CN103014680A - Surface chemical nickel-plating no-palladium activation method of magnesium alloy micro-arc oxidation ceramic layer and application - Google Patents
Surface chemical nickel-plating no-palladium activation method of magnesium alloy micro-arc oxidation ceramic layer and application Download PDFInfo
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Abstract
The invention discloses a surface chemical nickel-plating no-palladium activation method of a magnesium alloy micro-arc oxidation ceramic layer and application, belonging to the technical field of magnesium alloy surface treatment. The method comprises a step of pre-nickel plating and a step of no-palladium activation, wherein the pre-nickel plating step adopts an alcoholic solution of nickel acetate, the concentration of nickel salt is 1-10g/L, and the pre-nickel plating time is 10-30 seconds; and the no-palladium activation step adopts an alcoholic solution of sodium borohydride or potassium borohydride, the concentration of the boron salt is 1-10g/L, and the activation time is 1-10 minutes. A magnesium alloy micro-arc oxidation ceramic layer sample is activated by the method disclosed by the invention and then subjected to chemical nickel plating, and a metal nickel layer with good uniformity and high bonding strength can be formed on the surface of the ceramic layer. According to the invention, the raw materials are widely available, and the cost is low; the technological process is performed at room temperature, and the solution is low-toxic and environment-friendly; and the activation liquid system is near neutral, thus damage to the workpiece surface is reduced in the activation process, and the requirements of practical engineering application can be met.
Description
Technical field
The invention belongs to technical field of magnesium alloy surface treatment, be specifically related to a kind of magnesium alloy micro-arc oxidization ceramic coating chemical nickel plating on surface palladium-free activation process and application.
Background technology
Magnesium alloy light weight, antivibration and to fall low noise ability very high, the vital role of magnesium alloy in automobile loss of weight, improved performance, environmental protection, save energy more and more is subject to people's attention in recent years.Yet the thermodynamic stability of magnesium is poor, and oxide compound (film) short texture, causes the corrosion resistance of magnesium alloy relatively poor.In addition, the chemically reactive of magnesium is high, to be coated with/integrity of coating, anti-physical abuse Capability Requirement are higher, existing being coated with/coating technology is difficult to satisfy actual needs.
At present, differential arc oxidation is the most promising technique means of realizing this goal.It is a kind of technology at metallic surface growth in situ pottery oxide film, has the advantages such as simple, the easy to operate or oxide film bonding force of technique, solidity to corrosion, hardness be better.Yet magnesium alloy micro-arc oxidization ceramic coating is a kind of loose microvoid structure, causes its barrier propterty limited.
At the Mg alloy surface direct electroless nickel, not only can carry out " sealing of hole " to arc differential oxide ceramic layer, also can play ornamental effect to Mg alloy surface simultaneously.But because there is larger difference with general ceramic layer in magnesium alloy micro-arc oxidization ceramic coating at structure and composition, therefore, it is particularly important that the pre-treatment of arc differential oxide ceramic layer chemical nickel plating and activating process just seem.
Current, mainly contain precious metal system and base metal system for the activating process of magnesium alloy micro-arc oxidization ceramic coating chemical nickel plating on surface.For example patent ZL 00103011.6 and 200510031184 mainly discloses the activating process of palladium and silver salt, although can obtain the chemical Ni-plating layer of better performances, palladium metal and silver are expensive, if the magnesium alloy sample area is larger, its cost can increase greatly; Patent 200910232926 mainly discloses a kind of without the acidic activated technique of palladium, and its mineral acid composition concentration is 3~10% phosphoric acid or nitric acid, and the magnesium alloy differential arc oxidation workpiece surface is had slight etching and damage, and range of application can be restricted.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, a kind of magnesium alloy micro-arc oxidization ceramic coating chemical nickel plating on surface palladium-free activation process and application are provided, the method has reduced the cost of magnesium alloy micro-arc oxidization ceramic coating chemical nickel plating on surface, reduces reactivation process to the damage of workpiece surface.
Technical solution of the present invention is as follows:
A kind of magnesium alloy micro-arc oxidization ceramic coating chemical nickel plating on surface palladium-free activation process may further comprise the steps:
(1) nickel preplating: the magnesium alloy sample that the surface has been prepared arc differential oxide ceramic layer is put into pre-nickel plating solution, uses deionized water wash after taking out; Described pre-nickel plating solution is the alcoholic solution of nickelous acetate, and nickel salt concentration 1~10g/L, solvent are methyl alcohol or ethanol;
(2) activation: the magnesium alloy sample behind the nickel preplating in the step (1) is put into activated solution, use deionized water wash after taking out, be immersed in again in the chemical nickel-plating liquid; Described activated solution is the alcoholic solution of boron salt, the concentration 1~10g/L of boron salt; Solvent is methyl alcohol or ethanol; Described boron salt is sodium borohydride or POTASSIUM BOROHYDRIDE.
10~30 seconds nickel preplating time, soak time 1~10 minute.
Described nickel preplating and reactivation process are carried out at ambient temperature.
Aforesaid method is applicable to AZ, ZM, MB is the magnesium alloy micro-arc oxidization ceramic coating of matrix: such as AZ91D, AZ31B, ZM5, ZM6, MB5 etc.
Aforesaid method is applicable to single nickel salt and basic nickel carbonate is the chemically coating nickel by magnesium-alloy liquid of main salt.
Advantage of the present invention and beneficial effect are as follows:
1, raw material sources of the present invention are extensive, and are with low cost; The solution low toxic and environment-friendly; Activation solution system partial neutral reduces reactivation process to the damage of workpiece surface.
2, adopt the present invention even at the nickel layer that the arc differential oxide ceramic layer surface forms, bonding strength large (between 18~24MPa).
3, the present invention is based on the Practical Project application, and its technological process can be carried out at ambient temperature, is the activating process of the stronger magnesium alloy micro-arc oxidization ceramic coating chemical nickel plating on surface of a kind of operability.
Description of drawings
Fig. 1 is the section S EM pattern after magnesium alloy micro-arc oxidization ceramic coating of the present invention surface forms nickel layer.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described further.
Embodiment 1
1, the configuration of nickel preplating and activation solution.Be configured to respectively ethanolic soln with nickelous acetate, sodium borohydride, wherein the concentration of nickelous acetate is 2g/L, and the concentration of sodium borohydride is 8g/L.
2, the configuration of magnesium alloy chemical nickel plating solution.Take by weighing medicine by following prescription: single nickel salt 25g, inferior sodium phosphate 20g, Trisodium Citrate 20g, boric acid 20g, lactic acid 15ml, thiocarbamide trace.Above-mentioned medicine is used respectively a small amount of dissolved in distilled water, and then mixed diluting is regulated the pH value to 7.0-8.0 to 1L with ammoniacal liquor.
3, will adopt AZ31B is that the magnesium alloy differential arc oxidation ceramic sample of matrix was immersed in first in the ethanolic soln of nickelous acetate nickel preplating 15 seconds, taking-up is cleaned with deionized water, immerse again in the ethanolic soln of sodium borohydride after the activation 4 minutes, take out with deionized water and clean.The plating bath that places step 2 to dispose on sample at last.The processing parameter of chemical nickel plating is: temperature normal temperature, and the time is 70 minutes, the chemical plating thickness of acquisition is 10~20 μ m.Nickel layer surface uniform (Fig. 1), good with basal body binding force, its bonding force is between 20~22MPa.
1, the configuration of nickel preplating and activation solution.Be configured to respectively methanol solution with nickelous acetate, POTASSIUM BOROHYDRIDE, wherein the concentration of nickelous acetate is 6g/L, and the concentration of POTASSIUM BOROHYDRIDE is 7g/L.
2, the configuration of magnesium alloy chemical nickel plating solution.Take by weighing medicine by following prescription: single nickel salt 20g, inferior sodium phosphate 25g, citric acid 15g, Succinic Acid 20g, lactic acid 10ml, ammonium molybdate trace.Above-mentioned medicine is used respectively a small amount of dissolved in distilled water, and then mixed diluting is regulated the pH value to 5.5-6.5 to 1L with ammoniacal liquor.
3, will adopt AZ91D is that the magnesium alloy differential arc oxidation ceramic sample of matrix was immersed in first in the methanol solution of nickelous acetate nickel preplating 20 seconds, taking-up is cleaned with deionized water, immerse again in the methanol solution of POTASSIUM BOROHYDRIDE after the activation 6 minutes, take out with deionized water and clean.The plating bath that places step 2 to dispose on sample at last.The processing parameter of chemical nickel plating is: temperature normal temperature, and the time is 50 minutes, the chemical plating thickness of acquisition is 10~20 μ m.Nickel layer surface uniform (Fig. 1), good with basal body binding force, its bonding force is between 19~24MPa.
Embodiment 3
1, the configuration of nickel preplating and activation solution.Be configured to respectively methanol solution with nickelous acetate, POTASSIUM BOROHYDRIDE, wherein the concentration of nickelous acetate is 2g/L, and the concentration of POTASSIUM BOROHYDRIDE is 4g/L.
2, the configuration of magnesium alloy chemical nickel plating solution.Take by weighing medicine by following prescription: basic nickel carbonate 10g, inferior sodium phosphate 20g, ammonium bifluoride 20g, Trisodium Citrate 20g, sodium acetate 20g, thiocarbamide trace.Above-mentioned medicine is used respectively a small amount of dissolved in distilled water, and then mixed diluting is regulated the pH value to 5.8-6.2 to 1L with ammoniacal liquor.
3, will adopt MB5 is that the magnesium alloy differential arc oxidation ceramic sample of matrix was immersed in first in the methanol solution of nickelous acetate nickel preplating 20 seconds, takes out with deionized water and cleans, and immerses in the methanol solution of POTASSIUM BOROHYDRIDE after the activation 8 minutes again, takes out with deionized water and cleans.The plating bath that places step 2 to dispose on sample at last.The processing parameter of chemical nickel plating is: temperature normal temperature, and the time is 60 minutes, the chemical plating thickness of acquisition is 10~15 μ m.Nickel layer surface uniform (Fig. 1), good with basal body binding force, its bonding force is between 18~23MPa.
Claims (5)
1. magnesium alloy micro-arc oxidization ceramic coating chemical nickel plating on surface palladium-free activation process is characterized in that: may further comprise the steps:
(1) nickel preplating: the magnesium alloy sample that the surface has been prepared arc differential oxide ceramic layer is put into pre-nickel plating solution, uses deionized water wash after taking out; Described pre-nickel plating solution is the alcoholic solution of nickelous acetate, and nickel salt concentration 1~10g/L, solvent are methyl alcohol or ethanol;
(2) activation: the magnesium alloy sample behind the nickel preplating in the step (1) is put into activated solution, use deionized water wash after taking out, be immersed in again in the chemical nickel-plating liquid; Described activated solution is the alcoholic solution of boron salt, the concentration 1~10g/L of boron salt; Solvent is methyl alcohol or ethanol; Described boron salt is sodium borohydride or POTASSIUM BOROHYDRIDE.
2. method according to claim 1 is characterized in that: 10~30 seconds nickel preplating time, soak time 1~10 minute.
3. method according to claim 1, it is characterized in that: described nickel preplating and reactivation process are carried out at ambient temperature.
4. as claimed in claim 1 application of method is characterized in that: the method is applicable to AZ, ZM, MB is the magnesium alloy micro-arc oxidization ceramic coating of matrix; Being applicable to single nickel salt and basic nickel carbonate is the chemically coating nickel by magnesium-alloy liquid of main salt.
5. application according to claim 4 is characterized in that: described matrix is AZ91D, AZ31B, ZM5, ZM6 or MB5.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105803433A (en) * | 2016-04-20 | 2016-07-27 | 青岛科技大学 | Aluminum oxide ceramic surface palladium-free activating and chemical nickel-plating technology |
CN107523814A (en) * | 2013-11-21 | 2017-12-29 | 纳米及先进材料研发院有限公司 | Surface treatment method on the magnesium alloy of differential arc oxidation processing |
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CN101270474A (en) * | 2007-03-21 | 2008-09-24 | 内蒙古农业大学 | Activation technique for lumber chemical nickel plating |
CN101760733A (en) * | 2010-01-28 | 2010-06-30 | 西安理工大学 | Magnesium alloy chemical nickel-plating surface treatment method taking microarc oxidation process as pretreatment |
CN102002688A (en) * | 2010-08-24 | 2011-04-06 | 桂林理工大学 | No-palladium activate fluid formula and activation method of fabric chemical plating iron and nickel |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101270474A (en) * | 2007-03-21 | 2008-09-24 | 内蒙古农业大学 | Activation technique for lumber chemical nickel plating |
CN101760733A (en) * | 2010-01-28 | 2010-06-30 | 西安理工大学 | Magnesium alloy chemical nickel-plating surface treatment method taking microarc oxidation process as pretreatment |
CN102002688A (en) * | 2010-08-24 | 2011-04-06 | 桂林理工大学 | No-palladium activate fluid formula and activation method of fabric chemical plating iron and nickel |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107523814A (en) * | 2013-11-21 | 2017-12-29 | 纳米及先进材料研发院有限公司 | Surface treatment method on the magnesium alloy of differential arc oxidation processing |
CN105803433A (en) * | 2016-04-20 | 2016-07-27 | 青岛科技大学 | Aluminum oxide ceramic surface palladium-free activating and chemical nickel-plating technology |
CN105803433B (en) * | 2016-04-20 | 2019-07-30 | 青岛科技大学 | A kind of alumina ceramic face no-palladium activating nickel chemical plating technology |
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