CN101671821B - Chemical conversion solution and chemical conversion process for magnesium alloy surface treatment - Google Patents
Chemical conversion solution and chemical conversion process for magnesium alloy surface treatment Download PDFInfo
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- CN101671821B CN101671821B CN2008100131873A CN200810013187A CN101671821B CN 101671821 B CN101671821 B CN 101671821B CN 2008100131873 A CN2008100131873 A CN 2008100131873A CN 200810013187 A CN200810013187 A CN 200810013187A CN 101671821 B CN101671821 B CN 101671821B
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- chemical conversion
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Abstract
The invention relates to magnesium alloy surface treatment technology, in particular to chemical conversion solution for magnesium alloy surface treatment chemical. The chemical conversion solution is prepared by using ethanol as a solvent and comprises 5 to 50 grams of cerous nitrate and 0.1 to 5 grams of citric acid per liter. In addition, the invention also provides a magnesium alloy surface treatment process which adopts a basic flow comprising oil removal, pickling, washing, drying, chemical conversion, washing and sealing by aqueous solution of sodium phosphate, wherein the mass percentage concentration of sodium phosphate is 1 to 5 percent. The rare earth chemical conversion treatment provided by the invention is particularly suitable for AZ91D magnesium alloy. A golden chemically converted film obtained by the process has a large adhesive force and high corrosion resistance. And the treatment process is simple, can be performed at normal temperature, is easy to control and applicable to industrial production, avoids the use of fluoride, hexavalent chromium and other harmful substances thoroughly and contributes to environmental protection.
Description
Technical field
The present invention relates to magnesium alloy surface treatment, particularly a kind of Mg alloy surface is handled chemical conversion solution and technology.
Background technology
Magnesium alloy has the advantages that density is little, specific tenacity is high, it is the lightest engineering materials, its density is equivalent to engineering plastics, have good heat conductivity, workability, easily castibility, good dimensional stability, damping property and electromagnetic wave shielding and easy recovery property, obtained application more and more widely in daily life and industrial circle, as fields such as automobile, mobile phone, computer, sports goodss, be described as " the green engineering material " of 21st century.As a kind of emerging structured material, corrosion-resistant has seriously restricted its application, and the protection question of magnesium alloy more and more is subject to people's attention, and it is more and more important that process for treating surface seems, its purpose mainly is to improve corrosion-resistant and Corrosion Protection.
Because the chemical property of magnesium alloy is very active, be easy to oxidized and corrosion, even magnesium alloy also can corrode in tap water, this has just seriously limited Application of Magnesium.Common surface treatment method of Mg alloy, complex process, process are restive, and often contain sexavalent chrome and fluorochemical in the inactivating treatment liquid to human body and the deleterious material of environment.
The corrosion resistance nature that substitute chromium hydrochlorate surface-treated rare earth chemistry conversion processing is used to improve materials such as aluminium alloy, stainless steel, carbon steel, magnesium alloy has obtained extensive studies, but in rare earth aqueous solution, handle the particularly non-constant of bonding strength of the resulting conversion film of AZ91D magnesium alloy and matrix alloy of magnesium alloy, this may be since in water solution system since the magnesium oxide that loosens that the corrosion of magnesium alloy forms cause, thereby cause further application difficulty, therefore this processing mode is badly in need of improving.
Summary of the invention
In view of above problem, one purpose of the present invention is to provide a kind of Mg alloy surface to handle the rare earth ethanol chemical conversion solution of usefulness, and this solution is made up of rare earth compound and organic acid, and composition is few, nontoxic pollution-free.
This kind Mg alloy surface provided by the invention is handled chemical conversion solution, and it is solvent with ethanol, comprises in every liter of this solution:
Cerous nitrate 5～50g;
Citric acid 0.1～5g;
Its preferred concentration range for is:
Cerous nitrate 5～10g/L;
Citric acid 0.5～1.5g/L;
As seen, Mg alloy surface provided by the invention is handled chemical conversion solution (rare earth ethanol chemical conversion solution) and is formed for rare earth compound and organic acid evenly are dissolved in ethanol, and this prescription is simple, does not contain the material of harmful to human such as sexavalent chrome and fluorochemical and environment.In this prescription:
Cerous nitrate is main film forming matter, and cerium required in the conversion processing process is provided, and citric acid is a film forming accelerating, promotes the formation of cerium conversion film.
In addition, another object of the present invention is to provide a kind of magnesium alloy surface rare earth treatment technique, this method especially more is applicable to the AZ91D magnesium alloy, has significantly improved the resistance to corrosion of magnesium alloy.
This kind magnesium alloy surface treatment process provided by the invention, its basic procedure is: oil removing → pickling → washing → drying → chemical conversion → washing → sodium phosphate aqueous solution sealing.The concrete steps of this method are:
A. oil removing, this step is in order to remove the greasy dirt on magnesium alloy component surface;
B. pickling, this step are to remove the oxide compound on magnesium alloy component surface, improve chemical conversion and handle quality;
C. washing, this step, are beneficial to chemical conversion and handle to avoid bringing in the Ethanol Treatment liquid for removing the remaining acid of Mg alloy surface;
D. dry, this step is for removing the remaining moisture content of Mg alloy surface, causes the corrosion of magnesium alloy to avoid bringing in the Ethanol Treatment liquid;
E. chemical conversion, this step are specially cleaning magnesium alloy component surface, at room temperature are impregnated in then in the Mg alloy surface processing chemical conversion solution and handle 1～2h, and obtaining thickness is the chemical conversion film of 3～6 μ m.
Among the present invention, chemical conversion film is analyzed through X-ray diffraction (XRD), learns that it mainly consists of cerium dioxide.
F. washing, this step be for removing the residual treatment solution of Mg alloy surface, in order to avoid bring in subsequently the sealing treatment liquid;
G. sodium phosphate aqueous solution sealing, this step is in order to improve the resistance to corrosion of Mg alloy surface, and its concrete steps are to handle 10～15min in 1～5% sodium phosphate aqueous solution (weight percent concentration of sodium phosphate is preferably 3%) for will impregnated in weight percent concentration through the magnesium alloy component of above-mentioned processing under normal temperature condition.
H. after treating that above-mentioned steps is finished, magnesium alloy component is taken out, use hot-air seasoning.
Like this; this kind Mg alloy surface ethanolic soln rare earth chemistry conversion treatment process provided by the invention; it is specially adapted to the AZ91D magnesium alloy; good by the chemical conversion film sticking power that this technology obtains; corrosion resistance significantly improves, and treatment temp is room temperature, save energy; do not use the material of harm health of human body such as containing sexavalent chrome and fluorochemical and environment in the entire treatment process, help environment protection.
Embodiment
Embodiment 1
Handle chemical conversion solution by following formulated Mg alloy surface:
Cerous nitrate 10g/L;
Citric acid 0.5g/L;
The sealing sodium phosphate aqueous solution:
Sodium phosphate 3% (weight percent concentration);
At first get an AZ91D magnesium alloy sample, put into gasoline, oxalic acid, deionized water then successively and clean, put into chemical conversion solution after the oven dry and carry out chemical conversion and handle, temperature is a room temperature, and the treatment time is 1h, obtains chemical conversion film.In the present embodiment, the thickness of chemical conversion film is 3 μ m, and chemical conversion film learns that through XRD analysis it mainly consists of cerium dioxide.
After above-mentioned processing, carry out sealing treatment 15min with putting into 3% sodium phosphate aqueous solution after the washed with de-ionized water, at last oven dry.The golden yellow rare earth chemistry conversion film of AZ91D magnesium alloy sticking power through above-mentioned processing is good, and by the 100h salt-fog test.
Embodiment 2
Handle chemical conversion solution by following formulated Mg alloy surface:
Cerous nitrate 20g/L;
Citric acid 1g/L;
The sealing sodium phosphate aqueous solution:
Sodium phosphate 5% (weight percent concentration);
At first get an AZ91D magnesium alloy sample, put into gasoline, oxalic acid, deionized water then successively and clean, put into chemical conversion solution after the oven dry and carry out chemical conversion and handle, temperature is a room temperature, and the treatment time is 1.5h, obtains chemical conversion film.In the present embodiment, the thickness of chemical conversion film is 5 μ m, and chemical conversion film learns that through XRD analysis it mainly consists of cerium dioxide.
After above-mentioned processing, carry out sealing treatment 12min with putting into 5% sodium phosphate aqueous solution after the washed with de-ionized water, at last oven dry.The golden yellow rare earth chemistry conversion film of AZ91D magnesium alloy sticking power through above-mentioned processing is good, and by the 100h salt-fog test.
Embodiment 3
Handle chemical conversion solution by following formulated Mg alloy surface:
Cerous nitrate 30g/L;
Citric acid 0.3g/L;
The sealing sodium phosphate aqueous solution:
Sodium phosphate 2% (weight percent concentration);
At first get an AZ91D magnesium alloy sample, put into gasoline, oxalic acid, deionized water then successively and clean, put into chemical conversion solution after the oven dry and carry out chemical conversion and handle, temperature is a room temperature, and the treatment time is 1.2h, obtains chemical conversion film.In the present embodiment, the thickness of chemical conversion film is 4 μ m, and chemical conversion film learns that through XRD analysis it mainly consists of cerium dioxide.
After above-mentioned processing, carry out sealing treatment 13min with putting into 2% sodium phosphate aqueous solution after the washed with de-ionized water, at last oven dry.The golden yellow rare earth chemistry conversion film of AZ91D magnesium alloy sticking power through above-mentioned processing is good, and by the 100h salt-fog test.
Embodiment 4
Handle chemical conversion solution by following formulated Mg alloy surface:
Cerous nitrate 35g/L;
Citric acid 2g/L;
The sealing sodium phosphate aqueous solution:
Sodium phosphate 4% (weight percent concentration);
At first get an AZ91D magnesium alloy sample, put into gasoline, oxalic acid, deionized water then successively and clean, put into chemical conversion solution after the oven dry and carry out chemical conversion and handle, temperature is a room temperature, and the treatment time is 1.8h, obtains chemical conversion film.In the present embodiment, the thickness of chemical conversion film is 6 μ m, and chemical conversion film learns that through XRD analysis it mainly consists of cerium dioxide.
After above-mentioned processing, carry out sealing treatment 15min with putting into 4% sodium phosphate aqueous solution after the washed with de-ionized water, at last oven dry.The golden yellow rare earth chemistry conversion film of AZ91D magnesium alloy sticking power through above-mentioned processing is good, and by the 100h salt-fog test.
Embodiment 5
Handle chemical conversion solution by following formulated Mg alloy surface:
Cerous nitrate 25g/L;
Citric acid 1.5g/L;
The sealing sodium phosphate aqueous solution:
Sodium phosphate 2.5% (weight percent concentration);
At first get an AZ91D magnesium alloy sample, put into gasoline, oxalic acid, deionized water then successively and clean, put into chemical conversion solution after the oven dry and carry out chemical conversion and handle, temperature is a room temperature, and the treatment time is 1.6h, obtains chemical conversion film.In the present embodiment, the thickness of chemical conversion film is 5 μ m, and the chemical conversion film chemical conversion film learns that through XRD analysis it mainly consists of cerium dioxide.
After above-mentioned processing, carry out sealing treatment 10min with putting into 2.5% sodium phosphate aqueous solution after the washed with de-ionized water, at last oven dry.The golden yellow rare earth chemistry conversion film of AZ91D magnesium alloy sticking power through above-mentioned processing is good, and by the 100h salt-fog test.
Embodiment result shows; the golden yellow chemical conversion film sticking power of magnesium alloy that obtains by this technology is good; has excellent corrosion resisting performance; treatment process is simple; can carry out at normal temperatures, be easy to control, be fit to suitability for industrialized production; and do not use objectionable impuritiess such as fluorochemical, sexavalent chrome in the entire treatment process, help health of human body and environment protection.
In addition, the above only is the preferable feasible embodiment of the present invention, the interest field that can not limit to the present invention with this, and described rare earth chemistry conversion treating solution can be used for the AZ91D magnesium alloy, also can be applicable to the magnesium alloy of other type.Therefore, make other various corresponding changes and distortion, still belong within the protection domain that the present invention contains according to technical scheme of the present invention and technical thought.
Claims (8)
1. a Mg alloy surface is handled chemical conversion solution, it is characterized in that, comprises in every liter of ethanolic soln:
Cerous nitrate 5～50g;
Citric acid 0.1～5g.
2. Mg alloy surface according to claim 1 is handled chemical conversion solution, it is characterized in that, the screening formulation that described Mg alloy surface is handled chemical conversion solution is:
Cerous nitrate 5～10g/L;
Citric acid 0.5～1.5g/L.
3. Mg alloy surface according to claim 1 is handled chemical conversion solution, it is characterized in that, the optimum formula that described Mg alloy surface is handled chemical conversion solution is:
Cerous nitrate 5g/L;
Citric acid 1g/L.
4. a magnesium alloy surface treatment process is characterized in that, its basic procedure is: oil removing → pickling → washing → drying → chemical conversion → washing → sodium phosphate aqueous solution sealing, and the concrete steps of this method are:
A. oil removing, this step is in order to remove the greasy dirt on magnesium alloy component surface;
B. pickling, this step are to remove the oxide compound on magnesium alloy component surface;
C. washing, this step is for removing the remaining acid of Mg alloy surface;
D. dry, this step is for removing the remaining moisture content of Mg alloy surface;
E. chemical conversion, this step are specially cleaning magnesium alloy component surface, are impregnated in aforesaid right requirement 1～3 any described Mg alloy surface then and handle in the chemical conversion solution;
F. washing, this step is for removing the residual chemical conversion solution of Mg alloy surface;
G. sodium phosphate aqueous solution sealing, this step is handled in the sodium phosphate aqueous solution for impregnated under normal temperature condition through the magnesium alloy component of above-mentioned processing;
H. after treating that above-mentioned steps is finished, magnesium alloy component is taken out, use hot-air seasoning.
5. magnesium alloy surface treatment process according to claim 4 is characterized in that, in the chemical conversion, magnesium alloy is handled 1～2h in chemical conversion solution, obtains chemical conversion film, and the thickness range of chemical conversion film is 3～6 μ m.
6. magnesium alloy surface treatment process according to claim 4 is characterized in that, in the described sodium phosphate aqueous solution, the weight percent concentration of sodium phosphate is 1～5%.
7. magnesium alloy surface treatment process according to claim 4 is characterized in that, in the described sodium phosphate aqueous solution, the weight percent concentration of sodium phosphate is preferably 3%.
8. magnesium alloy surface treatment process according to claim 4 is characterized in that, handles 10～15min in the sodium phosphate aqueous solution.
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| CN2008100131873A CN101671821B (en) | 2008-09-12 | 2008-09-12 | Chemical conversion solution and chemical conversion process for magnesium alloy surface treatment |
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| CN2008100131873A CN101671821B (en) | 2008-09-12 | 2008-09-12 | Chemical conversion solution and chemical conversion process for magnesium alloy surface treatment |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101200526B1 (en) * | 2010-06-09 | 2012-11-13 | 주식회사 엔유씨전자 | Method for surface treating available the metallic effect |
| CN102181851B (en) * | 2011-04-21 | 2012-08-22 | 哈尔滨工程大学 | Anhydrous pretreatment method for coating surfaces of magnesium alloys |
| CN107815626B (en) * | 2017-11-02 | 2019-03-22 | 上海瀚氏模具成型有限公司 | A kind of almag making Nano surface technique |
| CN108018544A (en) * | 2017-12-01 | 2018-05-11 | 博罗县东明化工有限公司 | Magnesium alloy rare-earth conversion coatings inorganic agent and its processing method |
| CN110670054B (en) * | 2019-10-11 | 2021-06-29 | 青海民族大学 | Magnesium alloy surface cerate conversion repair film and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1786270A (en) * | 2005-11-08 | 2006-06-14 | 大连理工大学 | Treatment method of magnosium alloy surface |
| CN101113518A (en) * | 2006-07-28 | 2008-01-30 | 佛山市顺德区汉达精密电子科技有限公司 | Magnesium alloy surface rare earth treatment technique |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1786270A (en) * | 2005-11-08 | 2006-06-14 | 大连理工大学 | Treatment method of magnosium alloy surface |
| CN101113518A (en) * | 2006-07-28 | 2008-01-30 | 佛山市顺德区汉达精密电子科技有限公司 | Magnesium alloy surface rare earth treatment technique |
Non-Patent Citations (2)
| Title |
|---|
| 张勇等.稀土铈对AZ91镁合金表面腐蚀性能的影响.《哈尔滨工业大学学报》.2002,第34卷(第3期),第376-378页. * |
| 许越等.AZ91镁合金表面稀土转化膜的制备及耐蚀性能研究.《中国稀土学报》.2005,第23卷(第1期),第40-43页. * |
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