CN1641075B - Magnesium and Mg alloy surface activating method and surface plating method - Google Patents
Magnesium and Mg alloy surface activating method and surface plating method Download PDFInfo
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- CN1641075B CN1641075B CN 200410000431 CN200410000431A CN1641075B CN 1641075 B CN1641075 B CN 1641075B CN 200410000431 CN200410000431 CN 200410000431 CN 200410000431 A CN200410000431 A CN 200410000431A CN 1641075 B CN1641075 B CN 1641075B
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Abstract
The present invention discloses the magnesium and magnesium alloy surface activating process. The surface activating process includes eliminating surface oxide film and deactivating alkaline carbonate film with strong alkali solution containing fluoride, eliminating segregated intermetallic compound with soaking acid solution, creating active protecting film inside activating liquid, and strengthening the protecting film inside the strengthening liquid. The magnesium or magnesium alloy workpiece with the protecting film may be set inside zinc coating solution containing activating agent to coat zinc before plating with copper cyanide, or may be nickel plating directly through chemical plating process.
Description
Technical field
The present invention relates to a kind of be suitable for bright plating with and the surface activating process of the magnesium used of chemical nickel plating and magnesium alloy and this is carried out the method that magnesium, magnesium alloy after the surface activation process carries out light plating or chemical nickel plating.
Background technology
Because the chemically reactive of MAGNESIUM METAL is higher, in air, easily generate oxide film and subcarbonate passive film, thereby cause its electroplate and the electroless plating process in metal plating not strong with the sticking power of magnesium, magnesium alloy substrate, do not reach and electroplate and the processing requirement of electroless plating.So must eliminate passive film before plating and electroless plating, and be replaced by the activation film, the active state that just can guarantee magnesium, Mg alloy surface like this is to obtain good electrolytic coating and the chemical plating of sticking power.
At present, on the magnesium material, impose and electroplate or the direct chemical plating, do not have cover method fully reliably in the world.The U.S. material calibrating ASTM B480-68 of association has advised a kind of electro-plating method at magnesium and alloy surface thereof, U.S. Dow Chemicals, move into Norsk Hydro and Britain W.Canning Materials company and all disclose its unique method (The Dow Process separately, The Norsk Hydro Process, Euro Pat 030 305 ﹠amp; The WCM Process).Aforesaid method but all exists activation not enough, or the activation film suitably do not consolidated, and causes coating adhesion bad and etch is excessive, causes coating surface coarse, does not reach problems such as bright plating purpose.
Summary of the invention
The object of the present invention is to provide the magnesium that but a kind of bright plating is used and chemical nickel plating is used, the method that magnesium alloy surface activation is handled.
Another object of the present invention is to provide a kind of method of magnesium, magnesium alloy being carried out bright plating.
A further object of the present invention is to provide a kind of method of magnesium, magnesium alloy being carried out chemical nickel plating.
The surface activating process of magnesium, magnesium alloy among the present invention comprises the following steps: oxide film and the subcarbonate passive film of elder generation with the aqueous alkali removal workpiece surface of fluoride; Remove the segregation intermetallic compound with pickling bath liquor again; Workpiece is put into activation solution, activated carbon is come out, and generate the living condition protection film, however after put into neutralization and consolidate the liquid protective membrane and consolidate.
Magnesium, magnesium alloy carry out the method for bright plating among the present invention, comprise the following step: oxide film and the subcarbonate passive film of removing workpiece surface earlier with the aqueous alkali of fluoride; Remove the segregation intermetallic compound with pickling bath liquor again; Then workpiece is put into activation solution; putting into neutralization behind the living condition protection film to be generated consolidates liquid and consolidates protective membrane; then described magnesium, the magnesium alloy workpiece of consolidating after protective membrane is handled taken out with soaking the zinc pre-treatment behind the deionized water rinsing, put into the cupric cyanide plating bath at last and carry out preplating.
Magnesium, magnesium alloy carry out the method for chemical nickel plating among the present invention, comprise the following step: oxide film and the subcarbonate passive film of removing workpiece surface earlier with the aqueous alkali of fluoride; Remove the segregation intermetallic compound with pickling bath liquor again; Then workpiece is put into activation solution, putting into neutralization behind the living condition protection film to be generated and consolidating liquid and consolidate protective membrane, then described work is consolidated magnesium, magnesium alloy workpiece after protective membrane is handled and taken out with directly carrying out chemical nickel plating behind the deionized water and handle.
In the surface activating process of magnesium of the present invention, magnesium alloy because common magnesium, thicker oxide film and the subcarbonate passive film in magnesium alloy metallic surface can remove passive film with electrochemical reduction method, and in containing the strong alkali solution of Sodium Fluoride, make magnesium, Mg alloy surface by highdensity cathodic current, produce intensive cathodic polarization and very high cathodic polarization potential, after treating certain hour, because the acting in conjunction of the electrochemical reduction of negative electrode and the atomic hydrogen of cathodic reaction is eliminated the passive film of magnesium, Mg alloy surface.
Owing to still have segregation intermetallic compound, for example Mg on the surface of magnesium, magnesium alloy after removing passive film
17Al
12Remove these magnalium segregation intermetallic compounds so need to use special pickling bath liquor, after treating that the passive film of compact structure and intermetallic compound are eliminated, aerial magnesium, Mg alloy surface still can very fast formation oxide films, but compare with the aerial workpiece of long-term exposure, thinner thickness, structure be not fine and close, be dissolved in the acidic activated liquid easily, and activated carbon is come out.Meanwhile, the hydrogen ion in the activation solution obtains electronics and forms labile atom hydrogen, and is adsorbed on magnesium, Mg alloy surface, and wherein a part forms grey magnesium hydride film with activated carbon.The magnesium hydride film obtains consolidating under specified conditions in the liquid are consolidated in neutralization, stops that magnesium metal and alloy thereof further corrode.Simultaneously, this unimolecular layer can be used as the blocking layer, keeps the chemically reactive of activation film in air.
So, can soak the zinc pre-treatment to this magnesium, magnesium alloy with activation film, and after soaking zinc, carry out cupric cyanide preplating or protective membrane consolidated after directly carry out chemical nickel plating.
In addition, remove the operation of workpiece surface oxide film and subcarbonate passive film in the method for the present invention, can be undertaken by method well known in the prior art, for example, magnesium or magnesium alloy sample workpiece surface be treated to put into the fluorochemical MF that contains weight ratio 10% and 10% MOH strong alkali aqueous solution behind the glossy surface, its pH=13 makes magnesium, Mg alloy surface by highdensity cathodic current 2 ± 1A/dm
2, the cathodic polarization time is 10 minutes, with the oil stain of eliminating workpiece surface, spot with owing to be exposed to oxide film and the subcarbonate passive film that airborne magnesium, Mg alloy surface generate.
Embodiment
Embodiment 1:
Bright plating is used and bright chemical nickel plating is used among the present invention magnesium, magnesium alloy surface activation treatment process follow these steps to handle:
1) die casting magnesium, magnesium alloy work-piece surface are treated to put into that to contain weight ratio be 10% Sodium Fluoride and 10% aqueous sodium hydroxide solution behind the glossy surface earlier, pass through 2A/dm
2After the cathodic current electrolysis 10 minutes, remove the oxide film and the subcarbonate passive film of workpiece surface;
2) take out in the aqueous solution with the chromic acid that immerses weight percent 12% behind the deionized water rinsing, 5% saltpetre, 10% nitric acid and carry out dip treating, to remove the segregation intermetallic compound, as Mg
17Al
12, this steeping fluid is prepared with deionized water, and the temperature of dipping is 30 ℃, and dipping time is 3 minutes;
3) take out with immersing behind the deionized water rinsing in the aqueous solution that weight percent is 10% ammonium bifluoride, 5% phosphoric acid and carry out activation treatment, generate the activates relay film, this activation treatment liquid is prepared with deionized water, and wherein the temperature of activation treatment is 30 ℃, 5 minutes time;
4) take out with consolidating in the aqueous solution that immerses weight percent 20% trisodium phosphate, 5% Sodium Fluoride behind the deionized water rinsing, promptly consolidate the activates relay film, this is consolidated liquid and prepares with deionized water, and wherein the temperature of Gong Guing is 60 ℃, and the time is 10 minutes.
To carry out workpiece after the surface activation process and take out trisodium phosphate with the zinc sulfate of putting into weight percent 10% behind the deionized water rinsing and 20%, Sodium Fluoride with 5% (weight), with soak the zinc pre-treatment in the yellow soda ash of 5% (weight), this soaks the zinc pretreatment liquid and adopts the deionized water preparation, the temperature of soaking the zinc pre-treatment is 70 ℃, time is 10 minutes, taking out workpiece then puts into the cupric cyanide plating bath again after with deionized water rinsing and carries out preplating, the pre-plating bath of the cupric cyanide that is adopted is CuCN 20-70g/l, NaCN 30-100g/l, KNaC
4H
4O
630-50g/l, temperature is 50 ℃, and pH is 10.5-12, and current density first minute was 4A/dm
2, reduce to 2A/dm then
2, electroplating time is 12 minutes.
In the present embodiment because the existence of activates relay film and suitably being consolidated, thereby the electroplated metal layer that can guarantee strong adhesion and then can be used as the media layer of further electroplated metal layer more than its surface growth to 1 micron.
Embodiment 2:
Bright plating is used and bright chemical nickel plating is used among the present invention magnesium, magnesium alloy surface activation treatment process follow these steps to handle:
1) die casting magnesium, magnesium alloy work-piece surface are treated to put into the Sodium Fluoride that contains weight ratio 10% and 10% potassium hydroxide sodium water solution behind the glossy surface earlier, pass through 1A/dm
2Cathodic current electrolysis 10 minutes;
2) take out with carrying out dip treating in the immersion weight percent 2% oxalic acid liquid behind the deionized water rinsing, this steeping fluid is prepared with deionized water, 25 ℃ of the temperature of dipping, 2 minutes time;
3) take out with behind the deionized water rinsing according among the embodiment 1 the 3rd) step and subsequent step carry out.
In the present embodiment because the existence of activates relay film and suitably being consolidated, thereby the electroplated metal layer that can guarantee strong adhesion and then can be used as the media layer of further electroplated metal layer more than its surface growth to 1 micron.
Embodiment 3:
Bright plating is used and bright chemical nickel plating is used among the present invention magnesium, magnesium alloy surface activation treatment process follow these steps to handle:
1) die casting magnesium, magnesium alloy work-piece surface are treated to put into the Sodium Fluoride that contains weight ratio 10% and 10% aqueous sodium hydroxide solution behind the glossy surface earlier, pass through 2A/dm
2Cathodic current electrolysis 10 minutes;
2) take out with immersing weight percent 1.5% oxalic acid behind the deionized water rinsing, with carry out dip treating in 200ppm oxyethyl group butynediol (wetting agent) aqueous solution, this steeping fluid is prepared with deionized water, and strict control chlorine ion concentration can not be greater than 2ppm, 25 ℃ of temperature, dipping time 1 minute;
3) take out with handling according to the 3rd step and subsequent step among the embodiment 1 behind the deionized water rinsing.
In the present embodiment because the existence of activates relay film and suitably being consolidated, thereby the electroplated metal layer that can guarantee strong adhesion and then can be used as the media layer of further electroplated metal layer more than its surface growth to 1 micron.
Embodiment 4:
Bright plating is used and bright chemical nickel plating is used among the present invention magnesium, magnesium alloy surface activation treatment process follow these steps to handle:
1) die casting magnesium, magnesium alloy work-piece surface are treated to put into the Sodium Fluoride that contains weight ratio 10% and 10% aqueous sodium hydroxide solution behind the glossy surface earlier, the aqueous solution is prepared with deionized water, and chlorine ion concentration can not pass through 1A/dm greater than 2ppm
2Cathodic current electrolysis 10 minutes;
2) take out with carrying out dip treating in the aqueous solution that immerses weight percent 12% chromic acid, 5% saltpetre, 10% nitric acid behind the deionized water rinsing, this steeping fluid is prepared with deionized water, 25 ℃ of temperature, dipping time 2 minutes;
3) take out with activating in the aqueous solution that immerses weight percent 10% ammonium bifluoride, 5% phosphoric acid behind the deionized water rinsing, this activation solution is prepared with deionized water, 25 ℃ of temperature, soak time 3 minutes;
4) take out with consolidating processing in the aqueous solution that immerses weight percent 20% trisodium phosphate, 5% Sodium Fluoride behind the deionized water rinsing, this is consolidated liquid and prepares with deionized water, and 80 ℃ of temperature are consolidated 10 minutes time.
The workpiece that will carry out after the surface activation process takes out with directly carrying out chemical nickel plating behind the deionized water rinsing, and the plating bath of this chemical nickel plating can adopt in the prior art by the public known prescription or other special close prescription, for example: 2NiCO
333Ni (OH)
24H
2O 10g/l, HF (48%) 9ml/l, C
6H
8O
75g/l, NH
4HF
210g/l, NH
4OH (30%) 31ml/l, 80 ℃ of temperature, pH 4.5, deposition 20-25 μ m/hr.
In the present embodiment, because the existence of activates relay film and suitably being consolidated, thereby the chemical plating metal layer that can guarantee strong adhesion and then can be used as the media layer of further electroplated metal layer more than its surface growth to 1 micron.
Embodiment 5:
Bright plating is used and bright chemical nickel plating is used among the present invention magnesium, magnesium alloy surface activation treatment process follow these steps to handle:
1) die casting magnesium, magnesium alloy work-piece surface are treated to put into the Sodium Fluoride that contains weight ratio 10% and 10% potassium hydroxide sodium water solution behind the glossy surface earlier, pass through 1A/dm
2Cathodic current electrolysis 10 minutes;
2) take out with carrying out dip treating in the immersion weight percent 2% oxalic acid liquid behind the deionized water rinsing, this steeping fluid is prepared with deionized water, and temperature is 25 ℃, dipping time 2 minutes;
3) take out with behind the deionized water rinsing according among the embodiment 4 the 3rd) step and subsequent step handle.
In the present embodiment because the existence of activates relay film and suitably being consolidated, thereby the chemical plating metal layer that can guarantee strong adhesion and then can be used as the media layer of further electroplated metal layer more than its surface growth to 1 micron.
Embodiment 6:
Bright plating is used and bright chemical nickel plating is used among the present invention magnesium, magnesium alloy surface activation treatment process follow these steps to handle:
1) die casting magnesium, magnesium alloy work-piece surface are treated to put into the Sodium Fluoride that contains weight ratio 10% and 10% aqueous sodium hydroxide solution behind the glossy surface earlier, pass through 2A/dm
2Cathodic current electrolysis 10 minutes;
2) take out with immersing weight percent 1.5% oxalic acid behind the deionized water rinsing, with carry out dip treating in 200ppm oxyethyl group butynediol (wetting agent) aqueous solution, this steeping fluid is prepared with deionized water, and strict control chlorine ion concentration can not be greater than 2ppm, 25 ℃ of temperature, dipping time 1 minute;
3) take out with behind the deionized water rinsing according among the embodiment 4 the 3rd) step and subsequent step handle.
In the present embodiment because the existence of activation film and suitably being consolidated, thereby the chemical plating metal layer that can guarantee strong adhesion and then can be used as the media layer of further electroplated metal layer more than its surface growth to 1 micron.
Claims (8)
1. the surface activating process of a magnesium, magnesium alloy comprises the following steps: to remove with the aqueous alkali of fluoride earlier the oxide film and the subcarbonate passive film of workpiece surface; Remove the segregation intermetallic compound with pickling bath liquor again; Then workpiece is put into activation solution, putting into neutralization behind the living condition protection film to be generated and consolidating liquid and consolidate protective membrane; Wherein:
The aqueous alkali of described fluoride is: the aqueous solution of the Sodium Fluoride of weight ratio 10% and 10% sodium hydroxide;
Consisting of of described pickling bath liquor: the aqueous solution of the chromic acid of weight percent 12%, 5% saltpetre and 10% nitric acid, the perhaps oxalic acid of weight percent 2%, the perhaps aqueous solution of the oxalic acid of weight percent 1.5% and 200ppm oxyethyl group butynediol;
Described activation solution is: the aqueous solution of the ammonium bifluoride of weight percent 10% and 5% phosphoric acid;
Liquid is consolidated in described neutralization: the aqueous solution of the trisodium phosphate of weight percent 20% and 5% Sodium Fluoride;
The step that described aqueous alkali with fluoride is removed workpiece surface oxide film and subcarbonate passive film is that the aqueous solution that magnesium or magnesium alloy work-piece surface are treated to the sodium hydroxide of putting into the Sodium Fluoride that contains weight ratio 10% and 10% behind the glossy surface is carried out catholyte.
2. according to the surface activating process of the magnesium described in the claim 1, magnesium alloy, it is characterized in that: described pickling bath liquor adopts the deionized water preparation, and wherein the temperature of acid dipping is 20-50 ℃, and the time is 0.1-30 minute.
3. according to the surface activating process of the magnesium described in the claim 1, magnesium alloy, it is characterized in that: described activation solution adopts the deionized water preparation, and wherein the temperature of activation treatment is 20-50 ℃, and the time is 0.1-30 minute.
4. according to the surface activating process of the magnesium described in the claim 1, magnesium alloy, it is characterized in that: described neutralization is consolidated liquid and is adopted the deionized water preparation, and wherein the temperature of neutralization consolidation is 20-90 ℃, and the time is 0.1-30 minute.
5. the surperficial electroplating method of a magnesium, magnesium alloy comprises the following step: oxide film and the subcarbonate passive film of removing workpiece surface earlier with the aqueous alkali of fluoride; Remove the segregation intermetallic compound with pickling bath liquor again; Then workpiece is put into activation solution, putting into neutralization behind the living condition protection film to be generated consolidates liquid and consolidates protective membrane, then described magnesium, the magnesium alloy workpiece of consolidating after protective membrane is handled taken out with soaking the zinc pre-treatment behind the deionized water rinsing, put into the cupric cyanide plating bath at last and carry out preplating; Wherein:
The aqueous alkali of described fluoride is: the aqueous solution of the Sodium Fluoride of weight ratio 10% and 10% sodium hydroxide;
Consisting of of described pickling bath liquor: the aqueous solution of the chromic acid of weight percent 12%, 5% saltpetre and 10% nitric acid, the perhaps oxalic acid of weight percent 2%, the perhaps aqueous solution of the oxalic acid of weight percent 1.5% and 200ppm oxyethyl group butynediol;
Described activation solution is: the aqueous solution of the ammonium bifluoride of weight percent 10% and 5% phosphoric acid;
Liquid is consolidated in described neutralization: the aqueous solution of the trisodium phosphate of weight percent 20% and 5% Sodium Fluoride;
The step that described aqueous alkali with fluoride is removed workpiece surface oxide film and subcarbonate passive film is that the aqueous solution that magnesium or magnesium alloy work-piece surface are treated to the sodium hydroxide of putting into the Sodium Fluoride that contains weight ratio 10% and 10% behind the glossy surface is carried out catholyte.
6. according to the surperficial electroplating method of the magnesium described in the claim 5, magnesium alloy, it is characterized in that: the described zinc treatment solution that soaks is a kind of aqueous solution of being made up of following component: the zinc sulfate of weight percent 10%, 20% trisodium phosphate, 5% Sodium Fluoride and 5% yellow soda ash; The pre-plating bath of described cupric cyanide is CuCN20-70g/l, NaCN30-100g/l, KNaC
4H
4O
630-50g/l, the temperature of preplating is 50 ℃, and the pH value is 10.5-12, and current density first minute was 4A/dm
2, reduce to 2A/dm then
2, electroplating time is 12 minutes.
7. the surperficial electroplating method of a magnesium, magnesium alloy comprises the following step: oxide film and the subcarbonate passive film of removing workpiece surface earlier with the aqueous alkali of fluoride; Remove the segregation intermetallic compound with pickling bath liquor again; Then workpiece is put into activation solution, putting into neutralization behind the living condition protection film to be generated and consolidating liquid and consolidate protective membrane, then described work is consolidated magnesium, magnesium alloy workpiece after protective membrane is handled and taken out with directly carrying out chemical nickel plating behind the deionized water rinsing and handle; Wherein:
The aqueous alkali of described fluoride is: the aqueous solution of the Sodium Fluoride of weight ratio 10% and 10% sodium hydroxide;
Consisting of of described pickling bath liquor: the aqueous solution of the chromic acid of weight percent 12%, 5% saltpetre and 10% nitric acid, the perhaps oxalic acid of weight percent 2%, the perhaps aqueous solution of the oxalic acid of weight percent 1.5% and 200ppm oxyethyl group butynediol;
Described activation solution is: the aqueous solution of the ammonium bifluoride of weight percent 10% and 5% phosphoric acid;
Liquid is consolidated in described neutralization: the aqueous solution of the trisodium phosphate of weight percent 20% and 5% Sodium Fluoride;
The step that described aqueous alkali with fluoride is removed workpiece surface oxide film and subcarbonate passive film is that the aqueous solution that magnesium or magnesium alloy work-piece surface are treated to the sodium hydroxide of putting into the Sodium Fluoride that contains weight ratio 10% and 10% behind the glossy surface is carried out catholyte.
8. according to the surperficial electroplating method of the magnesium described in the claim 7, magnesium alloy, it is characterized in that: the plating bath of described direct chemical nickel plating is 2NiCO
33Ni (OH)
24H
2O 10g/l, 48% HF 9ml/l, C
6H
8O
75g/l, NH
4HF
210g/l, 30% NH
4The mixed solution of OH 31ml/l, temperature are 80 ℃, and pH 4.5, deposition 20-25 μ m/hr.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100430520C (en) * | 2005-12-30 | 2008-11-05 | 东北大学 | Process for copper coating on surface of magnesium and 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 |
| CN103898581A (en) * | 2013-06-03 | 2014-07-02 | 无锡市锡山区鹅湖镇荡口青荡金属制品厂 | Cyanide-free electro-coppering process for electroplating nickel on surface of magnesium alloy die-cast piece |
| CN103898505B (en) * | 2013-06-04 | 2016-09-14 | 华文蔚 | A kind of Electroless Ni-P alloy plating on magnesium alloy of pre-galvanized admiro |
| CN103898588A (en) * | 2013-06-04 | 2014-07-02 | 无锡市锡山区鹅湖镇荡口青荡金属制品厂 | Magnesium alloy surface chemical nickel-plating combination solution for pre-electroplated zinc-nickel alloy |
| CN108624877A (en) * | 2018-06-15 | 2018-10-09 | 莱诺斯科技（北京）股份有限公司 | A kind of magnesium lithium alloy material surface anti-corrosive treatment method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19756845A1 (en) * | 1997-12-19 | 1999-06-24 | Alfred R Franz Fa | Pre-galvanization treatment of magnesium alloy parts |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19756845A1 (en) * | 1997-12-19 | 1999-06-24 | Alfred R Franz Fa | Pre-galvanization treatment of magnesium alloy parts |
Non-Patent Citations (2)
| Title |
|---|
| 朱祖芳.镁合金部件(制品)的表面保护和装饰工艺.材料保护35 6.2002,35(6),4-5. |
| 朱祖芳.镁合金部件(制品)的表面保护和装饰工艺.材料保护35 6.2002,35(6),4-5. * |
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