CN100519840C - Magnesium alloy surface phosphorization treatment method - Google Patents
Magnesium alloy surface phosphorization treatment method Download PDFInfo
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- CN100519840C CN100519840C CNB2007101445873A CN200710144587A CN100519840C CN 100519840 C CN100519840 C CN 100519840C CN B2007101445873 A CNB2007101445873 A CN B2007101445873A CN 200710144587 A CN200710144587 A CN 200710144587A CN 100519840 C CN100519840 C CN 100519840C
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Abstract
The present invention magnesium alloy material surface phosphatizing solution and its treating process. The surface phosphatizing solution consists of 85 % concentration phosphoric acid solution in 10-20 ml/l, zinc oxide in 1-5 g/l, sodium fluoride in 1-3 g/l, sodium nitrate in 0.1-0.4 g/l, hydrogen peroxide in 0.5-1 g/l and water for the rest. Hydrogen peroxide is adopted as the promoter to speed film formation and raise the corrosion resistance of the produced conversion film and adhesion of the lacquer film, and as the environment friendly oxidant. The surface phosphatizing solution has simple composition, easy control, stable technological process and low cost, and is suitable for industrial production.
Description
(1) technical field
The present invention is to provide a kind of metallic surface treatment process, specifically a kind of surface treatment method of magnesium alloy.
(2) background technology
Magnesium alloy has excellent performance such as low density, high specific stiffness and specific tenacity, but because the magnesium alloy chemical activity is high, electropotential is low, therefore, the corrosion resistance nature of magnesium alloy is very poor, has restricted the use of magnesium alloy.The method of raising corrosion stability of magnesium alloy commonly used mainly contains chemical conversion film processing, anodic oxidation, plasma micro-arc anodic oxidation, surperficial infiltration layer, Laser Surface Treatment or the like at present.Wherein the chemical conversion film processing is effective ways of magnesium alloy surface protective, chemical conversion film is handled and mainly can be divided into two kinds of chromate treating and chromium-free treatment, chromate treating is because chromic existence can cause serious environmental to be polluted, and its use range has been subjected to serious control.Bonderizing is one of method that replaces deleterious chromate treating.Existing parkerizing method is to add nitrite ion or permanganate has been reduced the effect of quickening phosphatization as oxygenant in phosphatization liquid, but nitrite ion is poisonous, so exploitation environment-friendly type treatment solution has become certainty.
(3) summary of the invention
The object of the present invention is to provide a kind of environmental pollution little, and on magnesium alloy, obtain better solidity to corrosion and paint film adhesion, the Mg alloy surface parkerizing method that the treatment time is short, efficient is high.
The object of the present invention is achieved like this:
The prescription of etching solution of the present invention is: the water of 85% phosphatase 11,0~20mL/L, zinc oxide 1~5g/L, Sodium Fluoride 1~3g/L, SODIUMNITRATE 0.1~0.4g/L, hydrogen peroxide 0.5~1g/L and surplus.
Treatment process of the present invention is:
1, mechanical pretreatment: with 1000
#Abrasive paper for metallograph polishing magnesium alloy, washing then;
2, degreasing: use the 10%NaOH solution washing, temperature is controlled between 45-50 ℃, and the time is 4-5 minute, then washing;
3, pickling: use 75%H
3PO
4Solution washing, temperature are controlled at 28-30 ℃, and the time is 1 minute, then washing;
4, activation: under 40 ℃ of situations of temperature, adopting concentration is that 46% HF, 200mL/L handled washing then 1 minute.
5, film forming: will immerse through the magnesium alloy of pre-treatment in the film-forming soln of forming by the water of 85% phosphatase 11,0~20mL/L, zinc oxide 1~5g/L, Sodium Fluoride 1~3g/L, SODIUMNITRATE 0.1~0.4g/L, hydrogen peroxide 0.5~1g/L and surplus, temperature is controlled at 45-47 ℃, and the immersion time is 2 minutes;
6, aftertreatment: use the deionized water clean surface, dry up.
The reaction of phosphoric acid among the present invention and zinc oxide generates primary zinc phosphate, and zine ion and dihydrogen phosphate ions are provided, and under the promoter action of Sodium Fluoride and hydrogen peroxide, generates insoluble phosphate and forms phosphatize phosphate coat; The effect of Sodium Fluoride provides F
-(1) plays shock absorption, effectively stablize phosphatization liquid pH value (2) F
-Can partly block the positive column, impel collective's metal anode to dissolve, reduce the overvoltage of hydrogen to a certain extent, play the cathodic depolarization effect, its surface is formed be beneficial to the active zone of phosphate crystal growth, thereby has quickened film forming, (3) F that shortened the reaction times
-Can also crystal grain thinning, make the rete densification; Hydrogen peroxide promotes phosphatize phosphate coat to form as oxidation promotor, improves membranous layer corrosion resistance.The present invention by to the selection of each raw material in the etching solution with cooperate, to the optimization of operational path and condition, can receive following effect:
1. the present invention adopts hydrogen peroxide to make oxidation promotor, has quickened film forming speed, and the conversion film of generation has the higher erosion resistance of conversion film that forms as oxidation promotor than nitrate ion/nitrite ion or potassium permanganate;
2. the phosphorization filming time of the present invention is 2 minutes, and the treatment time is short, the production efficiency height;
3. phosphorization filming temperature of the present invention is 47 ℃, belongs to the normal temperature scope, and is not high to producing temperature requirement, is fit to suitability for industrialized production;
4. the present invention adopts hydrogen peroxide as oxidant, nontoxic pollution-free, environmental protection;
5. treatment solution composition of the present invention is simple, is easy to control, process stabilizing;
6. raw material of the present invention is easy to get, and cost is low, is fit to suitability for industrialized production.
These technique effects of the present invention have passed through experimental verification, and checking is the result embody by accompanying drawing.
(4) description of drawings
Fig. 1 is the anodic polarization curves of first kind of embodiment of the present invention;
Fig. 2 is the hydrogen-separating quantity comparison diagram before and after handling;
Fig. 3 is the corrosion weight loss comparison diagram before and after handling.
(5) embodiment
For example the present invention is done in more detail below and describes:
The composition of magnesium alloy phosphating film film-forming soln by
Its preparation method is: sample is a die casting AZ91D magnesium alloy
1) mechanical pretreatment: with 1000
#Foreign matter is removed in the abrasive paper for metallograph polishing, reduces surfaceness, then washing;
2) degreasing: use the 10%NaOH solution washing, temperature is controlled between 50 ℃, and the time is 5 minutes, then washing;
3) pickling: use 75%H
3PO
4Solution washing is removed oxide on surface, and temperature is controlled at 30 ℃, and the time is 1 minute,
Washing then;
4) activation: under 40 ℃ of situations of temperature, adopt HF (46%) 200mL/L to remove metallic surface oxide film and pickling ash as thin as a wafer, the time is 1 minute, then washing.
4) film forming: will be immersed in through the magnesium alloy sample of pre-treatment in the film-forming soln, temperature is controlled at 47 ℃, and the immersion time is 2 minutes, can obtain the phosphate chemical conversion film.
5) aftertreatment: use the deionized water clean surface, dry up with blower.
Its preparation method is with embodiment 1
Its preparation method is with embodiment 1
The polarization curve of AZ91D in 3.5%NaCl after measurement AZ91D and the phosphatization is as Fig. 1.
Claims (1)
1, a kind of Mg alloy surface parkerizing method is characterized in that:
(1), mechanical pretreatment: with 1000
#Abrasive paper for metallograph polishing magnesium alloy, washing then, described magnesium alloy is a die casting AZ91D magnesium alloy;
(2), degreasing: use the 10%NaOH solution washing, temperature is controlled between 45-50 ℃, and the time is 4-5 minute, then washing;
(3), pickling: use 75%H
3PO
4Solution washing, temperature are controlled at 28-30 ℃, and the time is 1 minute, then washing;
(4), activation: under 40 ℃ of situations of temperature, adopting concentration is that 46% HF, 200mL/L handled washing then 1 minute;
(5), film forming: will immerse through the magnesium alloy of pre-treatment in the film-forming soln of forming by the water of 85% phosphoric acid 20mL/L, zinc oxide 5g/L, Sodium Fluoride 3g/L, SODIUMNITRATE 0.4g/L, hydrogen peroxide 1g/L and surplus, temperature is controlled at 45-47 ℃, and the immersion time is 2 minutes;
(6), aftertreatment: use the deionized water clean surface, dry up.
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Cited By (1)
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CN103469282A (en) * | 2013-09-27 | 2013-12-25 | 昆山纯柏精密五金有限公司 | Preprocessing method of magnesium alloy electro-coating technology |
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CN101906628A (en) * | 2010-07-30 | 2010-12-08 | 华南理工大学 | Phosphate conversion solution and method for processing surface of magnesium alloy by utilizing same |
CN102002697A (en) * | 2010-11-01 | 2011-04-06 | 云南滇科涂镀层材料有限公司 | Environmentally friendly chromium-free passivation solution for galvanization and preparation method thereof |
CN102199766B (en) * | 2011-04-22 | 2012-09-26 | 哈尔滨工程大学 | Method for preparing magnesium lithium alloy cerium salt and molybdate-phosphate-zirconium fluoride conversion coating |
CN102886569B (en) * | 2011-07-22 | 2014-10-29 | 浙江瑞翌新材料科技有限公司 | Pre-treatment method and pre-treatment system for core wire of diamond wire saw |
CN108165969A (en) * | 2017-12-26 | 2018-06-15 | 贵州钢绳股份有限公司 | A kind of preparation method of steel wire room temperature electrolytic phosphating liquid |
CN109183015B (en) * | 2018-08-03 | 2020-09-15 | 广州正利金属表面处理剂有限公司 | Nickel-free coating agent and preparation method thereof |
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2007
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Non-Patent Citations (2)
Title |
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镁合金表面的磷化处理工艺研究. 王洁,丁毅.2006年全国腐蚀电化学及测试方法学术会议论文集,第无卷第无期. 2006 |
镁合金表面的磷化处理工艺研究. 王洁,丁毅.2006年全国腐蚀电化学及测试方法学术会议论文集,第无卷第无期. 2006 * |
Cited By (1)
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CN103469282A (en) * | 2013-09-27 | 2013-12-25 | 昆山纯柏精密五金有限公司 | Preprocessing method of magnesium alloy electro-coating technology |
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