CN100532642C - Process for preparing magnesium alloy chemical conversion coating - Google Patents
Process for preparing magnesium alloy chemical conversion coating Download PDFInfo
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- CN100532642C CN100532642C CNB2005100353165A CN200510035316A CN100532642C CN 100532642 C CN100532642 C CN 100532642C CN B2005100353165 A CNB2005100353165 A CN B2005100353165A CN 200510035316 A CN200510035316 A CN 200510035316A CN 100532642 C CN100532642 C CN 100532642C
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Abstract
The invention discloses a chemical transmission film preparing technology of magnesium alloy, which comprises the following steps: a. proceeding degreasing disposal for magnesium or magnesium alloy through sodium hydroxide or one or multiple hybrid solutions of sodium phosphate with sodium hydroxide, sodium carbonate and sodium silicate solution; b. proceeding acid cleaning disposal for degreased magnesium or magnesium alloy through hybrid solution of phosphoric acid and sodium phosphate; c. proceeding activating disposal for acid cleaned magnesium or magnesium alloy through hybrid solution of fluohydric acid and sodium phosphate; d proceeding chemical synthesizing disposal for activated magnesium or magnesium alloy through composite solution of calcium nitrate hydrate, sodium nitrite, sodium iodide and hydrogen dioxide solution; e. packing hole of synthetic magnesium or magnesium alloy through deionized water. The invention doesn't utilize chromic composition, which eliminates danger for environment.
Description
Technical field
The present invention relates to metal surface treatment process, particularly relate to a kind of chromate-free corrosion-resistant treatments technology that is used for magnesium and magnesium alloy.
Background technology
Magnesium alloy is a lightest present metal engineering material, its density is 1.74g/cm3, only be aluminium 2/3, iron 1/4, has the specific tenacity height simultaneously, the characteristics of good processability, at aspects such as automobile, motorcycle, aerospace, electronics IT, war products wide application prospect is arranged, be described as " the green engineering material of 21 century ".But the chemical property of magnesium is active, and stability is low, standard potential negative (2.36eV), the solidity to corrosion extreme difference, even at room temperature also oxidation can take place in air, surface film oxide is loose and be alkalescence, its pH value is approximately 10.5, is unfavorable for application.Therefore, the solidity to corrosion difference becomes a principal element of its performance structure properties advantage of restriction.Carrying out suitable surface treatment has great significance to strengthen its solidity to corrosion.
The chemical surface treatment of magnesium alloy has chemical conversion, anodic oxidation, plasma micro-arc anodic oxidation and metal plating etc.Conversion film is to form the surface film that one deck is made up of oxide compound, chromium compounds, phosphide and some other compound by electrochemistry or chemical process in base metal surface.For magnesium alloy, conversion film has certain decorative and protective, also can be used as the pretreatment procedure of other treatment processs simultaneously.Conversion film is to prevent collective's corrosion by the compound rete that forms the low blocking layer of solubleness or have a corrosion inhibition between matrix metal and environment.Chemical conversion film is very thin, and the solidity to corrosion of chemical conversion film be studies show that chemical conversion film can only slow down corrosion speed, can not effectively prevent corrosion.
At present, many dissimilar conversion films are arranged, comprise chromate conversion coating, phosphoric acid-potassium permanganate conversion film, fluozirconate conversion film, stannate conversion film etc.The main drawback of existing conversion film is exactly that treatment solution contains deleterious chemical substance.Traditional conversion coating treating fluid all is based on all cpds of chromium, and chromium has very strong carinogenicity.Along with the enhancing of environmental consciousness, exploitation environment-friendly type treatment solution has become inevitable.
Summary of the invention
The present invention is intended to address the above problem, and provide a kind of simple to operate, cost is low, the not chromate-containing process for preparing magnesium alloy chemical conversion coating that is used for magnesium and magnesium-alloy material that is suitable for producing in batches is to satisfy environmental requirement.
For achieving the above object, the invention provides a kind of magnesium or process for preparing magnesium alloy chemical conversion coating, this technology comprises the steps:
A, magnesium or magnesium alloy are carried out skimming treatment with one or more the mixing solutions in sodium hydroxide solution, the sodium phosphate that contains sodium hydroxide, yellow soda ash, the sodium silicate solution;
B, will carry out cleanup acid treatment through the magnesium or the magnesium alloy of skimming treatment with the mixing solutions of phosphoric acid and sodium phosphate;
C, magnesium or magnesium alloy through pickling are carried out activation treatment with the mixing solutions of hydrofluoric acid and sodium phosphate;
D, change into processing with the mixing solutions of six water nitrocalcite, Sodium Nitrite, sodium iodide, hydrogen peroxide magnesium or the magnesium alloy after to activation;
E, magnesium or the magnesium alloy that changes into after the processing carried out sealing of hole with deionized water;
In the steps d, the weight percent content of each component of described mixing solutions is as follows:
Six water nitrocalcite 1～2%
Sodium Nitrite 5～6%
Sodium iodide 1.5～2.5%
Hydrogen peroxide 2.5～4%
Above-mentioned each component concentrations is respectively:
Six water nitrocalcite, 22～23g/L
Sodium Nitrite 62～66g/L
Sodium iodide 23～25g/L
Hydrogen peroxide 35～45g/L.
Among the step a, the weight percent content of each component of described mixing solutions is as follows:
Sodium hydroxide 0.5～2%
Sodium phosphate 2～4%
Yellow soda ash 1～2%
Water glass 1～2%
Surplus is a water;
Above-mentioned each component concentrations is respectively:
Sodium hydroxide 10g/L～20g/L
Sodium phosphate 35g/L～45g/L
Yellow soda ash 13g/L～17g/L
Water glass 13g/L～17g/L.
The temperature of skimming treatment is 60 ℃～70 ℃, and degreasing time is 2 minutes～5 minutes.
Among the step b, the weight percent content of phosphoric acid is 1～3%, and concentration is 18g/L～22g/L; The weight percent content of sodium phosphate is 0.5～2%, and concentration is 10g/L～20g/L; The pickling time is 40 seconds～80 seconds.
Among the step c, the weight percent content of hydrofluoric acid is 1～2%, and concentration is 14g/L～16g/L; The weight percent content of sodium phosphate is 0.5～2%, and concentration is 10g/L～20g/L; Soak time is 90 seconds～150 seconds.
The temperature that changes into processing is 45 ℃～55 ℃, and the time of changing into is 10 minutes～18 minutes.
Among the step e, the water temperature that sealing of hole is handled is 80 ℃～90 ℃, and the time is 2 minutes～5 minutes.
Contribution of the present invention is, owing to do not contain chromium cpd in treatment solution, and used chromate-free, thereby eliminated the harm that toxic substance may cause environment, has tangible environment protecting.Conversion film resistance to corrosion by method of the present invention preparation is better, and sticking power can satisfy and is coated with reload request.The present invention simultaneously also has technology and working method is simple, and is with low cost, is suitable for characteristics such as batch process.
Embodiment
The step of magnesium of the present invention or process for preparing magnesium alloy chemical conversion coating comprises: degreasing, washing, pickling, washing, activation, wash, change into, sealing of hole and oven dry, its concrete steps are as follows:
A, degreasing: with weight percent is 1%, concentration is that sodium hydroxide, the weight percent of 15g/L is 3%, concentration is that sodium phosphate, the weight percent of 40g/L is 1.5%, concentration is that yellow soda ash and the weight percent of 15g/L is 1.5%, concentration is that the water glass of 15g/L is formed mixing solutions, 65 ℃ temperature magnesium or magnesium alloy is carried out skimming treatment 3 minutes.Available deionized water repeatedly washes after the degreasing, and the degreasing fluid that remains on magnesium or the magnesium alloy workpiece is rinsed well.
B, pickling: with weight percent is 2%, concentration is that phosphoric acid and the weight percent of 20ml/L is 1%, concentration is that the sodium phosphate of 15g/L is formed mixing solutions, at room temperature will carry out cleanup acid treatment 1 minute through the magnesium or the magnesium alloy of skimming treatment, uses ultrasonic cleaning then 5 minutes.
C, be 1.5% with weight percent, concentration is that hydrofluoric acid and the weight percent of 15ml/L is 1%, concentration is that the sodium phosphate of 15g/L is formed mixing solutions, at room temperature magnesium or magnesium alloy through pickling were carried out activation treatment 2 minutes, repeatedly wash with deionized water after the activation treatment, the debris on magnesium or the magnesium alloy workpiece is rinsed well.
D, be 1.5% with weight percent, concentration is that six water nitrocalcite, the weight percent of 22g/L is 5.5%, concentration is that Sodium Nitrite, the weight percent of 64g/L is 2%, concentration is that sodium iodide, the weight percent of 23g/L is 3%, concentration is that the hydrogen peroxide of 40ml/L is formed mixing solutions, magnesium after 50 ℃ temperature are to activation or magnesium alloy change into to be handled 15 minutes, reached 7.0～7.2 to pH value.Change into time lengthening, then thickness increases, and corrosion resistance improves, and is loss of adhesion accordingly.
E, sealing of hole: the deionized water that with temperature is 85 ℃ carries out sealing of hole and handled 3 minutes changing into magnesium after the processing or magnesium alloy.
Behind the sealing of hole routinely technology oven dry get final product.
By the main component near magnesium or magnesium alloy substrate layer in the conversion film of above-mentioned prepared is substrate metal oxide; Middle layer and outermost layer are the inferior calcium of metal oxide, oxidation, four oxidation DFPs and three oxidation dicalcium.Conversion film behind the sealing of hole is a canescence, and resistance to corrosion is better, and sticking power can satisfy and is coated with reload request.
Claims (7)
1, a kind of magnesium or process for preparing magnesium alloy chemical conversion coating is characterized in that, this technology comprises the steps:
A, magnesium or magnesium alloy are carried out skimming treatment with one or more the mixing solutions in sodium hydroxide solution, the sodium phosphate that contains sodium hydroxide, yellow soda ash, the sodium silicate solution;
B, will carry out cleanup acid treatment through the magnesium or the magnesium alloy of skimming treatment with the mixing solutions of phosphoric acid and sodium phosphate;
C, magnesium or magnesium alloy through pickling are carried out activation treatment with the mixing solutions of hydrofluoric acid and sodium phosphate;
D, change into processing with the mixing solutions of six water nitrocalcite, Sodium Nitrite, sodium iodide, hydrogen peroxide magnesium or the magnesium alloy after to activation;
E, magnesium or the magnesium alloy that changes into after the processing carried out sealing of hole with deionized water;
In the step (d), the weight percent content of each component of described mixing solutions is as follows:
Six water nitrocalcite 1～2%
Sodium Nitrite 5～6%
Sodium iodide 1.5～2.5%
Hydrogen peroxide 2.5～4%
Above-mentioned each component concentrations is respectively:
Six water nitrocalcite, 22～23g/L
Sodium Nitrite 62～66g/L
Sodium iodide 23～25g/L
Hydrogen peroxide 35～45g/L.
2, magnesium as claimed in claim 1 or process for preparing magnesium alloy chemical conversion coating is characterized in that, in the step (a), the weight percent content of each component of described mixing solutions is as follows:
Sodium hydroxide 0.5～2%
Sodium phosphate 2～4%
Yellow soda ash 1～2%
Water glass 1～2%
Surplus is a water;
Above-mentioned each component concentrations is respectively:
Sodium hydroxide 10g/L～20g/L
Sodium phosphate 35g/L～45g/L
Yellow soda ash 13g/L～17g/L
Water glass 13g/L～17g/L.
3, magnesium as claimed in claim 2 or process for preparing magnesium alloy chemical conversion coating is characterized in that, in the step (a), the temperature of skimming treatment is 60 ℃～70 ℃, and degreasing time is 2 minutes～5 minutes.
4, magnesium as claimed in claim 1 or process for preparing magnesium alloy chemical conversion coating is characterized in that, in the step (b), the weight percent content of phosphoric acid is 1～3%, and concentration is 18g/L～22g/L; The weight percent content of sodium phosphate is 0.5～2%, and concentration is 10g/L～20g/L; The pickling time is 40 seconds～80 seconds.
5, magnesium as claimed in claim 1 or process for preparing magnesium alloy chemical conversion coating is characterized in that, in the step (c), the weight percent content of hydrofluoric acid is 1～2%, and concentration is 14g/L～16g/L; The weight percent content of sodium phosphate is 0.5～2%, and concentration is 10g/L～20g/L; Soak time is 90 seconds～150 seconds.
6, magnesium as claimed in claim 1 or process for preparing magnesium alloy chemical conversion coating is characterized in that, in the step (d), the temperature that changes into processing is 45 ℃～55 ℃, and the time of changing into is 10 minutes～18 minutes.
7, magnesium as claimed in claim 1 or process for preparing magnesium alloy chemical conversion coating is characterized in that, in the step (e), the water temperature that sealing of hole is handled is 80 ℃～90 ℃, and the time is 2 minutes～5 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100353165A CN100532642C (en) | 2005-06-13 | 2005-06-13 | Process for preparing magnesium alloy chemical conversion coating |
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|---|---|---|---|
| CNB2005100353165A CN100532642C (en) | 2005-06-13 | 2005-06-13 | Process for preparing magnesium alloy chemical conversion coating |
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| CN1880503A CN1880503A (en) | 2006-12-20 |
| CN100532642C true CN100532642C (en) | 2009-08-26 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101469421B (en) * | 2007-12-29 | 2010-12-22 | 比亚迪股份有限公司 | Film forming solution for magnesium alloy chemical composition coating and preparation thereof |
| CN101642585B (en) * | 2008-08-06 | 2013-01-16 | 中国科学院金属研究所 | Biological activating solution for surface of magnesium alloy and application thereof |
| CN101623944B (en) * | 2009-08-10 | 2013-08-21 | 北京华盛荣镁业科技有限公司 | Magnesium alloy sandwich plate and preparation method thereof |
| CN102115880B (en) | 2009-12-31 | 2015-10-14 | 汉高股份有限及两合公司 | The surface treating composition of light metal or its alloy and solution and surface treatment method |
| CN101886258B (en) * | 2010-07-01 | 2012-01-18 | 北方工业大学 | Method for preparing magnesium alloy surface conversion corrosion-resistant film layer |
| CN102586763B (en) * | 2012-03-21 | 2014-07-16 | 成都青元泛镁科技有限公司 | Novel chemical nickel-plating method for magnesium alloy |
| CN103625038A (en) * | 2012-08-20 | 2014-03-12 | 芳源企业（上海）有限公司 | Pvc plastic soft coating metal armrest and manufacturing method thereof |
| CN103668163B (en) * | 2013-10-31 | 2016-08-31 | 沈阳工业大学 | A kind of magnesium alloy die casting process for surface preparation |
| CN106987834A (en) * | 2016-01-21 | 2017-07-28 | 宝山钢铁股份有限公司 | A kind of film build method and chemical composition coating of magnesium-rare earth alloy chemical composition coating |
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Effective date of registration: 20201210 Address after: 214500 No. 18 Shannan Road, Chengbei Park, Jingjiang City, Taizhou City, Jiangsu Province Patentee after: Jiangdong Aerospace new materials (Jiangsu) Co., Ltd Address before: 518119 BYD Industrial Park, Yanan Road, Kwai Chung Town, Longgang District, Guangdong, Shenzhen Patentee before: BYD Co.,Ltd. |
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Effective date of registration: 20211025 Address after: 214500 No. 18 Shannan Road, Chengbei Park, Jingjiang City, Taizhou City, Jiangsu Province Patentee after: Jingjiang City Huaxin Technology Park Co.,Ltd. Address before: 214500 No. 18 Shannan Road, Chengbei Park, Jingjiang City, Taizhou City, Jiangsu Province Patentee before: Jiangdong Aerospace new materials (Jiangsu) Co., Ltd |