CN112725773A - Direct chemical nickel plating method universally used for AZ91D and ZK61M magnesium alloys - Google Patents
Direct chemical nickel plating method universally used for AZ91D and ZK61M magnesium alloys Download PDFInfo
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- CN112725773A CN112725773A CN202011522779.5A CN202011522779A CN112725773A CN 112725773 A CN112725773 A CN 112725773A CN 202011522779 A CN202011522779 A CN 202011522779A CN 112725773 A CN112725773 A CN 112725773A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 81
- 238000007747 plating Methods 0.000 title claims abstract description 79
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 73
- 239000000126 substance Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000002253 acid Substances 0.000 claims abstract description 38
- 238000001035 drying Methods 0.000 claims abstract description 31
- 230000004913 activation Effects 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 20
- 238000005488 sandblasting Methods 0.000 claims abstract description 15
- 238000004140 cleaning Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 10
- 238000005554 pickling Methods 0.000 claims description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 5
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 5
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 5
- 239000001488 sodium phosphate Substances 0.000 claims description 5
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 5
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 5
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 5
- 150000002680 magnesium Chemical class 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims 5
- 239000000243 solution Substances 0.000 claims 4
- 230000003213 activating effect Effects 0.000 claims 2
- 230000008569 process Effects 0.000 abstract description 14
- 238000000151 deposition Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000008021 deposition Effects 0.000 abstract description 5
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000956 alloy Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 15
- 238000005238 degreasing Methods 0.000 description 8
- 229910052720 vanadium Inorganic materials 0.000 description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 229910052725 zinc Inorganic materials 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 238000007598 dipping method Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- 229910001096 P alloy Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
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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
- 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
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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
- 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
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/12—Light metals
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/22—Light metals
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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- Inorganic Chemistry (AREA)
- Chemically Coating (AREA)
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Abstract
The invention discloses a direct chemical nickel plating method universally used for AZ91D and ZK61M magnesium alloys, which comprises the following steps: step 1, sand blasting; step 2, removing oil by ultrasonic waves; step 3, acid washing; step 4, activation; step 5, chemical nickel plating; and 6, drying, and adding running water for cleaning among the steps. The invention can be generally used for AZ91D and ZK61M magnesium alloys, and reduces the chemical nickel plating process, the production and the management cost caused by the difference of AZ91D and ZK61M magnesium alloy materials; the invention can directly carry out chemical nickel plating, and solves the problems of complex process, safe use of cyanide, environmental hazard of waste liquid, pollution of chemical nickel plating solution, unstable surface of chemical nickel plating layer, shortened service life of chemical nickel plating solution and the like in the prior art; the chemical nickel plating deposition speed of the invention is high, can reach 10-15 microns/hour, and can be used for mass production.
Description
Technical Field
The invention belongs to a magnesium alloy surface treatment technology, and particularly relates to a method for directly chemically plating nickel on magnesium alloy commonly used for AZ91D and ZK 61M.
Background
The AZ91D and ZK61M magnesium alloy is light engineering material with density being equal to that of engineering plastic, the density is 2/3 of aluminum, the density is 1/4 of iron, and the magnesium alloy is one of the lightest metal structure materials, and simultaneously has good processability, dimensional stability, electric and thermal conductivity, electromagnetic shielding property, shock absorption property, processability and recyclability, and the magnesium alloy becomes the metal structure material which is the first choice in lightweight design in the fields of aerospace and military industry due to the excellent properties of the magnesium alloy.
However, the electrode potential of the magnesium alloy is-2.37V, the magnesium alloy is an extremely active metal material, the corrosion resistance is extremely poor, and the application of the magnesium alloy is limited, but the performance of the magnesium alloy after chemical nickel plating is improved, and the application of the magnesium alloy is greatly promoted. The chemical nickel plating of magnesium alloy mainly comprises two methods of zinc dipping method and direct chemical plating method, and the zinc dipping method has the problems of complex process, safe use of cyanide, treatment of waste liquid and the like, so the method of direct chemical nickel plating of magnesium alloy is gradually emphasized.
The prior art has disclosed some chemical nickel plating technical schemes of AZ91D and ZK61M magnesium alloy, for example, the Chinese patent with publication number CN107937887A, "a method for chemical nickel plating of magnesium alloy" and the Chinese patent with publication number CN104894540A, "a chemical nickel plating process commonly used for magnesium-lithium alloy and magnesium-aluminum alloy" both adopt a zinc immersion method chemical nickel plating process. The Chinese patent with publication number CN 102994998A 'is used for direct chemical nickel plating solution and chemical nickel-phosphorus plating process for magnesium alloy', the direct chemical nickel plating solution for magnesium alloy can be used for magnesium alloy such as AZ91D, but the deposition speed of chemical nickel plating is 6-8 microns/hour, the plating speed is slow, the efficiency is low, and the direct chemical nickel plating solution is not suitable for mass production. Chinese patent with publication number CN107955944A, AZ91D magnesium alloy direct chemical nickel plating solution and preparation method thereof, has fast plating speed which can reach 11.25-14.70 microns/hour, but the invention is only suitable for AZ91D magnesium alloy. Chinese patent publication No. CN106835085A, "a method for chemically plating nickel-phosphorus alloy on ZK61M magnesium alloy complex pieces", but the method is only applicable to ZK61M magnesium alloy.
AZ91D and ZK61M are magnesium alloy materials used by the unit in a relatively large number, AZ91D and ZK61M magnesium alloys adopt different chemical nickel plating processes and methods in the past due to differences in material components, production and management costs are increased, a rapid, stable and general method for AZ91D and ZK61M magnesium alloys and a direct chemical nickel plating method are researched, and the method has very important practical significance.
Disclosure of Invention
The invention aims to provide a method for directly and chemically plating nickel on magnesium alloy commonly used for AZ91D and ZK61M, aiming at the defects that the chemical nickel plating process is different from the method due to the difference of the material components of the AZ91D and ZK61M magnesium alloys, and the problems of complex process, unstable chemical nickel plating layer, short service life of chemical plating solution and the like caused by the chemical nickel plating process adopting a zinc dipping method in the prior art.
The technical solution for realizing the purpose of the invention is as follows: a method for direct chemical nickel plating of magnesium alloy commonly used in AZ91D and ZK61M comprises the following steps:
step 1, sand blasting: respectively carrying out 100-mesh sand blasting treatment on the surfaces of magnesium alloy workpieces, wherein the magnesium alloy workpieces are AZ91D or ZK 61M;
step 2, ultrasonic oil removal: putting the magnesium alloy workpiece subjected to sand blasting treatment into ultrasonic cleaning equipment for ultrasonic oil removal;
step 3, acid washing: placing the degreased magnesium alloy workpiece into an acid-resistant tank with an air draft device for acid washing treatment at room temperature to remove rust and oxide skin on the surface of the magnesium alloy workpiece;
step 4, activation: placing an acid-proof tank with an air draft device at room temperature, and carrying out activation treatment on the magnesium alloy workpiece after pickling to remove oxides formed during pickling;
step 5, chemical nickel plating: carrying out chemical nickel plating treatment on the activated magnesium alloy workpiece in an acid-resistant groove with an air draft device;
and 6, drying: and drying the magnesium alloy workpiece after the chemical nickel plating in an oven until the magnesium alloy workpiece is completely dried.
Compared with the prior art, the invention has the remarkable advantages that:
(1) compared with other processes only suitable for single AZ91D or ZK61M magnesium alloy, the invention can be universally used for AZ91D and ZK61M magnesium alloy, reduces the process production and management cost of the magnesium alloy caused by material component difference, and enhances the market competitiveness.
(2) Compared with other chemical nickel plating processes of zinc dipping methods, the direct chemical nickel plating method adopted by the invention has the advantages of simple process, no safety problem of using cyanide, and avoidance of the problems of instability of a chemical nickel plating layer and short service cycle of a chemical nickel plating solution caused by the dissolution of zinc in the chemical nickel plating step.
(3) Compared with the chemical nickel plating deposition speed of 6-8 um/h of other technologies, the chemical nickel plating deposition speed is 10-15 um/h, the chemical nickel plating deposition speed is high, the efficiency is high, and the chemical nickel plating deposition method is suitable for mass production.
Drawings
FIG. 1 shows the general process steps of the present invention for direct electroless nickel plating of AZ91D and ZK61M magnesium alloys.
Detailed Description
The present invention is described in further detail below with reference to the attached drawing figures.
With reference to fig. 1, the invention provides a method for directly and chemically plating nickel on magnesium alloy commonly used for AZ91D and ZK61M, which comprises the following steps:
step 1, sand blasting: carrying out 100-mesh sand blasting treatment on the surface of an AZ91D or ZK61M magnesium alloy workpiece to remove defects such as pits on the surface of a base material;
step 2, ultrasonic oil removal: in a fixed groove with ultrasonic cleaning equipment, carrying out ultrasonic degreasing on an AZ91D or ZK61M magnesium alloy base material to remove oil stains on the surface, wherein in the ultrasonic degreasing step, an ultrasonic solution comprises 40-50 g/L of sodium hydroxide, 10-15 g/L of trisodium phosphate and 5-10 g/L of sodium carbonate, the time is 20-30 min, and the temperature is 50-55 ℃;
step 3, acid washing: performing acid pickling treatment in an acid-resistant tank with an air draft device at room temperature to remove rust and oxide skin on the surface of the AZ91D or ZK61M magnesium alloy base material, wherein in the acid pickling step, the acid pickling solution comprises 80-120 g/L chromic anhydride, 90-110 ml/L nitric acid (70% V/V) and 90-110 ml/L hydrofluoric acid, the time is 30-60 s, and the temperature is room temperature;
step 4, activation: performing activation treatment in an acid-resistant tank with an air draft device at room temperature to remove oxides formed during acid cleaning, wherein in the activation step, the activation solution comprises 340-360 mL/L hydrofluoric acid, 290-310 mL/L nitric acid (70% V/V) and 340-360 mL/L phosphoric acid, the time is 5-10 min, and the temperature is room temperature;
step 5, chemical nickel plating: in an acid-resistant tank with an air draft device, performing chemical nickel plating treatment on an AZ91D or ZK61M magnesium alloy matrix, wherein in the step of chemical nickel plating, the chemical nickel plating solution comprises 10-15 g/L of nickel carbonate, 18-22 g/L of sodium hypophosphite, 10-14 ml/L of hydrofluoric acid, 1-1.5 mg/L of thiourea, 6-8 g/L of ammonium bifluoride, 4.5-6 g/L of citric acid, 6-8 mg/L of sodium dodecyl sulfate, 6.0 +/-0.4 of pH, 80 +/-5 ℃ of temperature, 60-120 min of time, and is determined according to the thickness and 10-15 um/h.
And 6, drying: and drying in an oven until complete drying, wherein in the drying step, the drying temperature is 50-100 ℃ until drying.
And adding running water for cleaning among the steps.
Example 1
Step 1, sand blasting: the surface of the ZK61M magnesium alloy workpiece is subjected to 100-mesh sand blasting treatment to remove defects such as pits and the like on the surface of the base material.
Step 2, ultrasonic oil removal: in a fixed groove with ultrasonic cleaning equipment, the ZK61M magnesium alloy substrate is subjected to ultrasonic degreasing to remove oil stains on the surface, and in the ultrasonic degreasing step, the ultrasonic solution comprises 45 g/L of sodium hydroxide, 12 g/L of trisodium phosphate and 8 g/L of sodium carbonate, the time is 25 min, and the temperature is 52 ℃.
Step 3, acid washing: in the acid washing step, acid washing treatment is carried out in an acid-resistant tank with an air draft device at room temperature to remove rust and scale on the surface of the ZK61M magnesium alloy base material, wherein the acid washing solution comprises 110 g/L of chromic anhydride, 110 ml/L of nitric acid (70% V/V) and 105 ml/L of hydrofluoric acid, the time is 50 s, and the temperature is room temperature.
Step 4, activation: and performing activation treatment to remove oxides formed in acid cleaning in an acid-resistant tank with an air draft device at room temperature, wherein in the activation step, the activation solution comprises 340 mL/L hydrofluoric acid, 290 mL/L nitric acid (70% V/V) and 340 mL/L phosphoric acid, the time is 10 min, and the temperature is room temperature.
Step 5, chemical nickel plating: in an acid-proof tank with an air draft device, a ZK61M magnesium alloy substrate is subjected to chemical nickel plating treatment, and in the chemical nickel plating step, the chemical nickel plating solution comprises 15 g/L of nickel carbonate, 22 g/L of sodium hypophosphite, 14 ml/L of hydrofluoric acid, 1.5 mg/L of thiourea, 8 g/L of ammonium bifluoride, 6 g/L of citric acid, 8 mg/L of sodium dodecyl sulfate, the pH value is 6.4, the temperature is 85 ℃, and the time is 80 min.
And 6, drying: and (3) carrying out drying treatment in an oven until the drying is completely carried out, wherein in the drying step, the drying temperature is 80 ℃ until the drying is carried out.
And adding running water for cleaning among the steps.
Example 2
Step 1, sand blasting: and (3) carrying out 100-mesh sand blasting treatment on the surface of the AZ91D magnesium alloy workpiece to remove defects such as pits and the like on the surface of the base material.
Step 2, ultrasonic oil removal: in a fixed groove with ultrasonic cleaning equipment, the ZK61M magnesium alloy substrate is subjected to ultrasonic degreasing to remove oil stains on the surface, and in the ultrasonic degreasing step, the ultrasonic solution comprises 42 g/L of sodium hydroxide, 13 g/L of trisodium phosphate, 7 g/L of sodium carbonate, 22 min of time and 54 ℃ of temperature.
Step 3, acid washing: in the acid washing step, acid washing treatment is carried out in an acid-resistant tank with an air draft device at room temperature to remove rust and scale on the surface of the ZK61M magnesium alloy base material, wherein the acid washing solution comprises 100 g/L of chromic anhydride, 100 ml/L of nitric acid (70% V/V), 100 ml/L of hydrofluoric acid, the time is 40 s, and the temperature is room temperature.
Step 4, activation: and in the activation step, the activation solution comprises 360 mL/L hydrofluoric acid, 310 mL/L nitric acid (70% V/V) and 360 mL/L phosphoric acid, the time is 5 min, and the temperature is room temperature.
Step 5, chemical nickel plating: in an acid-proof tank with an air draft device, a ZK61M magnesium alloy substrate is subjected to chemical nickel plating treatment, and in the chemical nickel plating step, the chemical nickel plating solution comprises 10 g/L of nickel carbonate, 18 g/L of sodium hypophosphite, 10 ml/L of hydrofluoric acid, 1 mg/L of thiourea, 6 g/L of ammonium bifluoride, 4.5 g/L of citric acid, 6 mg/L of sodium dodecyl sulfate, the pH value is 6, the temperature is 75 ℃, and the time is 110 min.
And 6, drying: and (3) carrying out drying treatment in an oven until the drying is completely carried out, wherein in the drying step, the drying temperature is 80 ℃ until the drying is carried out.
And adding running water for cleaning among the steps.
Example 3
Step 1, sand blasting: and (3) carrying out 100-mesh sand blasting treatment on the surface of the AZ91D magnesium alloy workpiece to remove defects such as pits and the like on the surface of the base material.
Step 2, ultrasonic oil removal: in a fixed groove with ultrasonic cleaning equipment, the ZK61M magnesium alloy substrate is subjected to ultrasonic degreasing to remove oil stains on the surface, and in the ultrasonic degreasing step, the ultrasonic solution comprises 42 g/L of sodium hydroxide, 13 g/L of trisodium phosphate, 7 g/L of sodium carbonate, 22 min of time and 54 ℃ of temperature.
Step 3, acid washing: in the acid washing step, acid washing treatment is carried out in an acid-resistant tank with an air draft device at room temperature to remove rust and scale on the surface of the ZK61M magnesium alloy base material, wherein the acid washing solution comprises 100 g/L of chromic anhydride, 100 ml/L of nitric acid (70% V/V), 100 ml/L of hydrofluoric acid, the time is 40 s, and the temperature is room temperature.
Step 4, activation: and performing activation treatment to remove oxides formed in acid cleaning in an acid-resistant tank with an air draft device at room temperature, wherein in the activation step, the activation solution comprises 345 mL/L of hydrofluoric acid, 305 mL/L of nitric acid (70% V/V) and 355 mL/L of phosphoric acid, the time is 7 min, and the temperature is room temperature.
Step 5, chemical nickel plating: in an acid-proof tank with an air draft device, a ZK61M magnesium alloy substrate is subjected to chemical nickel plating treatment, and in the chemical nickel plating step, the chemical nickel plating solution comprises 14 g/L of nickel carbonate, 21 g/L of sodium hypophosphite, 13 ml/L of hydrofluoric acid, 1.4 mg/L of thiourea, 6.5 g/L of ammonium bifluoride, 5 g/L of citric acid and 6 mg/L of sodium dodecyl sulfate, the pH value is 6.2, the temperature is 80 ℃, and the time is 80 min.
And 6, drying: and (3) carrying out drying treatment in an oven until the drying is completely carried out, wherein in the drying step, the drying temperature is 80 ℃ until the drying is carried out.
And adding running water for cleaning among the steps.
Claims (9)
1. A method for directly and chemically plating nickel on magnesium alloy commonly used for AZ91D and ZK61M is characterized by comprising the following steps:
step 1, sand blasting: respectively carrying out 100-mesh sand blasting treatment on the surfaces of magnesium alloy workpieces, wherein the magnesium alloy workpieces are AZ91D or ZK 61M;
step 2, ultrasonic oil removal: putting the magnesium alloy workpiece subjected to sand blasting treatment into ultrasonic cleaning equipment for ultrasonic oil removal;
step 3, acid washing: placing the degreased magnesium alloy workpiece into an acid-resistant tank with an air draft device for acid washing treatment at room temperature to remove rust and oxide skin on the surface of the magnesium alloy workpiece;
step 4, activation: placing an acid-proof tank with an air draft device at room temperature, and carrying out activation treatment on the magnesium alloy workpiece after pickling to remove oxides formed during pickling;
step 5, chemical nickel plating: carrying out chemical nickel plating treatment on the activated magnesium alloy workpiece in an acid-resistant groove with an air draft device;
and 6, drying: and drying the magnesium alloy workpiece after the chemical nickel plating in an oven until the magnesium alloy workpiece is completely dried.
2. The method of direct chemical nickel plating of magnesium alloy of AZ91D and ZK61M as claimed in claim 1, wherein: in the step 2, the ultrasonic solution in the ultrasonic cleaning equipment adopts 40-50 g/L sodium hydroxide, 10-15 g/L trisodium phosphate and 5-10 g/L sodium carbonate to form a mixed solution, the cleaning time is 20-30 min, and the temperature is 50-55 ℃.
3. The method of direct chemical nickel plating of magnesium alloy of AZ91D and ZK61M as claimed in claim 1, wherein: in the step 3, the acid washing solution is a mixed solution of 80-120 g/L chromic anhydride, 90-110 ml/L nitric acid and 90-110 ml/L hydrofluoric acid, the acid washing time is 30-60 s, and the temperature is room temperature.
4. The method of the direct chemical nickel plating of the magnesium alloy of AZ91D and ZK61M in the common use according to claim 3, which is characterized in that: the nitric acid concentration was 70%.
5. The method of direct chemical nickel plating of magnesium alloy of AZ91D and ZK61M as claimed in claim 1, wherein: in the step 4, the activating solution is a mixed solution of 340-360 mL/L hydrofluoric acid, 290-310 mL/L nitric acid and 340-360 mL/L phosphoric acid, the activating time is 5-10 min, and the temperature is room temperature.
6. The method of direct chemical nickel plating of magnesium alloy of AZ91D and ZK61M as claimed in claim 5, wherein: the nitric acid concentration was 70%.
7. The method of direct chemical nickel plating of magnesium alloy of AZ91D and ZK61M as claimed in claim 1, wherein: in the step 5, the chemical nickel plating solution is a mixed solution of 10-15 g/L of nickel carbonate, 18-22 g/L of sodium hypophosphite, 10-14 ml/L of hydrofluoric acid, 1-1.5 mg/L of thiourea, 6-8 g/L of ammonium bifluoride, 4.5-6 g/L of citric acid and 6-8 mg/L of sodium dodecyl sulfate, the pH value of the mixed solution is 6.0 +/-0.4, the temperature is 80 +/-5 ℃, and the time is 60-120 min.
8. The method of direct chemical nickel plating of magnesium alloy of AZ91D and ZK61M as claimed in claim 1, wherein: in the step 6, the drying temperature is 50-100 ℃ until drying.
9. The method of direct chemical nickel plating of magnesium alloy of AZ91D and ZK61M as claimed in claim 1, wherein: and adding running water for cleaning among the steps.
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