CN101717926A - Chemical nickel-plating method for ZM6 magnesium alloy - Google Patents

Chemical nickel-plating method for ZM6 magnesium alloy Download PDF

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Publication number
CN101717926A
CN101717926A CN200910312432A CN200910312432A CN101717926A CN 101717926 A CN101717926 A CN 101717926A CN 200910312432 A CN200910312432 A CN 200910312432A CN 200910312432 A CN200910312432 A CN 200910312432A CN 101717926 A CN101717926 A CN 101717926A
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plating
nickel
solution
acid
magnesium alloy
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刘楚明
高艳蕊
傅圣利
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Central South University
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Central South University
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Abstract

The invention relates to a method for chemically plating nickel to a ZM6 magnesium alloy. The method comprises the steps of performing pretreatment on a magnesium alloy matrix before plating and then performing chemical nickel plating to deposit a chemical nickel-plating layer, wherein the pretreatment before plating comprises four steps, namely alkali washing, acid washing, acid etching and zinc dipping; and the chemical nickel-plating layer is obtained by adopting basic nickel carbonate serving as a main salt, sodium hypophosphite serving as a reducing agent, hydrofluoric acid serving as a corrosion inhibitor, lactic acid serving as a complexing agent and mixed solution of cadmium sulfate and potassium iodate serving as a brightening agent and a stabilizing agent. The bright and flat nickel-plating layer can be obtained by plating at the temperature of about 85 DEG C after the zinc dipping of a plated piece. The method is suitable for chemically plating the nickel to the ZM6 magnesium alloy material to achieve the aim of protecting the ZM6 magnesium alloy. The method has the advantages of high plating speed and good protection.

Description

A kind of ZM6 magnesium-alloy chemical nickel coating method
Technical field
The present invention relates to a kind of ZM6 magnesium-alloy chemical nickel coating method, belong to the metal corrosion and protection technical field.
Background technology
Magnesium alloy is the density minimum in practical structural metallic materials, is 1.74g/cm 3, be 1/3 of iron and steel, 2/3 of aluminium.Because that it has is as far as possible light, specific tenacity is high, shock resistance good, good electro-magnetic screen function and heat conduction, electroconductibility is good and be easy to excellent properties such as recycling, makes magnesium and alloy thereof have broad application prospects in fields such as defence and military, traffic, communications.Yet corrosion failure very easily takes place in magnesium alloy chemical activity height, further promotes and uses so the solidity to corrosion difference is restricting it.For this reason, magnesium alloy must carry out the surfacecti proteon processing before use.Wherein chemical nickel plating not only can make it obtain stronger solidity to corrosion and wear resistance, and have the texture and the outward appearance of weldability and electroconductibility and metal as a kind of effective guard technology.
ZM6 (Mg-2.6Nd-0.6Zn-0.8Zr) alloy system is mainly used in housing parts such as casing, oil pump cover as heat-resistance high-strength degree cast magnesium alloys, however the rare report of its surfacecti proteon problem.The chemically coating nickel by magnesium-alloy pre-treatment is subjected to matrix effect bigger, and the pre existing treatment process easily causes the ZM6 magnesium alloy decortication to occur in nickel process and plating speed waits problem slowly, therefore seeks the pre-treating process of suitable ZM6 matrix, and is favourable to subsequent chemistry nickel plating.
Summary of the invention
The objective of the invention is to remedy existing deficiency, proposed a kind of chemical nickel plating method at the ZM6 magnesium alloy surface protective, plating speed is fast, and solidity to corrosion and bonding force are good.
The objective of the invention is to realize by following technical proposals: a kind of ZM6 magnesium-alloy chemical nickel coating method may further comprise the steps:
Pre-treatment before A, the plating:
Earlier magnesium alloy substrate is carried out alkali cleaning, pickling, acid etching and soaks zinc; Soda-wash solution is sodium hydroxide 50-70g/L and OP-100.5-1.5ml/L, and the solution-operated temperature is 60-80 ℃, treatment time 1min; Acidwash solution is the oxalic acid of 15-25g/L, and service temperature is a room temperature, and the treatment time is 10-25s; The acid etching solution composition is nitric acid 80-100ml/L and chromic acid 80-100g/L, and the solution-operated temperature is a room temperature, and the treatment time is 1min; Zinc dipping solution is zinc oxide 20-30g/L, hydroxyl bisphosphate 70-80ml/L, quadrol 12-18ml/L and phosphoric acid 8-10ml/L; Service temperature is 82-86 ℃, and pH value is 9.2-9.6, treatment time 1min.
B, chemical nickel plating and sealing of hole are handled, and it is main salt that nickel plating solution adopts basic nickel carbonate, and inferior sodium phosphate is a reductive agent, and lactic acid is complexing agent, and hydrofluoric acid is inhibiter, and Cadmium Sulphate and Potassium Iodate are brightening agent; Hole sealing solution is a paraffin oil.
Nickel plating solution consists of basic nickel carbonate 12-18g/L; Ortho phosphorous acid 25-35g/L; Hydrofluoric acid 40-50ml/L; Lactic acid 28-35ml/L; Brightening agent 3.5-5ml/L; The service temperature 82-86 of nickel plating solution ℃, pH value is 4.5-5.0, treatment time 2h.
Described brightening agent is made up of 2-3mg/L Cadmium Sulphate and 5.5-7.5mg/L Potassium Iodate.
Hole sealing solution is a paraffin oil, and service temperature 180-200 ℃, the treatment time is 3-5min.
At alkali cleaning, pickling, acid etching, soak between zinc and electroless nickel step and all wash, the washing time is 30s.
The present invention compared with prior art has the following advantages: 1. employing current pretreatment approaches, and plating bath is carried out chemical nickel plating to the ZM6 magnesium alloy, can produce decortication, and plating speed is slow, cause solidity to corrosion and bonding force not strong.And the present invention has carried out big improvement according to the own characteristic of ZM6 magnesium alloy on pretreatment process, has improved plating bath simultaneously, creates the chemical nickel plating method that a cover is suitable for the ZM6 magnesium alloy first; Existing chemical nickel plating method can plate 2h continuously and not peel, and has accelerated plating speed, and corrosion resistance of coating is good, and is firm with matrix bond; 2, the main salt of chemical nickel plating employing of the present invention is basic nickel carbonate, and little to magnesium alloy substrate corrodibility, simple to operate, bath stability is good, is easy to safeguard; 3. pretreatment process of the present invention, solution compolision is simple, is easy to control, process stabilizing; 4. the zinc-impregnating layer that obtains with zinc dipping solution of the present invention is even and bonding force is good.
Description of drawings
Fig. 1 is a ZM6 nickel chemical plating technology schema provided by the invention;
Fig. 2 is that the ZM6 magnesium alloy is handled the rear surface pattern through chemical nickel plating;
Fig. 3 is ZM6 matrix and nickel layer polarization curve comparison diagram.
Embodiment
Be described further for the present invention below in conjunction with example, and can not limit the present invention.
Embodiment
Below in conjunction with the flow process among Fig. 1 ZM6 magnesium-alloy chemical nickel coating method of the present invention is described.
Test materials is the ZM6 magnesium alloy, and casting is after T6 thermal treatment, and concrete technology is 520 ℃/12h+200 ℃/17h.Size of sample is the square sample of 20mm * 15mm * 5mm, and it is handled by following operation steps:
Step 1: with magnesium alloy through 180#, 360#, 1000# sand paper water mill is until surface clean, there is not obvious impurity.
Step 2, magnesium alloy is immersed soda-wash solution carry out oil removing.
The prescription of soda-wash solution is as follows: sodium hydroxide 60g/L; OP-10 1ml/L; During alkali cleaning, controlled temperature is 65 ℃, and the time is 1 minute.
Step 3, usefulness flushing with clean water magnesium alloy 30s, flush away surface alkaline wash.
Step 4, magnesium alloy is immersed Acidwash solution, the oxide film that generates when removing alkali cleaning.The prescription of Acidwash solution is as follows: oxalic acid 20g/L; The pickling service temperature is a room temperature, and the time is 20 seconds.
Step 5, usefulness flushing with clean water magnesium alloy 30s, flush away surface acid washing lotion.
Step 6, magnesium alloy is immersed acid etching solution.The prescription of acid etching solution is as follows: nitric acid 90ml/L; Chromic acid 90g/L; The acid etching service temperature is a room temperature.
Step 7, usefulness flushing with clean water magnesium alloy 30s, flush away surface pickling solution.
Step 8, magnesium alloy immersed soak zinc in the zinc dipping solution and handle.The zinc dipping solution prescription is as follows: zinc oxide 25g/L, hydroxyl bisphosphate 75ml/L, quadrol 15ml/L and phosphatase 79 ml/L; Service temperature is 85 ℃, and pH value is 9.5,1 minute treatment time.
Step 9, usefulness flushing with clean water magnesium alloy 30s, flush away surface zincate solution.
Step 10: will carry out chemical plating in the ZM6 magnesium alloy immersion chemical nickel-plating solution.The prescription of chemical nickel-plating solution is as follows: basic nickel carbonate 15g/L; Inferior sodium phosphate 30g/L is as reductive agent; Hydrofluoric acid 45ml/L is as inhibiter; Lactic acid 33ml/L is as complexing agent; Cadmium Sulphate 3mg/L and Potassium Iodate 6mg/L be as brightening agent, brightening agent 4ml/L; During the chemistry plating, controlled temperature is 80-85 ℃, and pH value is 4.8, and the time is 2 hours.
Step 11: with clear water the chemical nickel-plating solution on magnesium alloy materials surface is rinsed well, and oven dry.
Step 12: magnesium alloy materials is put into hole sealing solution carry out sealing of hole.Pore-sealing liquid is a paraffin oil, and service temperature is 180 ℃, and the time is 3 minutes.
Step 13: room temperature is dried.
Adopt its nickel layer of ZM6 magnesium alloy nickel plating part that above-mentioned technology obtains after tested, performance is shown in subordinate list:
Subordinate list: the chemical Ni-plating layer performance that adopts the inventive method to obtain
Test event Testing method Test result
Thickness of coating Get the coating cross section, after the polishing of 1000# silicon carbide paper, under scanning electron microscope, measure. The about 62 μ m of bed thickness
Thermal shock test Take out plating piece is incubated 1 hour in 130 ℃ of loft drier after and drop into that not to be higher than in 15 ℃ of water be a circulation Cycle index is no less than 20 times, and nickel layer does not have bubble, comes off or other inefficacy defective
Salt fog Salts solution 50 ± 1g/L, 35 ℃ keep PH down between 6.5=7.2, rate of salt spray precipitation, 1.0-2.0ml/h (80cm 2Horizontal collecting region in); Temperature in the salt-spray cabinet efficiency test space is 35 ± 2 ℃; Continue spraying in the duration of test, then off-test of first hot spot occurs. Salt-fog resistant time reaches 158 hours
Fig. 2 is the surface topography of this ZM6 magnesium alloy after chemical nickel plating is handled, and as seen from Figure 2, coating is even tiny born of the same parents' shape thing, no significant defect and hole.Fig. 3 is ZM6 matrix and nickel layer polarization curve comparison diagram, and there is tangible passivation region in the coating anodic process, and the nickel layer solidity to corrosion obviously improves than matrix, and current potential is obviously shuffled, and corrosion current reduces an order of magnitude.

Claims (5)

1. a ZM6 magnesium-alloy chemical nickel coating method is characterized in that, may further comprise the steps:
Pre-treatment before A, the plating:
Earlier magnesium alloy substrate is carried out alkali cleaning, pickling, acid etching and soaks zinc; Soda-wash solution is sodium hydroxide 50-70g/L and OP-10 0.5-1.5ml/L, and the solution-operated temperature is 60-80 ℃, treatment time 1min; Acidwash solution is the oxalic acid of 15-25g/L, and service temperature is a room temperature, and the treatment time is 10-25s; Acid etching solution is nitric acid 80-100ml/L and chromic acid 80-100g/L, and the solution-operated temperature is a room temperature, and the treatment time is 1min; Zinc dipping solution is zinc oxide 20-30g/L, hydroxyl bisphosphate 70-80ml/L, quadrol 12-18ml/L and phosphoric acid 8-10ml/L; Service temperature is 82-86 ℃, and pH value is 9.2-9.6, treatment time 1min;
B, carry out chemical nickel plating and sealing of hole and handle, it is main salt that nickel plating solution adopts basic nickel carbonate, and inferior sodium phosphate is a reductive agent, and lactic acid is complexing agent, and hydrofluoric acid is inhibiter, and Cadmium Sulphate and Potassium Iodate are brightening agent, adopt the paraffin oil sealing of hole to handle at last.
2. ZM6 magnesium-alloy chemical nickel coating method according to claim 1 is characterized in that: nickel plating solution consists of basic nickel carbonate 12-18g/L; Inferior sodium phosphate 25-35g/L; Hydrofluoric acid 40-50ml/L; Lactic acid 28-35ml/L; Brightening agent 3.5-5ml/L; The service temperature 82-86 of nickel plating solution ℃, pH value is 4.5-5.0, treatment time 2h.
3. ZM6 magnesium-alloy chemical nickel coating method according to claim 1 is characterized in that: described brightening agent is made up of 2-3mg/L Cadmium Sulphate and 5.5-7.5mg/L Potassium Iodate.
4. ZM6 magnesium-alloy chemical nickel coating method according to claim 1 is characterized in that: hole sealing solution is a paraffin oil, and service temperature 180-200 ℃, the treatment time is 3-5min.
5. ZM6 magnesium-alloy chemical nickel coating method according to claim 1 is characterized in that: at alkali cleaning, pickling, acid etching, soak between zinc and electroless nickel step and all wash, the washing time is 30s.
CN200910312432A 2009-12-28 2009-12-28 Chemical nickel-plating method for ZM6 magnesium alloy Pending CN101717926A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101892471A (en) * 2010-07-09 2010-11-24 中南大学 Chemical nickel plating process of Mg-Gd-Y-Zr magnesium alloy
CN102817019A (en) * 2012-08-01 2012-12-12 西安理工大学 Plating solution for chemical plating of nickel-phosphorus metal layer on surface of magnesium alloy as well as preparation and use method for plating solution
CN103757614A (en) * 2014-01-02 2014-04-30 上海交通大学 Magnesium and magnesium alloy coating and preparation method thereof
CN104195533A (en) * 2014-09-15 2014-12-10 国家电网公司 Nickel zinc phosphorus chemical plating layer and preparation method thereof as well as chemical plating liquid
CN108165957A (en) * 2017-07-27 2018-06-15 中国航发哈尔滨东安发动机有限公司 Aluminum alloy material surface chemical nickel plating method
CN113008650A (en) * 2019-12-20 2021-06-22 中核北方核燃料元件有限公司 Metallographic corrosive agent and metallographic corrosive method for UN fuel pellets

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101892471A (en) * 2010-07-09 2010-11-24 中南大学 Chemical nickel plating process of Mg-Gd-Y-Zr magnesium alloy
CN101892471B (en) * 2010-07-09 2012-06-06 中南大学 Chemical nickel plating process of Mg-Gd-Y-Zr magnesium alloy
CN102817019A (en) * 2012-08-01 2012-12-12 西安理工大学 Plating solution for chemical plating of nickel-phosphorus metal layer on surface of magnesium alloy as well as preparation and use method for plating solution
CN103757614A (en) * 2014-01-02 2014-04-30 上海交通大学 Magnesium and magnesium alloy coating and preparation method thereof
CN103757614B (en) * 2014-01-02 2016-08-17 上海交通大学 A kind of coating of magnesium and magnesium alloy and preparation method thereof
CN104195533A (en) * 2014-09-15 2014-12-10 国家电网公司 Nickel zinc phosphorus chemical plating layer and preparation method thereof as well as chemical plating liquid
CN108165957A (en) * 2017-07-27 2018-06-15 中国航发哈尔滨东安发动机有限公司 Aluminum alloy material surface chemical nickel plating method
CN113008650A (en) * 2019-12-20 2021-06-22 中核北方核燃料元件有限公司 Metallographic corrosive agent and metallographic corrosive method for UN fuel pellets

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Open date: 20100602