrosion resistance of a plating layer is effectively improved, the surface is bright, uniform and continuous, and the phenomena of peeling, falling and local roughness are avoided, and the prepared aluminum alloy plating piece has good bonding and corrosion resistance, is beneficial to being applied to large-scale industrial production, and has obvious economic and social benefits.
Drawings
FIG. 1 is a schematic view of anodization.
FIG. 2 is an SEM image of the surface of an aluminum material from which an anodic oxide film has been removed according to the present invention.
FIG. 3 is an AFM image of the aluminum material surface after removal of the anodic oxide film according to the present invention.
FIG. 4 is a SEM image of the surface of the aluminum material (left) and the electroplated copper (right) of the present invention.
FIG. 5 is a friction coefficient test chart of a plated part according to the present invention.
FIG. 6 is a SEM image of a cross section of a plated part after electroless nickel plating according to the present invention.
FIG. 7 is a SEM image of a cross section of an electroplated copper plated part according to the present invention.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
A preparation method of an aluminum alloy metal plated part comprises the following preparation methods:
(1) mechanical polishing, alkaline degreasing, heat treatment and electrochemical polishing. The polishing paste used for the mechanical polishing is white polishing paste polished to a mirror surface, and the surface roughness Ra is 0.1-0.3 mu m.
The alkaline oil removal is 7g/L trisodium phosphate and 20g/L sodium carbonate aqueous solution at the temperature of 75oC。
The heat treatment temperature is 420 DEGoAnd C, the time is 5 hours, and the atmosphere is nitrogen.
The electrochemical polishing is carried out by mixing perchloric acid and ethanol at a volume ratio of 1:10 and at a current density of 700mA/cm2And the time is 3 min.
(2) And (6) anodizing.
The anode is oxidized into 0.4M sulfuric acid solution, and the volume ratio of the solvent is 2: 3 deionized water and ethylene glycol, the voltage of anodic oxidation is 20V, and the time is 30 min.
(3) And removing the anodic oxide film.
6wt.% H for removing anodic oxide film3PO4With 1.8wt.% of H2CrO4The mixed solution of (2) is at 60oAnd C, removing, washing with deionized water to be neutral, and drying in vacuum.
(4) And (4) adsorbing nickel and copper ions.
The copper ion adsorption solution comprises 10g/L copper sulfate, 2g/L nickel sulfate, 5g/L citric acid complexing agent, 1g/L phytic acid stabilizer and deionized water, and the soaking time is 1 min.
(5) Chemical plating nickel-phosphorus alloy.
The solution of the chemical nickel-phosphorus plating alloy is 10g/L of nickel sulfate main salt, 10g/L of sodium hypophosphite reducing agent, 5-g/L of hydroxyacetic acid complexing agent, 0.1g/L of mercaptobenzothiazole stabilizer and 1g/L of lanthanum chloride additive, ammonia water is used for adjusting the pH value to be 5.2 +/-0.2, and the temperature is 50 DEGoC。
(6) Copper electroplating:the electrolytic solution for the electrolytic copper plating comprises 140g/L of copper sulfate, 40g/L of sulfuric acid and Cl-60ppm, 0.05g/L of diazeniumblack, 0.02g/L of polyethylene glycol, 0.01g/L of sodium polydithio-dipropyl sulfonate and 25 percent of electrolyte temperatureoC, Current Density 1A/dm2。
Example 2
A preparation method of an aluminum alloy metal plated part comprises the following preparation methods:
(1) mechanical polishing, alkaline degreasing, heat treatment and electrochemical polishing. The polishing paste used for the mechanical polishing is white polishing paste polished to a mirror surface, and the surface roughness Ra is 0.1-0.3 mu m.
The alkaline oil removal is 7g/L trisodium phosphate and 20g/L sodium carbonate aqueous solution at the temperature of 75oC。
The heat treatment temperature is 420 DEGoAnd C, the time is 5 hours, and the atmosphere is nitrogen.
The electrochemical polishing is carried out by mixing perchloric acid and ethanol at a volume ratio of 1:10 and at a current density of 700mA/cm2And the time is 3 min.
(2) And (6) anodizing.
Anodizing to 0.425M sulfuric acid solution, solvent by volume ratio of 2: 3.5 deionized water and ethylene glycol, the voltage of anodic oxidation is 20V, and the time is 35 min.
(3) And removing the anodic oxide film.
6wt.% H for removing anodic oxide film3PO4With 1.8wt.% of H2CrO4The mixed solution of (2) is at 60oAnd C, removing, washing with deionized water to be neutral, and drying in vacuum.
(4) And (4) adsorbing nickel and copper ions.
The copper ion adsorption solution comprises 12.5g/L copper sulfate, 2.5g/L nickel sulfate, 5.5g/L citric acid complexing agent, 1.5g/L phytic acid stabilizer and deionized water, and the soaking time is 1.5 min.
(5) Chemical plating nickel-phosphorus alloy.
The solution of the chemical nickel-phosphorus plating alloy comprises 15g/L of nickel sulfate main salt, 12.5g/L of sodium hypophosphite reducing agent, 6g/L of hydroxyacetic acid complexing agent, 0.3g/L of mercaptobenzothiazole stabilizer and chlorinationLanthanum additive 1.5g/L, adjusted pH =5.2 ± 0.2 with ammonia, temperature 55oC。
(6) Copper electroplating: the electrolytic solution for electroplating copper comprises 160g/L of copper sulfate, 45g/L of sulfuric acid, and Cl-65ppm, 0.06g/L of diazeniumblack, 0.03g/L of polyethylene glycol, 0.025g/L of sodium polydithio-dipropyl sulfonate and the temperature of electrolyte is 28oC, current density 1.5A/dm2。
Example 3
A preparation method of an aluminum alloy metal plated part comprises the following preparation methods:
(1) mechanical polishing, alkaline degreasing, heat treatment and electrochemical polishing. The polishing paste used for the mechanical polishing is white polishing paste polished to a mirror surface, and the surface roughness Ra is 0.1-0.3 mu m.
The alkaline oil removal is 7g/L trisodium phosphate and 20g/L sodium carbonate aqueous solution at the temperature of 75oC。
The heat treatment temperature is 420 DEGoAnd C, the time is 5 hours, and the atmosphere is nitrogen.
The electrochemical polishing is carried out by mixing perchloric acid and ethanol at a volume ratio of 1:10 and at a current density of 700mA/cm2And the time is 3 min.
(2) And (6) anodizing.
Anodizing to 0.45M sulfuric acid solution, wherein the volume ratio of a solvent is 2: 4 deionized water and ethylene glycol, the voltage of anodic oxidation is 20V, and the time is 40 min.
(3) And removing the anodic oxide film.
6wt.% H for removing anodic oxide film3PO4With 1.8wt.% of H2CrO4The mixed solution of (2) is at 60oAnd C, removing, washing with deionized water to be neutral, and drying in vacuum.
(4) And (4) adsorbing nickel and copper ions.
The copper ion adsorption solution comprises 15g/L copper sulfate, 3g/L nickel sulfate, 6g/L citric acid complexing agent, 2g/L phytic acid stabilizer and deionized water, and the soaking time is 2 min.
(5) Chemical plating nickel-phosphorus alloy.
The solution of the chemical nickel-phosphorus plating alloy is20g/L of nickel sulfate main salt, 15g/L of sodium hypophosphite reducing agent, 7g/L of glycolic acid complexing agent, 0.5g/L of mercaptobenzothiazole stabilizer and 2g/L of lanthanum chloride additive, wherein the pH value is adjusted to be 5.2 +/-0.2 by using ammonia water, and the temperature is 60%oC。
(6) Copper electroplating: the electrolytic solution for electroplating copper comprises 170g/L of copper sulfate, 50g/L of sulfuric acid, and Cl-70ppm, 0.0.07g/L of dinitrobenzene black, 0.04g/L of polyethylene glycol, 0.04g/L of sodium polydithio-dipropyl sulfonate and 30-percent electrolyte temperatureoC, Current Density 2A/dm2。
Comparative example 1
A preparation method of an aluminum alloy metal plated part comprises the following preparation methods:
(1) mechanical polishing, alkaline degreasing, heat treatment and electrochemical polishing. The polishing paste used for the mechanical polishing is white polishing paste polished to a mirror surface, and the surface roughness Ra is 0.1-0.3 mu m.
The alkaline oil removal is 7g/L trisodium phosphate and 20g/L sodium carbonate aqueous solution at the temperature of 75oC。
The heat treatment temperature is 420 DEGoAnd C, the time is 5 hours, and the atmosphere is nitrogen.
The electrochemical polishing is carried out by mixing perchloric acid and ethanol at a volume ratio of 1:10 and at a current density of 700mA/cm2And the time is 3 min.
(2) Chemical plating nickel-phosphorus alloy.
The solution of the chemical nickel-phosphorus plating alloy is 15g/L of nickel sulfate main salt, 12.5g/L of sodium hypophosphite reducing agent, 6g/L of hydroxyacetic acid complexing agent, 0.3g/L of mercaptobenzothiazole stabilizer and 1.5g/L of lanthanum chloride additive, ammonia water is used for adjusting the pH value to be 5.2 +/-0.2, and the temperature is 55 DEGoC。
(3) Copper electroplating: the electrolytic solution for electroplating copper comprises 160g/L of copper sulfate, 45g/L of sulfuric acid, and Cl-65ppm, 0.06g/L of diazeniumblack, 0.03g/L of polyethylene glycol, 0.025g/L of sodium polydithio-dipropyl sulfonate and the temperature of electrolyte is 28oC, current density 1.5A/dm2。
Comparative example 2
A preparation method of an aluminum alloy metal plated part comprises the following preparation methods:
(1) mechanical polishing, alkaline degreasing, heat treatment and electrochemical polishing. The polishing paste used for the mechanical polishing is white polishing paste polished to a mirror surface, and the surface roughness Ra is 0.1-0.3 mu m.
The alkaline oil removal is 7g/L trisodium phosphate and 20g/L sodium carbonate aqueous solution at the temperature of 75oC。
The heat treatment temperature is 420 DEGoAnd C, the time is 5 hours, and the atmosphere is nitrogen.
The electrochemical polishing is carried out by mixing perchloric acid and ethanol at a volume ratio of 1:10 and at a current density of 700mA/cm2And the time is 3 min.
(2) And (4) adsorbing nickel and copper ions.
The copper ion adsorption solution comprises 12.5g/L copper sulfate, 2.5g/L nickel sulfate, 5.5g/L citric acid complexing agent, 1.5g/L phytic acid stabilizer and deionized water, and the soaking time is 1.5 min.
(3) Chemical plating nickel-phosphorus alloy.
The solution of the chemical nickel-phosphorus plating alloy is 15g/L of nickel sulfate main salt, 12.5g/L of sodium hypophosphite reducing agent, 6g/L of hydroxyacetic acid complexing agent, 0.3g/L of mercaptobenzothiazole stabilizer and 1.5g/L of lanthanum chloride additive, ammonia water is used for adjusting the pH value to be 5.2 +/-0.2, and the temperature is 55 DEGoC。
(4) Copper electroplating: the electrolytic solution for electroplating copper comprises 160g/L of copper sulfate, 45g/L of sulfuric acid, and Cl-65ppm, 0.06g/L of diazeniumblack, 0.03g/L of polyethylene glycol, 0.025g/L of sodium polydithio-dipropyl sulfonate and the temperature of electrolyte is 28oC, current density 1.5A/dm2。
Comparative example 3
A preparation method of an aluminum alloy metal plated part comprises the following preparation methods:
(1) mechanical polishing, alkaline degreasing, heat treatment and electrochemical polishing. The polishing paste used for the mechanical polishing is white polishing paste polished to a mirror surface, and the surface roughness Ra is 0.1-0.3 mu m.
The alkaline oil removal is 7g/L trisodium phosphate and 20g/L sodium carbonate aqueous solution at the temperature of 75oC。
The heat treatmentAt a temperature of 420 deg.CoAnd C, the time is 5 hours, and the atmosphere is nitrogen.
The electrochemical polishing is carried out by mixing perchloric acid and ethanol at a volume ratio of 1:10 and at a current density of 700mA/cm2And the time is 3 min.
(2) And (6) anodizing.
Anodizing to 0.425M sulfuric acid solution, solvent by volume ratio of 2: 3.5 deionized water and ethylene glycol, the voltage of anodic oxidation is 20V, and the time is 35 min.
(3) And removing the anodic oxide film.
6wt.% H for removing anodic oxide film3PO4With 1.8wt.% of H2CrO4The mixed solution of (2) is at 60oAnd C, removing, washing with deionized water to be neutral, and drying in vacuum.
(4) And (4) adsorbing nickel and copper ions.
The copper ion adsorption solution comprises 12.5g/L copper sulfate, 5.5g/L citric acid complexing agent, 1.5g/L phytic acid stabilizer and deionized water, and the soaking time is 1.5 min.
(5) Chemical plating nickel-phosphorus alloy.
The solution of the chemical nickel-phosphorus plating alloy is 15g/L of nickel sulfate main salt, 12.5g/L of sodium hypophosphite reducing agent, 6g/L of hydroxyacetic acid complexing agent, 0.3g/L of mercaptobenzothiazole stabilizer and 1.5g/L of lanthanum chloride additive, ammonia water is used for adjusting the pH value to be 5.2 +/-0.2, and the temperature is 55 DEGoC。
(6) Copper electroplating: the electrolytic solution for electroplating copper comprises 160g/L of copper sulfate, 45g/L of sulfuric acid, and Cl-65ppm, 0.06g/L of diazeniumblack, 0.03g/L of polyethylene glycol, 0.025g/L of sodium polydithio-dipropyl sulfonate and the temperature of electrolyte is 28oC, current density 1.5A/dm2。
Figure 243145DEST_PATH_IMAGE002
Generally, the corrosion potential of the aluminum matrix is-1.636V, and the invention effectively promotes the chemical nickel plating process and electroplates copper by adsorbing copper and nickel ions in the pore passages left after anodic oxidation to form nickel catalytic particlesThen, the corrosion potential was-0.213V and the corrosion current syphilis was 0.321 x 10-4Compared with comparative example 1 for directly electroplating copper on the surface of the aluminum material, the corrosion potential is-0.769V, and the corrosion current density is 2.72 x 10-4As known to those skilled in the art, for the plated metal, the smaller the corrosion current is, the larger the corrosion potential is, the better the corrosion resistance of the plated part is, the subsequent comparative example 2 does not perform anodic oxidation to obtain a pore channel treatment, thereby reducing the progress of formation of nickel catalytic particles, and in comparative example 3, nickel particles are not catalyzed during adsorption, only a small amount of copper is used to catalyze nickel ions in the chemical nickel plating solution in an extremely excessive amount, so the effect is poor.
And (3) testing the friction coefficient of the plated part: the friction coefficient is shown in figure 5, and after copper electroplating, the friction coefficient of the plating layer is between 0.5 and 0.6.
Testing the coating binding force of the coated part
(1) Thermal shock test
According to GB/T5270-2005, the temperature of the thermal shock test is set at 250 ℃, and the sample is put into distilled water for quenching after being kept in a drying oven for 30 min. And observing whether the coating is bubbled, peeled and fallen after two thermal shocks.
(2) Cross cut test
Referring to GB/T5270-2005 and GB/T9286-1998, 100 grids with the side length of 1mm are scribed on the surface of a sample by a hundred-grid knife, then an adhesive tape meeting the requirements of the two standards is tightly attached to the surface, the adhesive tape is forcibly torn off in the vertical direction, and the number of grids stripped from the coating is used as the standard for judging the binding force of the coating.
The bonding force test was performed for example 2 and comparative examples 1 to 3.
The embodiment 2 has no bubbling, peeling and falling in a thermal shock test, the bubbling, peeling and falling phenomena occur in the comparative example 1 after one thermal shock, the comparative example 3 has the peeling phenomenon compared with the comparative example 2, and in comparison, the pore channels left after the anodic oxidation treatment are beneficial to improving the combination of the coating and the base material. The number of the peeled cells of example 2 and comparative examples 1 to 3 was 0, 92, 12 and 8 by the cross cut test, respectively, and the high bonding force of the plated article of the present invention was further verified.
Although the present invention has been described above by way of examples of preferred embodiments, the present invention is not limited to the specific embodiments, and can be modified as appropriate within the scope of the present invention.

Claims (10)

1. The preparation method of the aluminum alloy metal plated part is characterized by comprising the following steps:
(1) mechanical polishing, alkaline degreasing, heat treatment and electrochemical polishing;
(2) anodizing;
(3) removing the anodic oxide film;
(4) adsorption of nickel and copper ions
(5) Chemical nickel-phosphorus plating alloy
(6) And (4) electroplating copper.
2. The method of claim 1, wherein the mechanical polishing step uses a white polishing paste with a surface roughness Ra of 0.1-0.3 μm, and the alkaline degreasing step comprises a 7g/L trisodium phosphate solution and a 20g/L aqueous sodium carbonate solution at a temperature of 75 deg.CoC。
3. The method of claim 1, wherein the heat treatment temperature is 420 ℃oC, the time is 5h, the electrochemical polishing uses nitrogen atmosphere, the volume ratio of the electrochemical polishing used is perchloric acid and ethanol mixed solution, the current density is 700mA/cm2And the time is 3 min.
4. The method of claim 1, wherein the anodic oxidation solution is a 0.4-0.45M sulfuric acid solution, and the solvent is a solvent in a volume ratio of 2: (3-4) deionized water and ethylene glycol, wherein the voltage of anodic oxidation is 20V, and the time is 30-40 min.
5. The method of claim 1, wherein 6wt.% of H is used for removing the anodic oxide film3PO4With 1.8wt.% of H2CrO4The mixed solution of (2) is at 60oAnd C, removing, washing with deionized water between the step (3) and the step (4) to be neutral, and drying in vacuum.
6. The method of claim 1, wherein the copper ion adsorption solution comprises 10-15g/L copper sulfate, 2-3g/L nickel sulfate, 5-6g/L citric acid complexing agent, 1-2g/L phytic acid stabilizer and deionized water, and the soaking time is 1-2 min.
7. The method of claim 1, wherein the solution of the electroless nickel-phosphorus alloy plating is 10-20g/L of nickel sulfate main salt, 10-15g/L of sodium hypophosphite reducing agent, 5-7g/L of glycolic acid complexing agent, 0.1-0.5g/L of mercaptobenzothiazole stabilizer, 1-2g/L of lanthanum chloride additive, and ammonia is used for adjusting pH =5.2 +/-0.2 and temperature is 50-60oC。
8. A method for producing an aluminum alloy metal plated article according to claim 7, wherein the electroless nickel-phosphorus plating is carried out for 10 to 20min and the thickness is 7 to 12 μm.
9. The method as claimed in claim 1, wherein the electrolyte solution for electroplating copper comprises 170g/L of copper sulfate 140--60-70ppm, 0.05-0.07g/L of diazeniumblack, 0.02-0.04g/L of polyethylene glycol and 0.01-0.04g/L of sodium polydithio dipropyl sulfonate.
10. The method of claim 9, wherein the electrolytic solution temperature of the electrolytic copper plating is 25 to 30 degrees centigradeoC, current density 1-2A/dm2The thickness is 14-24 μm.
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