CN101892471B - Chemical nickel plating process of Mg-Gd-Y-Zr magnesium alloy - Google Patents
Chemical nickel plating process of Mg-Gd-Y-Zr magnesium alloy Download PDFInfo
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- CN101892471B CN101892471B CN2010102216835A CN201010221683A CN101892471B CN 101892471 B CN101892471 B CN 101892471B CN 2010102216835 A CN2010102216835 A CN 2010102216835A CN 201010221683 A CN201010221683 A CN 201010221683A CN 101892471 B CN101892471 B CN 101892471B
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Abstract
The invention relates to a chemical nickel plating method of an Mg-Gd-Y-Zr (wt%) magnesium alloy. The method comprises pre-plating pretreatment of a magnesium alloy matrix and deposition of a chemical nickel plating layer through chemical nickel plating, wherein the pre-plating pretreatment process comprises five steps of removing oil, activating, acid-washing, reactivating and zinc galvanizing; chemical nickel plating solution takes basic nickel carbonate as main salt, sodium hypophosphite as a reducing agent, hydrofluoric acid as a corrosion inhibitor, lactic acid as a complex agent and mixed liquor of cadmium sulfate and potassium iodate as a brightening agent; and a plating component is subject to zinc galvanizing and then electroless plating at the temperature about 85 DEG C to obtain the bright, flat, uniform and compact nickel plating layer. The chemical nickel plating method is applicable to chemical nickel plating on the surface of the Mg-Gd-Y-Zr magnesium alloy, thus achieving the purpose of protecting the magnesium alloy. The chemical nickel plating method has the advantages of fast plating speed, good protectiveness, simple operation and easy control.
Description
Technical field
The present invention relates to a kind of Mg-Gd-Y-Zr chemical nickel plating process on magnesium alloy, belong to the metal corrosion and protection field.
Background technology
Magnesiumalloy has excellent properties such as high specific strength, shock resistance is good, amount is light, makes them have broad application prospects in fields such as aerospace, electronics, automotive industrys.Yet the magnesium alloy chemical activity is high, very easily corrodes, and further applies so the solidity to corrosion difference is restricting it.Therefore, magnesiumalloy must carry out the surfacecti proteon processing before practical application.Chemical nickel plating is one of a kind of simple, the most most economical surface protection technique that is widely used, and can make magnesiumalloy obtain good solidity to corrosion and wear resistance, also has weldability and electroconductibility and metal-like and outward appearance.
Research shows that Mg-Gd-Y-Zr is that alloy has that height ratio is strong, the height ratio mould, corrosion-resistant, be prone to advantages such as welding, resistance toheat are good; Its mechanical property all obviously is superior to generally acknowledging at present heat resistance magnesium alloys such as outstanding WE54, ZM6; And the intensity of alloy is very high; Can partly replace duraluminum at aerospace field and carry out loss of weight, have good development prospect.Yet be that the surface protection technique research report of alloy is few at present to Mg-Gd-Y-Zr.Magnesiumalloy belongs to difficult plating base material, therefore must plate preceding pre-treatment, and matrix is very big to pretreated influence; Current pretreatment approaches is not too suitable to the Mg-Gd-Y-Zr magnesiumalloy; Cause in Ni-Speed, producing a lot of problems, fail to plate, produce defectives such as peeling, bubbling like part.Therefore seek the pretreatment process that is fit to the Mg-Gd-Y-Zr magnesiumalloy, help follow-up nickel process.
Summary of the invention
The objective of the invention is to remedy the deficiency of existing nickel chemical plating technology, proposed a kind of chemical nickel plating method to the Mg-Gd-Y-Zr magnesium alloy surface protective, this method plating speed is fast, and it is good to obtain coating even compact, solidity to corrosion and bonding force.
The objective of the invention is to realize through following technical proposals: a kind of Mg-Gd-Y-Zr magnesium-alloy chemical nickel coating method may further comprise the steps:
Pre-treatment before A, the plating:
Earlier magnesium alloy substrate is carried out oil removing, activation, pickling, reactivate and soaks zinc.Removing oil solution is yellow soda ash 30g/L, sodium phosphate 30g/L and OP-101-2ml/L, and the solution-operated temperature is 60-80 ℃, treatment time 1min; Activated solution is chromium+oxalic acid 92g/L, and service temperature is a room temperature, and the treatment time is 30s; Acidwash solution is nitric acid 90ml/L and chromic acid 90g/L, and the solution-operated temperature is a room temperature, and the treatment time is 90-150s; Reactivate solution is chromium+oxalic acid 92g/L, and service temperature is a room temperature, and the treatment time is 5-10s; Zinc dipping solution is zinc oxide 20-30g/L, hydroxy ethylidene-diphosphate 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 Passivation Treatment, it is main salt that nickel plating solution adopts basic nickel carbonate, and inferior sodium phosphate is a reductive agent, agent, and lactic acid is complexing agent, and hydrofluoric acid is inhibiter, and Cadmium Sulphate and Potassium Iodate are brightening agent, make Passivation Treatment at last.
Nickel plating solution consists of basic nickel carbonate 12-18g/L, inferior sodium phosphate 25-35g/L, and hydrofluoric acid 40-50ml/L, lactic acid are 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.
Passivating dip is chromic anhydride 50g/L, and operating temperature is 82-86 ℃, processing time 5min.
At oil removing, activation, pickling, reactivate, soak between zinc and each step of chemical nickel plating and all carry out flushing with clean water, the washing time is 30s.
The present invention compared with prior art; Have the following advantages: 1. adopt current pretreatment approaches and plating bath that the Mg-Gd-Y-Zr magnesiumalloy is carried out chemical nickel plating; Be prone to part and fail to plate, even phenomenons such as decortication, bubbling, cause coating performance not good; Bonding force is not strong, can not play the effect of protection.And the present invention carries out big improvement according to the own characteristic of Mg-Gd-Y-Zr magnesiumalloy on pretreatment process, creates the chemical nickel plating method that a cover is suitable for the Mg-Gd-Y-Zr magnesiumalloy first; Existing chemical nickel plating method, the continuous plating 2h of ability does not peel, bubbling, and can all go up plating, and plating is soon fast, and corrosion resistance of coating is good, and is strong with basal body binding force; 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 composition is simple, be easy to control, process stabilizing; 4, the zinc-impregnating layer that obtains of zinc dipping solution of the present invention is even and bonding force is good.
Description of drawings
Fig. 1 is a Mg-Gd-Y-Zr chemical nickel plating process on magnesium alloy schema provided by the invention;
Fig. 2 is the surface topography of Mg-Gd-Y-Zr magnesiumalloy behind chemical nickel plating;
Fig. 3 is Mg-Gd-Y-Zr magnesium alloy substrate and nickeling layer polarization curve comparison diagram.
Embodiment
Be described further for the present invention below in conjunction with instance, and can not limit the present invention.
Embodiment
Below in conjunction with the flow process among Fig. 1 Mg-Gd-Y-Zr magnesium-alloy chemical nickel coating method of the present invention is described.
Experiment material is the Mg-Gd-Y-Zr magnesiumalloy, and this alloying constituent is (wt.%): Gd:8-13%, Y:2-6%, and Zr:0.3-0.8%, all the other are Mg and the impurity element that can not remove.Timeliness again after extruding, thermal treatment process is 220 ℃/2h.Size of sample is the square appearance of 18mm * 10mm * 3mm, and it is handled by following operation steps:
Step 1: with magnesiumalloy through 180#, 360#, 1000#, 1500# sand paper water mill is until surface clean, there is not obvious impurity.
Step 2: the magnesiumalloy after will polishing immerses to remove in the oil solution and carries out oil removing.
The prescription that removes oil solution is following: yellow soda ash 30g/L, sodium phosphate 30g/L and OP-102ml/L.Service temperature is 75 ℃, and the time is 1min.
Step 3: with flushing with clean water magnesiumalloy 30s, flush away surface remove oil solution.
Step 4: magnesiumalloy is immersed activated solution.
The activated solution prescription is following: chromium+oxalic acid 92g/L.Service temperature is a room temperature, and the treatment time is 30s.
Step 5: with flushing with clean water magnesiumalloy 30s, the activation solution on flush away surface.
Step 6: magnesiumalloy is immersed Acidwash solution.
The Acidwash solution prescription is following: nitric acid 90ml/L and chromic acid 90g/L.Service temperature is a room temperature, and the treatment time is 90s.
Step 7: with flushing with clean water magnesiumalloy 30s, the pickle solution on flush away surface.
Step 8: magnesiumalloy immersed carry out reactivate in the activated solution.
The activated solution prescription is following: chromium+oxalic acid 92g/L.Service temperature is a room temperature, and the treatment time is 5s.
Step 9: with flushing with clean water magnesiumalloy 30s, flush away activation solution.
Step 10: magnesiumalloy immersed soak zinc in the zinc dipping solution and handle.
The zinc dipping solution prescription is following: zinc oxide 25g/L, hydroxy ethylidene-diphosphate 75ml/L, quadrol 15ml/L and phosphatase 79 ml/L.Service temperature is 85 ℃, and pH value is 9.5, treatment time 1min.
Step 11: with flushing with clean water magnesiumalloy 30s, flush away surface zincate solution.
Step 12: magnesiumalloy immersed carry out chemical nickel plating in the plating bath.
The chemical nickel-plating solution prescription is following: 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 are as brightening agent.Service temperature is 80-85 ℃, and pH value is 4.8, and the time is 2h.
Step 13: the plating bath with the Mg alloy surface of clear water after with nickel plating is rinsed well, and room temperature is dried.
Step 14: with carrying out Passivation Treatment in the immersion of the magnesiumalloy after the nickel plating passivating dip.
The passivating dip prescription is following: road acid anhydride 50g/L.Service temperature is 82-85 ℃, and the time is 5min.
Step 15: with clear water the passivating dip of Mg alloy surface is rinsed well, room temperature is dried.
Adopt its nickeling layer of Mg-Gd-Y-Zr magnesiumalloy nickel plating part that above-mentioned technology obtains through test, performance is shown in subordinate list:
Subordinate list: the chemical Ni-plating layer performance that adopts the inventive method to obtain
Fig. 2 is the coating morphology behind the Mg-Gd-Y-Zr chemically coating nickel by magnesium-alloy, can find out that from figure coating is evenly tiny born of the same parents' shape thing, densification, no significant defect.Fig. 3 is Mg-Gd-Y-Zr magnesium alloy substrate and nickeling layer polarization curve comparison diagram; From figure, can know; The matrix corrosion potential is about-1.325V, and the nickeling layer corrosion potential is about-0.251V, and hence one can see that nickeling layer is significantly improved than the erosion resistance of matrix; Current potential is shuffled, and current density has reduced an one magnitude.
Claims (5)
1. a Mg-Gd-Y-Zr 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 oil removing, activation, pickling, reactivate and soaks zinc; Removing oil solution is yellow soda ash 30g/L, sodium phosphate 30g/L and OP-101-2ml/L, and the solution-operated temperature is 60-80 ℃, treatment time lmin; Activated solution is chromium+oxalic acid 92g/L, and service temperature is a room temperature, and the treatment time is 30s; Acidwash solution is nitric acid 90ml/L and chromic acid 90g/L, and the solution-operated temperature is a room temperature, and the treatment time is 90-150s; Reactivate solution is chromium+oxalic acid 92g/L, and service temperature is a room temperature, and the treatment time is 5-10s; Zinc dipping solution is zinc oxide 20-30g/L, hydroxy ethylidene-diphosphate 70-80ml/L, 7 diamines 12-18ml/L and phosphoric acid 8-10ml/L; Service temperature is 82-86 ℃, and the pH value is 9.2-9.6, treatment time 1min;
B, carry out chemical nickel plating and Passivation Treatment, 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, make Passivation Treatment at last.
2. Mg-Gd-Y-Zr 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 is 28-35ml/L, brightening agent 3.5-5ml/L, the service temperature 82-86 of nickel plating solution ℃; The pH value is 4.5-5.0, treatment time 2h.
3. Mg-Gd-Y-Zr 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. Mg-Gd-Y-Zr magnesium-alloy chemical nickel coating method according to claim 1 is characterized in that: passivating dip consists of chromic anhydride 50g/L, and service temperature is 82-86 ℃, treatment time 5min.
5. Mg-Gd-Y-Zr magnesium-alloy chemical nickel coating method according to claim 1 is characterized in that: at oil removing, activation, pickling, reactivate, soak between zinc and each step of chemical nickel plating and all carry out flushing with clean water, the washing time is 30s.
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| CN102517570A (en) * | 2011-12-28 | 2012-06-27 | 南京工程学院 | Environment-friendly magnesium and magnesium alloy chemical nickel phosphor plating process |
| CN106048568B (en) * | 2016-08-21 | 2018-07-24 | 贵州大学 | The method of environmentally friendly chemical nickel plating |
| CN109852365A (en) * | 2018-12-17 | 2019-06-07 | 中国石油天然气股份有限公司 | Prepare method, the guanidine gum fracturing fluid by this method preparation and its application of guanidine gum fracturing fluid |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB830597A (en) * | 1957-06-06 | 1960-03-16 | Dow Chemical Co | Nickel plating by chemical means |
| CN1434149A (en) * | 2002-01-23 | 2003-08-06 | 中国科学院金属研究所 | Method for preparing corrosion-resisting wearing-resisting coat used for magnesium and alloy thereof |
| 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 |
| CN1641075A (en) * | 2004-01-18 | 2005-07-20 | 香港生产力促进局 | Magnesium and Mg alloy surface activating method and surface palting method |
| CN101717926A (en) * | 2009-12-28 | 2010-06-02 | 中南大学 | Chemical nickel-plating method for ZM6 magnesium alloy |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB830597A (en) * | 1957-06-06 | 1960-03-16 | Dow Chemical Co | Nickel plating by chemical means |
| CN1434149A (en) * | 2002-01-23 | 2003-08-06 | 中国科学院金属研究所 | Method for preparing corrosion-resisting wearing-resisting coat used for magnesium and alloy thereof |
| CN1641075A (en) * | 2004-01-18 | 2005-07-20 | 香港生产力促进局 | Magnesium and Mg alloy surface activating method and surface palting method |
| 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 |
| CN101717926A (en) * | 2009-12-28 | 2010-06-02 | 中南大学 | Chemical nickel-plating method for ZM6 magnesium alloy |
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