CN112626573A - Method for directly electroplating copper on surface of magnesium alloy - Google Patents
Method for directly electroplating copper on surface of magnesium alloy Download PDFInfo
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- CN112626573A CN112626573A CN202011495728.8A CN202011495728A CN112626573A CN 112626573 A CN112626573 A CN 112626573A CN 202011495728 A CN202011495728 A CN 202011495728A CN 112626573 A CN112626573 A CN 112626573A
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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
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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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
- 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
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
Abstract
The method for directly electroplating the copper on the surface of the magnesium alloy cancels zinc dipping or chemical nickel plating pretreatment, optimizes the process steps, directly electroplates by using the copper pyrophosphate solution added with a special additive, has short process flow, stable process, no cyanide and simple sewage treatment, ensures uniform and delicate coating, also meets the aim of good bonding force with a magnesium alloy substrate when being applied to the magnesium alloy part of a product, achieves the aim of subsequent plating and effective protection of the magnesium alloy part, is easy to implement, reduces the production cost, ensures the product quality and improves the reliability.
Description
Technical Field
The invention belongs to the technical field of metal surface treatment, and particularly relates to a method for directly electroplating copper on a magnesium alloy surface.
Background
The magnesium alloy is an alloy formed by adding other elements into magnesium as a base. The main alloy elements comprise aluminum, zinc, manganese, cerium, thorium, lithium, a small amount of zirconium or cadmium and the like. The most widely used at present are magnesium-aluminum alloy, magnesium-manganese alloy and magnesium-zinc-zirconium alloy, and novel magnesium-lithium alloy; the magnesium alloy has the advantages of small density, high specific strength and specific stiffness, good thermal conductivity, damping vibration attenuation, electromagnetic shielding, easy processing and forming, easy recovery and the like, has larger impact load bearing capacity than aluminum alloy, better organic matter and alkali corrosion resistance, has extremely important application value and wide application prospect in the fields of automobiles, electronic communication, aerospace, national defense and military and the like, is known as a '21 st century green engineering material', but has an electrode potential of-2.37V, a stable potential of-1.45V in a 5% NaCl solution and a stable potential of-1.5V to-1.6V in seawater, and is the most negative of industrial alloys. In addition, the magnesium oxide film is loose and porous (the mass ratio of MgO/Mg is 0.81), so that the magnesium alloy has extremely high chemical and electrochemical activity and poor corrosion resistance, and besides the high corrosion resistance in kerosene, gasoline, mineral oil and strong alkali, the magnesium and the magnesium alloy can be corroded at normal temperature in the atmospheric environment; in dry air, magnesium oxide is generated on the surface of magnesium; in a humid environment, magnesium oxide on the surface of magnesium is converted into magnesium hydroxide; carbon dioxide in the atmosphere and water form carbonic acid, and the carbonic acid reacts with magnesium hydroxide on the surface to generate magnesium carbonate; in addition, magnesium hydroxide on the surface of the magnesium alloy can react with pollutants in the atmosphere, such as sulfur dioxide, and the substances form a surface film outside the magnesium alloy, but the surface film cannot protect the magnesium alloy; therefore, the protective performance of the magnesium alloy is generally improved by adopting methods such as electroplating, chemical oxidation, anodization, micro-arc oxidation, organic coating and the like.
In the aspect of electroplating, because the electrode potential of the magnesium alloy is very low and the chemical property is extremely active, the magnesium alloy is difficult to be directly electroplated, and special pretreatment measures before plating are required to ensure that the plating layer and a substrate have good bonding force. At present, the most applied electroplating methods at home and abroad have two types: 1) the zinc dipping method comprises the following general process flows: cleaning, etching, activating, zinc dipping, pre-plating copper cyanide and electroplating; 2) the chemical nickel plating method comprises the following general process flows: cleaning, etching, fluoride activating, chemical nickel plating and electroplating; the disadvantages of both methods are: the method has the advantages of multiple processes, long process flow, multiple process control points and difficult mastering; secondly, different grades of magnesium alloy are subjected to different zinc dipping processes, the quality of a zinc dipping layer is difficult to control, repeated tests are needed during electroplating, and the process is unstable; the preplating copper cyanide solution has high toxicity, and sewage needs special treatment, so that the problem of environmental protection exists; fourthly, the chemical nickel plating has high cost, the chemical nickel plating layer is not easy to remove, and the repair is difficult, so the improvement is needed.
Disclosure of Invention
The technical problems solved by the invention are as follows: the method for directly electroplating copper on the surface of the magnesium alloy cancels zinc dipping or chemical nickel plating pretreatment, shortens the working procedures, optimizes the process steps, directly electroplates by using the copper pyrophosphate solution added with special additives, has short process flow, stable process, no cyanide and simple sewage treatment, is applied to the magnesium alloy part of a product, ensures that the plating layer is uniform, fine and free of defects, also meets the aim of good bonding force with the magnesium alloy substrate, and achieves the aim of subsequent plating and effective protection of the magnesium alloy part.
The technical scheme adopted by the invention is as follows: the method for directly electroplating copper on the surface of the magnesium alloy comprises the following steps:
1) immersing the hung parts into absolute ethyl alcohol at normal temperature to carry out ultrasonic oil removal;
2) the chemical degreasing fluid is prepared by adding pure water into the following components according to the formula: 8-12 g/L of trisodium phosphate and 40-50 g/L of sodium hydroxide, and immersing the parts subjected to ultrasonic oil removal into chemical degreasing liquid for surface chemical degreasing treatment;
3) the etching solution is prepared by adding pure water into the following components according to the formula: 100-120 g/L of chromic anhydride and 90-110 ml/L of nitric acid, and placing the part subjected to chemical degreasing treatment into etching solution for treatment;
4) the activating solution is prepared by adding pure water into the following components according to the formula: 210-230 ml/L of hydrofluoric acid, and immersing the etched part into an activating solution for treatment;
5) the copper pyrophosphate electroplating solution is prepared by adding pure water according to the following formula: 20-30 g/L of copper pyrophosphate, 390-460 g/L of potassium pyrophosphate, 20-25 g/L of ammonium citrate, 5-50 g/L of special additive, and 8.5-9.0 of the pH value of copper pyrophosphate electroplating solution, and adding the activated parts into the copper pyrophosphate electroplating solution for direct electroplating;
6) and drying the parts taken out of the copper pyrophosphate electroplating solution for 30min at the temperature of 80-100 ℃ after drying the parts by compressed air.
In the step 1), the part is immersed in absolute ethyl alcohol at normal temperature for ultrasonic oil removal for 8-12 min.
In the step 2), the part is immersed in the chemical degreasing liquid at the temperature of 60-70 ℃ for 10-15 min.
In the step 3), the part is placed in the etching solution at the temperature of 15-30 ℃ for 30-50 s.
In the step 4), the part is immersed in the activating solution at a temperature of 15-30 ℃ for 10-15 min.
In the step 5), the special additive is inorganic salt or organic compound containing fluorine ions.
Further, the inorganic salt or organic compound of the fluoride ion is ammonium bifluoride, potassium fluoride, sodium fluoride, ammonium fluoride or ammonium bifluoride.
In the step 5), the part after the activation treatment is added into the copper pyrophosphate electroplating solution at the temperature of 25-40 ℃ for electroplating for 20-120 min.
Compared with the prior art, the invention has the advantages that:
1. the technical scheme optimizes the process steps, adopts the pyrophosphate copper solution added with special additives for direct electroplating, cancels the pretreatment of zinc immersion or chemical nickel plating, firstly cleans magnesium alloy parts for oil removal, then etches, activates and directly electroplates copper, and has short process flow, stable process, no cyanide and simple sewage treatment;
2. the technical scheme is applied to the magnesium alloy part of a product, not only ensures that the plating layer is uniform, fine and free of defects, but also meets the purpose of good bonding force with the magnesium alloy substrate, and achieves the purposes of subsequent plating and effective protection of the magnesium alloy part;
3. the technical scheme cancels the zinc dipping or chemical nickel plating pretreatment, has less working procedures, short process flow and stable process, improves the production efficiency and solves the problem of unstable quality caused by the zinc dipping or chemical nickel plating pretreatment;
4. the technical scheme can meet the requirement of electro-coppering of magnesium alloy parts in any shapes, solves the problem of unstable quality caused by zinc dipping or chemical nickel plating pretreatment, and improves the electro-coppering quality of the magnesium alloy parts, thereby improving the reliability of products;
5. the technical scheme does not contain cyanide, does not need to specially treat the sewage, has simple sewage treatment and reduces the sewage treatment cost.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the present invention is further described in detail with reference to the following embodiments, and the specific embodiments described herein are only used for explaining the present invention, and are only a part of the embodiments of the present invention, not all of the embodiments.
Example 1:
the method for directly electroplating copper on the surface of the magnesium alloy comprises the following steps:
1) immersing the hung magnesium alloy part into absolute ethyl alcohol at normal temperature to carry out ultrasonic oil removal; the magnesium alloy part is immersed into absolute ethyl alcohol at normal temperature for ultrasonic oil removal for 8 min;
2) the chemical degreasing fluid is prepared by adding pure water into the following components according to the formula: 8g/L of trisodium phosphate and 40g/L of sodium hydroxide, and immersing the magnesium alloy part subjected to ultrasonic degreasing into chemical degreasing liquid for surface chemical degreasing treatment; immersing the magnesium alloy part into chemical degreasing liquid at the temperature of 60 ℃ for 10 min;
3) the etching solution is prepared by adding pure water into the following components according to the formula: 100g/L of chromic anhydride and 90ml/L of nitric acid, and placing the magnesium alloy part subjected to chemical degreasing treatment into etching solution for treatment; the magnesium alloy part is put into the etching solution at the temperature of 18 ℃ for 35s, so that oxides formed on the surface of the magnesium alloy part in the air are effectively removed, and the binding force between a plating layer and a substrate is ensured;
4) the activating solution is prepared by adding pure water into the following components according to the formula: 215ml/L of hydrofluoric acid (HF, 70 percent), and immersing the magnesium alloy part subjected to etching treatment into activating solution for treatment; the magnesium alloy part is immersed in the activating solution for 12min at the temperature of 18 ℃, so that the active surface of the magnesium alloy part is effectively maintained, and the binding force between the coating and the substrate is further improved;
5) the copper pyrophosphate electroplating solution is prepared by adding pure water according to the following formula: 22g/L of copper pyrophosphate, 400g/L of potassium pyrophosphate, 21g/L of ammonium citrate and 15g/L of special additive, wherein the special additive is ammonium bifluoride, the pH value of the copper pyrophosphate electroplating solution is 8.5-9.0, and the magnesium alloy part subjected to activation treatment is added into the copper pyrophosphate electroplating solution for direct electroplating; selecting electroplating time according to the thickness of a coating of the magnesium alloy part and the requirement of the coating thickness, and adding the magnesium alloy part subjected to activation treatment into a copper pyrophosphate electroplating solution at the temperature of 25-40 ℃ for 35min when the thickness of the electroplating layer is 5-9 mu m; the special additive is inorganic salt or organic compound containing fluorine ions; specifically, the special additive can also be selected from potassium fluoride, sodium fluoride, ammonium fluoride or ammonium bifluoride and the like; copper is added in the form of copper pyrophosphate, so that a protective film layer can be formed on the surface of the magnesium alloy substrate, the activity of the magnesium alloy substrate in a solution is reduced, the continuous corrosion of the magnesium alloy substrate in the electroplating process can be effectively prevented, and a uniform, fine, defect-free and good-binding-force coating is obtained;
6) and drying the magnesium alloy part taken out of the copper pyrophosphate electroplating solution for 30min at the temperature of 80-100 ℃ after drying by compressed air.
Example 2:
the method for directly electroplating copper on the surface of the magnesium alloy comprises the following steps:
1) immersing the hung magnesium alloy part into absolute ethyl alcohol at normal temperature to carry out ultrasonic oil removal; the time for ultrasonic degreasing of the magnesium alloy part by immersing the magnesium alloy part into absolute ethyl alcohol at normal temperature is 10 min.
2) The chemical degreasing fluid is prepared by adding pure water into the following components according to the formula: 10g/L of trisodium phosphate and 45g/L of sodium hydroxide, and immersing the magnesium alloy part subjected to ultrasonic degreasing into chemical degreasing liquid for surface chemical degreasing treatment; the magnesium alloy parts are immersed in the chemical degreasing liquid at the temperature of 65 ℃ for 12 min.
3) The etching solution is prepared by adding pure water into the following components according to the formula: chromic anhydride of 110g/L and nitric acid of 100ml/L, and the magnesium alloy part after chemical degreasing treatment is put into etching solution for treatment; the magnesium alloy part is put into the etching solution at the temperature of 20 ℃ for 40s, so that oxides formed on the surface of the magnesium alloy part in the air are effectively removed, and the binding force of a plating layer and a substrate is ensured;
4) the activating solution is prepared by adding pure water into the following components according to the formula: immersing the etched magnesium alloy part into activating liquid for treatment, wherein the hydrofluoric acid is 220 ml/L; the magnesium alloy part is immersed in the activating solution for 13min at the temperature of 20 ℃, so that the active surface of the magnesium alloy part is effectively maintained, and the binding force between the coating and the substrate is further improved;
5) the copper pyrophosphate electroplating solution is prepared by adding pure water according to the following formula: 25g/L of copper pyrophosphate, 420g/L of potassium pyrophosphate, 22-23g/L of ammonium citrate and 24g/L of special additive, wherein the special additive is potassium fluoride, the PH value of the copper pyrophosphate electroplating solution is 8.5-9.0, and the magnesium alloy part subjected to activation treatment is added into the copper pyrophosphate electroplating solution for direct electroplating; selecting electroplating time according to the requirement of the thickness of the plating layer, and adding the activated magnesium alloy part into a copper pyrophosphate electroplating solution at the temperature of 25-40 ℃ for 50min when the thickness of the electroplating layer is 7-13 mu m; the special additive is inorganic salt or organic compound containing fluorine ions; specifically, the special additive can also be selected from ammonium bifluoride, sodium fluoride, ammonium fluoride or ammonium bifluoride and the like; copper is added in the form of copper pyrophosphate, so that a protective film layer can be formed on the surface of the magnesium alloy substrate, the activity of the magnesium alloy substrate in a solution is reduced, the continuous corrosion of the magnesium alloy substrate in the electroplating process can be effectively prevented, and a uniform, fine, defect-free and good-binding-force coating is obtained;
6) and drying the magnesium alloy part taken out of the copper pyrophosphate electroplating solution for 30min at the temperature of 80-100 ℃ after drying by compressed air.
Example 3:
the method for directly electroplating copper on the surface of the magnesium alloy comprises the following steps:
1) immersing the hung magnesium alloy part into absolute ethyl alcohol at normal temperature to carry out ultrasonic oil removal; the magnesium alloy part is immersed into absolute ethyl alcohol at normal temperature for ultrasonic oil removal for 8-12 min.
2) The chemical degreasing fluid is prepared by adding pure water into the following components according to the formula: 8-12 g/L of trisodium phosphate and 40-50 g/L of sodium hydroxide, and immersing the magnesium alloy part subjected to ultrasonic degreasing into chemical degreasing liquid for surface chemical degreasing treatment; and immersing the magnesium alloy part into the chemical degreasing liquid at the temperature of 60-70 ℃ for 10-15 min.
3) The etching solution is prepared by adding pure water into the following components according to the formula: 100-120 g/L of chromic anhydride and 90-110 ml/L of nitric acid, and placing the magnesium alloy part subjected to chemical degreasing treatment into etching solution for treatment; the magnesium alloy part is put into the etching solution at the temperature of 25 ℃ for 45s, so that oxides formed on the surface of the magnesium alloy part in the air are effectively removed, and the binding force of a plating layer and a substrate is ensured;
4) the activating solution is prepared by adding pure water into the following components according to the formula: 210-230 ml/L of hydrofluoric acid, and immersing the etched magnesium alloy part into an activating solution for treatment; immersing the magnesium alloy part into the activating solution at the temperature of 15-30 ℃ for 10-15 min, so that the active surface of the magnesium alloy part is effectively maintained, and the binding force between the coating and the substrate is further improved;
5) the copper pyrophosphate electroplating solution is prepared by adding pure water according to the following formula: 28g/L of copper pyrophosphate, 450g/L of potassium pyrophosphate, 24g/L of ammonium citrate and 40g/L of special additive, wherein the special additive is ammonium bifluoride, the pH value of the copper pyrophosphate electroplating solution is 8.5-9.0, and the magnesium alloy part subjected to activation treatment is added into the copper pyrophosphate electroplating solution for direct electroplating; selecting electroplating time according to the requirement of the thickness of the plating layer, and when the thickness of the electroplating layer is 11-20 microns, adding the activated magnesium alloy part into a copper pyrophosphate electroplating solution at the temperature of 25-40 ℃ for 80min, wherein the time is selected according to the requirement of the thickness of the plating layer; the special additive is inorganic salt or organic compound containing fluorine ions; specifically, the special additive can also be selected from ammonium bifluoride, potassium fluoride, sodium fluoride or ammonium fluoride and the like; copper is added in the form of copper pyrophosphate, so that a protective film layer can be formed on the surface of the magnesium alloy substrate, the activity of the magnesium alloy substrate in a solution is reduced, the continuous corrosion of the magnesium alloy substrate in the electroplating process can be effectively prevented, and a uniform, fine, defect-free and good-binding-force coating is obtained;
6) and drying the magnesium alloy part taken out of the copper pyrophosphate electroplating solution for 30min at the temperature of 80-100 ℃ after drying by compressed air.
The electroplated pyrophosphate copper layer obtained by the technical scheme is subjected to appearance and bonding force inspection according to HB5037 copper plating quality inspection standard: 1) appearance: the color is rose red, and the plating layer is uniform, fine and flawless in crystallization; 2) the binding force is as follows: the plating layer has no bubbles, no peeling and no falling off, and has good bonding force with the magnesium alloy matrix; the test method adopts a thermal shock test method according to GB 5270: the sample was heated at 200. + -. 10 ℃ for 1 hour and then rapidly immersed in cold water to be rapidly cooled.
The technical scheme optimizes the process steps, directly electroplates by using the copper pyrophosphate solution added with a special additive, cancels the pretreatment of zinc dipping or chemical nickel plating, shortens the working procedures, firstly cleans the magnesium alloy parts to remove oil, then etches, activates fluoride, and electroplates the copper pyrophosphate, has short process flow, stable process, no cyanide and simple sewage treatment, is applied to the magnesium alloy parts of the products, not only ensures the uniform and fine plating coat without defects, but also meets the purpose of good binding force with the magnesium alloy matrix, achieves the purpose of subsequent plating and effective protection of the magnesium alloy parts, does not contain cyanide, does not need to specially treat the sewage, has simple sewage treatment, reduces the sewage treatment cost, can meet the requirement of the copper plating of the magnesium alloy parts with any shape, solves the problem of unstable quality caused by the pretreatment of zinc dipping or chemical nickel plating, and improves the electroplating quality of the magnesium alloy parts, thereby improving the reliability of the product.
The above-mentioned embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and therefore, all equivalent changes made by the contents of the claims of the present invention should be included in the claims of the present invention.
Claims (8)
1. The method for directly electroplating copper on the surface of the magnesium alloy is characterized by comprising the following steps of:
1) immersing the hung parts into absolute ethyl alcohol at normal temperature to carry out ultrasonic oil removal;
2) the chemical degreasing fluid is prepared by adding pure water into the following components according to the formula: 8-12 g/L of trisodium phosphate and 40-50 g/L of sodium hydroxide, and immersing the parts subjected to ultrasonic oil removal into chemical degreasing liquid for surface chemical degreasing treatment;
3) the etching solution is prepared by adding pure water into the following components according to the formula: 100-120 g/L of chromic anhydride and 90-110 ml/L of nitric acid, and placing the part subjected to chemical degreasing treatment into etching solution for treatment;
4) the activating solution is prepared by adding pure water into the following components according to the formula: 210-230 ml/L of hydrofluoric acid, and immersing the etched part into an activating solution for treatment;
5) the copper pyrophosphate electroplating solution is prepared by adding pure water according to the following formula: 20-30 g/L of copper pyrophosphate, 390-460 g/L of potassium pyrophosphate, 20-25 g/L of ammonium citrate, 5-50 g/L of special additive, and 8.5-9.0 of the pH value of copper pyrophosphate electroplating solution, and adding the activated parts into the copper pyrophosphate electroplating solution for direct electroplating;
6) and drying the parts taken out of the copper pyrophosphate electroplating solution for 30min at the temperature of 80-100 ℃ after drying the parts by compressed air.
2. The method for direct copper electroplating on the surface of the magnesium alloy according to claim 1, wherein the method comprises the following steps: in the step 1), the part is immersed in absolute ethyl alcohol at normal temperature for ultrasonic oil removal for 8-12 min.
3. The method for direct copper electroplating on the surface of the magnesium alloy according to claim 1, wherein the method comprises the following steps: in the step 2), the part is immersed in the chemical degreasing liquid at the temperature of 60-70 ℃ for 10-15 min.
4. The method for direct copper electroplating on the surface of the magnesium alloy according to claim 1, wherein the method comprises the following steps: in the step 3), the part is placed in the etching solution at the temperature of 15-30 ℃ for 30-50 s.
5. The method for direct copper electroplating on the surface of the magnesium alloy according to claim 1, wherein the method comprises the following steps: in the step 4), the part is immersed in the activating solution at a temperature of 15-30 ℃ for 10-15 min.
6. The method for direct copper electroplating on the surface of the magnesium alloy according to claim 1, wherein the method comprises the following steps: in the step 5), the special additive is inorganic salt or organic compound containing fluorine ions.
7. The method for direct copper electroplating on the surface of the magnesium alloy according to claim 6, wherein the method comprises the following steps: the inorganic salt or organic compound of the fluorine ions is ammonium bifluoride, potassium fluoride, sodium fluoride, ammonium fluoride or ammonium bifluoride.
8. The method for direct copper electroplating on the surface of the magnesium alloy according to claim 1, wherein the method comprises the following steps: in the step 5), the part after the activation treatment is added into the copper pyrophosphate electroplating solution at the temperature of 25-40 ℃ for electroplating for 20-120 min.
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| CN104419952A (en) * | 2013-08-27 | 2015-03-18 | 上海航天设备制造总厂 | Method for copper electroplating, nickel chemical plating and nickel electroplating on the surface of magnesium alloy |
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| CN1598059A (en) * | 2004-08-05 | 2005-03-23 | 广州杰赛科技股份有限公司 | Magnesium alloy non cyanogen plating copper chemical plating nickle and its plating process |
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