CN103938253A - Magnesium alloy anodic oxidation electrolyte and method of processing magnesium alloy with the electrolyte - Google Patents
Magnesium alloy anodic oxidation electrolyte and method of processing magnesium alloy with the electrolyte Download PDFInfo
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- CN103938253A CN103938253A CN201310023957.3A CN201310023957A CN103938253A CN 103938253 A CN103938253 A CN 103938253A CN 201310023957 A CN201310023957 A CN 201310023957A CN 103938253 A CN103938253 A CN 103938253A
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- magnesium alloy
- anodic oxidation
- oxidation electrolyte
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Abstract
A magnesium alloy anodic oxidation electrolyte and a method of processing magnesium alloy with the electrolyte are disclosed. The electrolyte comprises a silicate having a concentration of 40-120 g/L; a gluconate having a concentration of 5-40 g/L; a hydroxide having a concentration of 60-200 g/L; and additives including one or more of carboxylate, fluoride, boride and polyol. The method includes: removing an oxidation layer mechanically, dusting, degreasing and washing with pure water; under a condition of room temperature, adding a pretreated magnesium alloy into the magnesium alloy anodic oxidation electrolyte and performing anodic oxidation for 1-15 min; washing the magnesium alloy subjected to anodic oxidation with water; and drying at 100 DEG C for 3 min. The electrolyte and the method has characteristics of simple production processes, less production equipment, convenient operation, low manufacturing cost, short processing processes, no need of acid washing or activation, short processing time and easy control. Surfaces of the obtained magnesium alloy product are uniform and have ceramic quality.
Description
[technical field]
The present invention relates to a kind of magnesium alloy surface treatment, be specifically related to a kind of magnesium alloy anodic oxidation electrolyte and the method to magnesium alloy processing thereof.
[background technology]
Magnesium alloy has high specific tenacity and specific rigidity, good castability, forging property and ductility, also there is the features such as the large and good electromagnetic wave shielding of energy decrement coefficient simultaneously, be described as 21 century desirable electronic product casing and automobile component for using material.But the chemical property of magnesium is active, often form at Magnesium Air alloy surface the oxide film that one deck is very thin, rete porous and more crisp, does not have provide protection to matrix metal.Therefore, poor the becoming of solidity to corrosion restricts the principal element that magnesium alloy is made the most of the advantage, and must carry out anti-corrosive treatment to its surface.
The method kind of magnesium and alloy treatment thereof is more at present, but mainly adopts the method for anodic oxidation and chemical conversion film, and anodic oxidation is a kind of conventional surface treatment method.As far back as the 1950's, the anodizing technology of magnesium alloy is just succeeded in developing, and mainly contains HAE, Dow17, GEC and Cr-22 etc.Typical technique is HAE and Dow17, is still widely used so far.HAE is a kind of anode oxidation method of magnesium alloy most worthy in alkaline technique, and Dow17 is magnesium alloy most widely used a kind of anode oxidation method in acidic solution.Anodic oxidation of magnetism alloy liquid in these methods has used the toxic compounds containing chromium more, and the shortcoming that aforesaid method all exists is simultaneously contaminate environment, and the processing cost of waste liquid is high, so be slowly eliminated.
A kind of electrolytic solution of anodic oxidation of magnetism alloy processing and the method to Mg alloy surface processing are disclosed in patent CN101498026.The component of described magnesium alloy anodic oxidation electrolyte comprises poly aspartic acid, silicate and oxyhydroxide etc.Under the condition that is 10～13 at PH by said components, carry out anodic oxidation treatment, can generate at Mg alloy surface the zone of oxidation of smooth, even and good corrosion resistance.But requiring of this anodic oxidation treatment voltage is too high, large to equipment requirements, bring certain difficulty thereby give to apply.
In patent US5385662, disclose and a kind ofly can allow metallic substance or metal object surface produce the method for ceramic layer by anodic oxidation.This method can make Al, Mg, Ti, Ta, Zr, Nb, Hf, W, Mo, V, Bi or its alloy, is 2～8, temperature is that-30 DEG C～15 DEG C and current density are 1A/cm at pH
2condition under make ceramic protection layer.Although the method can obtain ceramic layer, the electric current of application is excessive, thereby brings certain difficulty to actual production.
[summary of the invention]
In view of this, be in fact necessary to provide a kind of magnesium alloy anodic oxidation electrolyte and the method to magnesium alloy processing thereof, in anodic oxidation, process overtension and electric current excessive, the problem that is difficult to aforesaid method to be applied with the electrolytic solution that solves aforesaid method.
In order to achieve the above object, magnesium alloy anodic oxidation electrolyte provided by the invention, it comprises following component:
Silicate 40～120g/L;
Gluconate 5～40g/L;
Oxyhydroxide 60～200g/L;
Additive, it comprises one or more in carboxylate salt, fluorochemical, boride and polyvalent alcohol.
Preferably, described silicate is water glass or potassium silicate.
Preferably, described gluconate is maltonic acid sodium or maltonic acid potassium.
Preferably, described oxyhydroxide is potassium hydroxide or sodium hydroxide.
Preferably, in described additive, the concentration of carboxylate salt is 30～100g/L, and the concentration of fluorochemical is 2～20g/L, and the concentration of boride is 5～40g/L, and the concentration of polyvalent alcohol is 5～20g/L.
Preferably, described carboxylate salt is any one in tartrate, Citrate trianion, acetate and propionic salt.
Preferably, described fluorochemical is Potassium monofluoride or Sodium Fluoride.
Preferably, described boride is any one in Sodium Tetraborate, potassium borate and sodium tetraborate.
Preferably, described polyvalent alcohol is any one in glycerine, ethylene glycol, propylene glycol, butyleneglycol, trihydroxy methyl propane and sorbyl alcohol.
The method of magnesium alloy anodic oxidation electrolyte provided by the invention to magnesium alloy processing, it comprises the steps:
(1) magnesium alloy pre-treatment: machinery is removed zone of oxidation, ash disposal skimming treatment and washing;
(2) anodic oxidation treatment: under normal temperature condition, pretreated magnesium alloy is put into described magnesium alloy anodic oxidation electrolyte Anodic Oxidation 1～15min;
(3) magnesium alloy after above-mentioned anodic oxidation treatment is washed, and dried 3min under the condition of 100 DEG C.
Compared to prior art, magnesium alloy anodic oxidation electrolyte of the present invention and the method to magnesium alloy processing thereof have the following advantages:
(1) adopt constant-voltage method, the suitability for industrialized production of being more convenient for and production management and control;
(2) production technique is simple, and production unit is few, easy to operate and tooling cost is low;
(3) treatment scheme is short, without the step such as pickling, activation;
(4) the magnesium-alloy material smooth surface that obtains, evenly, has ceramic texture concurrently;
(5) treatment time short, the easy management and control of condition.
[embodiment]
Embodiment 1:
Magnesium alloy anodic oxidation electrolyte provided by the invention, it comprises following component:
Potassium silicate 80g/L;
Sunmorl N 60S 30g/L;
Sodium hydroxide 160g/L;
Seignette salt 50g/L;
Sodium Fluoride 10g/L;
Potassium borate 15g/L.
The present invention also provides the method for a kind of magnesium alloy anodic oxidation electrolyte to magnesium alloy processing, and the method comprises the following steps:
Step 101: magnesium alloy is carried out to machinery and remove the preprocessing process such as zone of oxidation, ash disposal skimming treatment and washing;
Step 102: be under 15 DEG C, the constant voltage condition that is 75V at tank liquor, pretreated magnesium alloy is put into above-mentioned magnesium alloy anodic oxidation electrolyte Anodic Oxidation 10min;
Step 103: the magnesium alloy after above-mentioned anodic oxidation treatment is washed, and dried 3min under the condition of 100 DEG C.
In above-described embodiment, through magnesium alloy anodic oxidation electrolyte, to the method for magnesium alloy processing magnesium alloy sample appearance after treatment homogeneous, the rete of generation is white, and slightly with ceramic texture; This magnesium alloy sample good corrosion resistance is tested 72h rear surface without any corrosion under neutral salt spray.
Embodiment 2:
Magnesium alloy anodic oxidation electrolyte provided by the invention, it comprises following component:
Water glass 60g/L;
Sunmorl N 60S 10g/L;
Potassium hydroxide 180g/L;
Tripotassium Citrate 40g/L;
Potassium monofluoride 15g/L;
Glycerine 10g/L.
The present invention also provides the method for a kind of magnesium alloy anodic oxidation electrolyte to magnesium alloy processing, and the method comprises the following steps:
Step 201: magnesium alloy is carried out to machinery and remove the preprocessing process such as zone of oxidation, ash disposal skimming treatment and washing;
Step 202: be under 25 DEG C, the constant voltage condition that is 70V at tank liquor, pretreated magnesium alloy is put into above-mentioned magnesium alloy anodic oxidation electrolyte Anodic Oxidation 8min;
Step 203: the magnesium alloy after above-mentioned anodic oxidation treatment is washed, and dried 3min under the condition of 100 DEG C.
In above-described embodiment, through magnesium alloy anodic oxidation electrolyte, to the method for magnesium alloy processing magnesium alloy sample appearance after treatment homogeneous, the rete of generation is white, and slightly with ceramic texture; This magnesium alloy sample good corrosion resistance is tested 72h rear surface without any corrosion under neutral salt spray.
Embodiment 3:
Magnesium alloy anodic oxidation electrolyte provided by the invention, it comprises following component:
Potassium silicate 50g/L;
Potassium Gluconate 20g/L;
Sodium hydroxide 140g/L;
Trisodium Citrate 60g/L;
Potassium monofluoride 20g/L;
Potassium borate 20g/L.
The present invention also provides the method for a kind of magnesium alloy anodic oxidation electrolyte to magnesium alloy processing, and the method comprises the following steps:
Step 301: magnesium alloy is carried out to machinery and remove the preprocessing process such as zone of oxidation, ash disposal skimming treatment and washing;
Step 302: be under 30 DEG C, the constant voltage condition that is 80V at tank liquor, pretreated magnesium alloy is put into above-mentioned magnesium alloy anodic oxidation electrolyte Anodic Oxidation 5min;
Step 303: the magnesium alloy after above-mentioned anodic oxidation treatment is washed, and dried 3min under the condition of 100 DEG C.
In above-described embodiment, through magnesium alloy anodic oxidation electrolyte, to the method for magnesium alloy processing magnesium alloy sample appearance after treatment homogeneous, the rete of generation is white, and slightly with ceramic texture; This magnesium alloy sample good corrosion resistance is tested 72h rear surface without any corrosion under neutral salt spray.
Embodiment 4:
Magnesium alloy anodic oxidation electrolyte provided by the invention, it comprises following component:
Potassium silicate 90g/L;
Potassium Gluconate 25g/L;
Sodium hydroxide 100g/L;
Sodium acetate 60g/L;
Potassium monofluoride 8g/L;
Ethylene glycol 15g/L.
The present invention also provides the method for a kind of magnesium alloy anodic oxidation electrolyte to magnesium alloy processing, and the method comprises the following steps:
Step 401: magnesium alloy is carried out to machinery and remove the preprocessing process such as zone of oxidation, ash disposal skimming treatment and washing;
Step 402: be under 30 DEG C, the constant voltage condition that is 75V at tank liquor, pretreated magnesium alloy is put into above-mentioned magnesium alloy anodic oxidation electrolyte Anodic Oxidation 5min;
Step 403: the magnesium alloy after above-mentioned anodic oxidation treatment is washed, and dried 3min under the condition of 100 DEG C.
In above-described embodiment, through magnesium alloy anodic oxidation electrolyte, to the method for magnesium alloy processing magnesium alloy sample appearance after treatment homogeneous, the rete of generation is white, and slightly with ceramic texture; This magnesium alloy sample good corrosion resistance is tested 72h rear surface without any corrosion under neutral salt spray.
Embodiment 5:
Magnesium alloy anodic oxidation electrolyte provided by the invention, it comprises following component:
Water glass 60g/L;
Potassium Gluconate 40g/L;
Sodium hydroxide 90g/L;
Sodium Propionate 75g/L;
Potassium monofluoride 16g/L;
Glycerine 5g/L.
The present invention also provides the method for a kind of magnesium alloy anodic oxidation electrolyte to magnesium alloy processing, and the method comprises the following steps:
Step 501: magnesium alloy is carried out to machinery and remove the preprocessing process such as zone of oxidation, ash disposal skimming treatment and washing;
Step 502: be under 20 DEG C, the constant voltage condition that is 80V at tank liquor, pretreated magnesium alloy is put into above-mentioned magnesium alloy anodic oxidation electrolyte Anodic Oxidation 3min;
Step 503: the magnesium alloy after above-mentioned anodic oxidation treatment is washed, and dried 3min under the condition of 100 DEG C.
In above-described embodiment, through magnesium alloy anodic oxidation electrolyte, to the method for magnesium alloy processing magnesium alloy sample appearance after treatment homogeneous, the rete of generation is white, and slightly with ceramic texture; This magnesium alloy sample good corrosion resistance is tested 72h rear surface without any corrosion under neutral salt spray.
Embodiment 6:
Magnesium alloy anodic oxidation electrolyte provided by the invention, it comprises following component:
Water glass 100g/L;
Sunmorl N 60S 15g/L;
Sodium hydroxide 150g/L;
Seignette salt 60g/L;
Potassium monofluoride 15g/L;
Boronation sodium 10g/L.
The present invention also provides the method for a kind of magnesium alloy anodic oxidation electrolyte to magnesium alloy processing, and the method comprises the following steps:
Step 601: magnesium alloy is carried out to machinery and remove the preprocessing process such as zone of oxidation, ash disposal skimming treatment and washing;
Step 602: be under 40 DEG C, the constant voltage condition that is 75V at tank liquor, pretreated magnesium alloy is put into above-mentioned magnesium alloy anodic oxidation electrolyte Anodic Oxidation 1min;
Step 603: the magnesium alloy after above-mentioned anodic oxidation treatment is washed, and dried 3min under the condition of 100 DEG C.
In above-described embodiment, through magnesium alloy anodic oxidation electrolyte, to the method for magnesium alloy processing magnesium alloy sample appearance after treatment homogeneous, the rete of generation is white, and slightly with ceramic texture; This magnesium alloy sample good corrosion resistance is tested 72h rear surface without any corrosion under neutral salt spray.
The magnesium alloy anodic oxidation electrolyte of the present invention and method of magnesium alloy processing is had the following advantages:
(1) adopt constant-voltage method, the suitability for industrialized production of being more convenient for and production management and control;
(2) production technique is simple, and production unit is few, easy to operate and tooling cost is low;
(3) treatment scheme is short, without the step such as pickling, activation;
(4) the magnesium-alloy material smooth surface that obtains, evenly, has ceramic texture concurrently;
(5) treatment time short, the easy management and control of condition.
Claims (10)
1. a magnesium alloy anodic oxidation electrolyte, is characterized in that, this magnesium alloy anodic oxidation electrolyte comprises following component:
Silicate 40～120g/L;
Gluconate 5～40g/L;
Oxyhydroxide 60～200g/L;
Additive, it comprises one or more in carboxylate salt, fluorochemical, boride and polyvalent alcohol.
2. magnesium alloy anodic oxidation electrolyte according to claim 1, is characterized in that, described silicate is water glass or potassium silicate.
3. magnesium alloy anodic oxidation electrolyte according to claim 1, is characterized in that, described gluconate is Sunmorl N 60S or Potassium Gluconate.
4. magnesium alloy anodic oxidation electrolyte according to claim 1, is characterized in that, described oxyhydroxide is potassium hydroxide or sodium hydroxide.
5. magnesium alloy anodic oxidation electrolyte according to claim 1, it is characterized in that, in described additive, the concentration of carboxylate salt is 30～100g/L, and the concentration of fluorochemical is 2～20g/L, the concentration of boride is 5～40g/L, and the concentration of polyvalent alcohol is 5～20g/L.
6. magnesium alloy anodic oxidation electrolyte according to claim 1, is characterized in that, described carboxylate salt is any one in tartrate, Citrate trianion, acetate and propionic salt.
7. magnesium alloy anodic oxidation electrolyte according to claim 1, is characterized in that, described fluorochemical is Potassium monofluoride or Sodium Fluoride.
8. magnesium alloy anodic oxidation electrolyte according to claim 1, is characterized in that, described boride is any one in Sodium Tetraborate, potassium borate and sodium tetraborate.
9. magnesium alloy anodic oxidation electrolyte according to claim 1, is characterized in that, described polyvalent alcohol is any one in glycerine, ethylene glycol, propylene glycol, butyleneglycol, trihydroxy methyl propane and sorbyl alcohol.
10. the method for magnesium alloy anodic oxidation electrolyte to magnesium alloy processing, it is the method that adopts the processing of the magnesium alloy anodic oxidation electrolyte described in any one Mg alloy surface in claim 1 to 9, it is characterized in that, the method comprises the steps:
(1) magnesium alloy pre-treatment: machinery is removed zone of oxidation, ash disposal skimming treatment and washing;
(2) anodic oxidation treatment: under normal temperature condition, pretreated magnesium alloy is put into described magnesium alloy anodic oxidation electrolyte Anodic Oxidation 1～15min;
(3) magnesium alloy after above-mentioned anodic oxidation treatment is washed, and dried 3min under the condition of 100 DEG C.
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Cited By (5)
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| CN106480487A (en) * | 2016-09-20 | 2017-03-08 | 东南大学 | A kind of preparation method of the corrosion-resistant film layer of magnesium based metal antibacterial and mouldproof |
| WO2017166995A1 (en) * | 2016-03-31 | 2017-10-05 | 比亚迪股份有限公司 | Magnesium alloy anodizing solution and preparation method therefor, and method for anodizing magnesium alloy |
| CN108468077A (en) * | 2018-03-29 | 2018-08-31 | 山西银光华盛镁业股份有限公司 | A kind of self-enclosed anode oxidation method of magnesium alloy |
| CN109267139A (en) * | 2018-10-31 | 2019-01-25 | 日照微弧技术有限公司 | A kind of electrolyte and preparation method thereof for magnesium alloy differential arc oxidation |
| CN110129858A (en) * | 2019-06-12 | 2019-08-16 | 北京石油化工学院 | A kind of ionic liquid auxiliary magnesium lithium alloy anode oxidation film-forming method |
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Cited By (6)
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| WO2017166995A1 (en) * | 2016-03-31 | 2017-10-05 | 比亚迪股份有限公司 | Magnesium alloy anodizing solution and preparation method therefor, and method for anodizing magnesium alloy |
| CN106480487A (en) * | 2016-09-20 | 2017-03-08 | 东南大学 | A kind of preparation method of the corrosion-resistant film layer of magnesium based metal antibacterial and mouldproof |
| CN108468077A (en) * | 2018-03-29 | 2018-08-31 | 山西银光华盛镁业股份有限公司 | A kind of self-enclosed anode oxidation method of magnesium alloy |
| CN109267139A (en) * | 2018-10-31 | 2019-01-25 | 日照微弧技术有限公司 | A kind of electrolyte and preparation method thereof for magnesium alloy differential arc oxidation |
| CN110129858A (en) * | 2019-06-12 | 2019-08-16 | 北京石油化工学院 | A kind of ionic liquid auxiliary magnesium lithium alloy anode oxidation film-forming method |
| CN110129858B (en) * | 2019-06-12 | 2020-12-01 | 北京石油化工学院 | Ionic liquid assisted magnesium-lithium alloy anodic oxidation film forming method |
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Application publication date: 20140723 |