CN102808210A - Micro-arc oxidation surface treatment method and product prepared by same - Google Patents
Micro-arc oxidation surface treatment method and product prepared by same Download PDFInfo
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- CN102808210A CN102808210A CN2012102946146A CN201210294614A CN102808210A CN 102808210 A CN102808210 A CN 102808210A CN 2012102946146 A CN2012102946146 A CN 2012102946146A CN 201210294614 A CN201210294614 A CN 201210294614A CN 102808210 A CN102808210 A CN 102808210A
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Abstract
The invention provides a micro-arc oxidation treatment method applicable to magnesium and magnesium alloy surfaces and a magnesium alloy product obtained by treatment. The optimal process suitable for MB3 magnesium alloy is obtained by making an intensive study on micro-arc oxidation treatment of the specific MB3 magnesium alloy and conducting a great number of repeated groping studies on the steps and details from pretreatment, micro-arc oxidation treatment to after-treatment, and energy consumption and pollution in treatment are greatly reduced with efficiency and film forming quality guaranteed. Results show that a compact and uniform ceramic oxidation film layer closely combined with a magnesium alloy matrix is generated on the magnesium alloy surface obtained by the micro-arc oxidation treatment process, so that corrosion resistance is greatly improved.
Description
Technical field
The present invention relates to the technical field of surface of light alloy; Differential arc oxidation treatment method and the light alloy goods of treated gained, especially a kind of differential arc oxidation treatment method of Mg alloy surface and the magnesium alloy product of treated gained on a kind of specifically light alloy surface.
Background technology
Differential arc oxidation is emerging at home and abroad in recent years a kind of light alloy process for treating surface; It is that the matrix metal that is processed is placed in the specific electrolytic solution; Utilize electrochemical method to produce the micro-arc discharge phenomenon at matrix surface; Under the acting in conjunction of plasma chemistry, thermochemistry and electrochemistry etc., directly become the oxide ceramics rete to base metal surface through the effect of microcell moment high temperature sintering.Compare just like traditional anodic oxidation with other surface treatment methods; Differential arc oxidation has the advantage of following uniqueness: for example both contained the high-temperature stable phase in the oxide membranous layer; Contain a certain amount of amorphous phase again, thereby make rete have excellent combination of strength and toughness and performance such as wear-resisting, anti-corrosion, anti-oxidant; The electrolytic solution that adopts scarcely contains Toxic and heavy metal element, is the treatment process of typical clean environment firendly; Technology is simple, need not gas or vacuum protection during processing, and the anodic oxidation that treatment temp is more traditional is low; It is little to handle back matrix metal size distortion.
Because the plurality of advantages of differential arc oxidation, it worldwide becomes the research focus very soon, especially for improving hardness, toughness, wear resistance and all relatively poor relatively light metal or its alloy of solidity to corrosion.This wherein, main research object is the differential arc oxidization technique of aluminium and alloy thereof, and also is in the starting exploratory stage for the research of other light alloys and metal thereof, and system and deep research are not arranged.
Magnesiumalloy has that density is low, the energy decrement coefficient is big, effectiveness good, specific tenacity and than numerous advantages such as Young's modulus height, is the environment-friendly type engineering materials of a kind of ultra-light, excellent property, is described as 21 century ideal electronic products case material.But magnesium is as lively as a cricket metal, and Standard Electrode Potentials is lower, and chemically reactive is high; In general environment, can receive corrosion seriously, even at room temperature also oxidation can take place in air, the natural oxide film of generation is loose porous; Solidity to corrosion is relatively poor; In addition, the quality of magnesium is softer, wear resistance also, these problems have all greatly limited the widespread use of magnesiumalloy.
And adopt emerging differential arc oxidization technique that the surface of magnesiumalloy is handled, to obtain the ceramic coating layer, the effective way that addresses the above problem beyond doubt.The present invention just is being based on above-mentioned consideration; Differential arc oxidization technique for magnesiumalloy has carried out careful deep research; Each treatment step and each processing parameter have all been carried out in large quantities, systematically studied; In the hope of obtaining to be suitable for most the microarc oxidation treatment process of magnesiumalloy, simultaneously, the inherent that overcomes existing arc differential oxide ceramic layer existence is because problems such as the compactness that cell texture caused, lack of homogeneitys.
Summary of the invention
The object of the present invention is to provide a kind of differential arc oxidation treatment method that is applicable to magnesium and alloy surface thereof, thereby obtain to have surface ceramic oxidation film layer suitable thickness, even compact.
For realizing above-mentioned purpose, the present invention adopts following technical scheme to be:
The differential arc oxidation treatment method of a kind of magnesium and alloy surface thereof is characterized in that comprising the steps:
The first, matrix metal is carried out sandblasting, remove surface and oil contaminant, adopt sand papering subsequently, adopt 500#-2000# polishing order from coarse to fine, until surperficial no marking;
The second, adopt basic soln to carry out dark skimming treatment, it is subsequent use to adopt zero(ppm) water to clean after the dark degreasing;
The 3rd, in alkaline electrolyte, carry out differential arc oxidation and handle, wherein adopt the method for boosted voltage gradually, final voltage is controlled at 300-370V, and current density is at 30mA/cm
2Below, the differential arc oxidation treatment time is greater than 20 minutes, and the temperature maintenance of electrolytic solution is less than 40 ℃;
The 4th, carry out warm air drying again after the metal after differential arc oxidation handled cleans with zero(ppm) water, thereby obtain final magnesium alloy product.
Preferably, it is the MB3 magnesiumalloy that described differential arc oxidation is handled what be directed against, MB3 magnesiumalloy light weight, good rigidly, has certain solidity to corrosion and dimensional stability, and mechanical properties such as shock resistance, wear-resisting, fade performance are all very excellent; Also have high heat conduction and conductivity in addition, nonmagnetic, shielding good and characteristics such as nontoxic easy recovery, be widely applicable a kind of in the magnesiumalloy.Yet very limited to its differential arc oxidation that carries out research at present, the present invention just is being based on the characteristics of MB3 magnesiumalloy its differential arc oxidation has been carried out detailed systematic research, to develop a kind of microarc oxidation treatment process that is fit to its use.
Preferably, comprising of the basic soln of described dark skimming treatment employing: the KOH of 130-200g/L, the NaOH of 130-200g/L, the two ratio is 1: 1, methoxyl group isopropylformic acid alkyl ester 15-20g/L, dimethyl-oxidation amine 35-40g/L.Adopt above-mentioned basic soln to carry out the degreasing effect excellence of dark skimming treatment, the ceramic oxide layer of gained is also more fine and close evenly.
Preferably, consisting of of the alkaline electrolyte of said differential arc oxidation processing: the KOH of 200-300g/L, the trisodium citrate of 25-30g/L; The sodium phosphate of 160-180g/L; The Sodium Fluoride of 50-70g/L, the matt salt of 20-30g/L, the sodium metaaluminate of 40-70g/L; The cerous nitrate of 1-5g/L with or Lanthanum trinitrate, surplus is a water.Above-mentioned alkaline electrolyte contains poisonous objectionable impurities hardly, and the electric conductivity of its concentration and electrolytic solution is moderate, long service life; Film forming speed and quality of forming film are good; After adopting above-mentioned alkaline electrolyte to carry out the differential arc oxidation processing, the ceramic coating layer of Mg alloy surface is evenly fine and close, and the aperture is tiny.
Preferably, when said differential arc oxidation was handled, final voltage was controlled at 320-340V, and current density is at 15-20mA/cm
2Below, the temperature maintenance of electrolytic solution is at 25-30 ℃, and the treatment time was controlled at 25-30 minute, in the differential arc oxidation treating processes, carried out induction stirring simultaneously, and stirring velocity is 300-400rpm.Adopt above-mentioned processing parameter to carry out differential arc oxidation and handle, not only effectively reduce energy consumption and pollution in the treating processes, on top, improved film forming efficiency simultaneously, guaranteed quality of forming film.
Preferably, after differential arc oxidation is handled, further comprise the sealing of hole post-processing step; Said sealing of hole aftertreatment is the magnesium alloy product after the differential arc oxidation processing to be immersed in the sodium silicate solution that configures be put in the encloses container, uses minipump to vacuumize, to 5mbar; Continue 30-40 minute; After the goods taking-up, hang in the drying oven, be cured.
Advantage of the present invention is: the differential arc oxidation of specific MB3 magnesiumalloy is handled carried out careful deep research; To such an extent as to each step and the details of handling aftertreatment from pre-treatment, differential arc oxidation all carried out a large amount of repeatedly grope research; Obtained the technology of the optimum of suitable MB3 magnesiumalloy; Under the prerequisite of guaranteed efficiency and quality of forming film, greatly reduce processing energy consumption and pollution.
Description of drawings
Fig. 1 is the Mg alloy surface microtexture pattern after surface treatment among the present invention;
Fig. 2 is the magnesiumalloy ceramic coating bed interface microtexture pattern after surface treatment among the present invention;
Fig. 3 is the chemical composition analysis of ceramic coating layer among the present invention.
Embodiment
Below, the embodiment of the optimum of summing up through the contriver is elaborated to the present invention.
The first, MB3 matrix magnesiumalloy is carried out sandblasting, remove surface and oil contaminant, adopt sand papering subsequently, adopt 500#-2000# polishing order from coarse to fine, until surperficial no marking;
The second, adopt basic soln to carry out dark skimming treatment, it is subsequent use to adopt zero(ppm) water to clean after the dark degreasing; Comprising of the basic soln that described dark skimming treatment is adopted: the KOH of 150g/L, the NaOH of 15g/L, the two ratio is 1: 1,18g/L methoxyl group isopropylformic acid alkyl ester, 35g/L dimethyl-oxidation amine;
The 3rd, in alkaline electrolyte, carry out differential arc oxidation and handle, wherein adopt the method for boosted voltage gradually, final voltage is controlled at 330V, and current density is at about 16mA/cm
2About, in 28 minutes differential arc oxidation treatment times, the temperature maintenance of electrolytic solution is at 27 ℃; Consisting of of the alkaline electrolyte that said differential arc oxidation is handled: the KOH of 240g/L, the trisodium citrate of 26g/L, the sodium phosphate of 170g/L; The Sodium Fluoride of 55g/L, the matt salt of 25g/L, the sodium metaaluminate of 50g/L; The cerous nitrate of 2g/L and/or Lanthanum trinitrate, surplus are water; In the differential arc oxidation treating processes, carry out induction stirring simultaneously, stirring velocity is 300rpm;
The 4th, the magnesium alloy product after differential arc oxidation handled is immersed in the sodium silicate solution that configures and is put in the encloses container, uses minipump to vacuumize, and to 5mbar, continues 35 minutes, after goods are taken out, hangs in the drying oven, is cured;
The 5th, carry out warm air drying again after the metal after differential arc oxidation handled cleans with zero(ppm) water, thereby obtain final magnesium alloy product.
Can know by Fig. 1-3, the magnesiumalloy after Microarc Oxidation Surface Treatment of the present invention, the ceramic coating layer even compact that its surface generates combines closely with magnesium alloy substrate, and thicknesses of layers reaches as high as about 97 μ m, and corrosion resistance nature improves greatly.
Claims (7)
1. the differential arc oxidation treatment method of magnesium and alloy surface thereof is characterized in that comprising the steps:
The first, matrix metal is carried out sandblasting, remove surface and oil contaminant, adopt sand papering subsequently, adopt 500#-2000# polishing order from coarse to fine, until surperficial no marking;
The second, adopt basic soln to carry out dark skimming treatment, it is subsequent use to adopt zero(ppm) water to clean after the dark degreasing;
The 3rd, in alkaline electrolyte, carry out differential arc oxidation and handle, wherein adopt the method for boosted voltage gradually, final voltage is controlled at 300-370V, and current density is at 30mA/cm
2Below, the differential arc oxidation treatment time is greater than 20 minutes, and the temperature maintenance of electrolytic solution is less than 40 ℃;
The 4th, carry out warm air drying again after the metal after differential arc oxidation handled cleans with zero(ppm) water, thereby obtain final magnesium alloy product.
2. the differential arc oxidation treatment method of magnesium as claimed in claim 1 and alloy surface thereof is characterized in that: it is the MB3 magnesiumalloy that described differential arc oxidation is handled what be directed against.
3. the differential arc oxidation treatment method of magnesium as claimed in claim 1 and alloy surface thereof; It is characterized in that: the comprising of the basic soln that described dark skimming treatment is adopted: the KOH of 130-200g/L, the NaOH of 130-200g/L; The two ratio is 1: 1; Methoxyl group isopropylformic acid alkyl ester 15-20g/L, dimethyl-oxidation amine 35-40g/L.
4. the differential arc oxidation treatment method of magnesium as claimed in claim 1 and alloy surface thereof is characterized in that: the consisting of of the alkaline electrolyte that said differential arc oxidation is handled: the KOH of 200-300g/L, the trisodium citrate of 25-30g/L; The sodium phosphate of 160-180g/L; The Sodium Fluoride of 50-70g/L, the matt salt of 20-30g/L, the sodium metaaluminate of 40-70g/L; The cerous nitrate of 1-5g/L with or Lanthanum trinitrate, surplus is a water.
5. the differential arc oxidation treatment method of magnesium as claimed in claim 1 and alloy surface thereof, it is characterized in that: when said differential arc oxidation was handled, final voltage was controlled at 320-340V; Current density is below 15-20mA/cm2; The temperature maintenance of electrolytic solution is at 25-30 ℃, and the treatment time was controlled at 25-30 minute, in the differential arc oxidation treating processes; Carry out induction stirring simultaneously, stirring velocity is 300-400rpm.
6. the differential arc oxidation treatment method of magnesium as claimed in claim 1 and alloy surface thereof is characterized in that: after differential arc oxidation is handled, further comprise the sealing of hole post-processing step; Said sealing of hole aftertreatment is the magnesium alloy product after the differential arc oxidation processing to be immersed in the sodium silicate solution that configures be put in the encloses container, uses minipump to vacuumize, to 5mbar; Continue 30-40 minute; After the goods taking-up, hang in the drying oven, be cured.
7. prepared magnesium alloy product that obtains of differential arc oxidation treatment method that utilizes described magnesium of claim 1-6 and alloy surface thereof.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103147109A (en) * | 2013-03-26 | 2013-06-12 | 西北工业大学 | Method for sealing aluminum alloy micro-arc oxidation film layer |
| CN103421997A (en) * | 2013-08-30 | 2013-12-04 | 山东大学 | Degradable Mg-Zn-Si-Ca magnesium-based biological ceramic composite implant material and preparation method thereof |
| CN103469280A (en) * | 2013-09-24 | 2013-12-25 | 重庆研镁科技有限公司 | Magnesium alloy micro-arc oxidation electrolyte and technology for carrying out black ceramic processing on magnesium alloy surface by using electrolyte |
| CN103526251A (en) * | 2013-10-15 | 2014-01-22 | 北京星航机电装备有限公司 | Method for preparing micro-arc oxidation film with photocatalysis function |
| CN104131324A (en) * | 2014-08-12 | 2014-11-05 | 广西玉柴机器股份有限公司 | Aluminum alloy piston for internal combustion engine |
| CN104651908A (en) * | 2013-11-25 | 2015-05-27 | 中国兵器科学研究院宁波分院 | Preparation method and hole sealing method of magnesium alloy surface ceramic coating |
| CN106112818A (en) * | 2016-06-29 | 2016-11-16 | 重庆铁马工业集团有限公司 | A kind of metallic element decontamination process |
| CN106521602A (en) * | 2016-10-25 | 2017-03-22 | 中国兵器科学研究院宁波分院 | Preparing method of magnesium alloy surface composite ceramic film layer |
| CN107779930A (en) * | 2016-08-31 | 2018-03-09 | 昆山汉鼎精密金属有限公司 | The surface decorating method and its products formed of magnesium alloy encapsulated products |
| CN107829125A (en) * | 2016-11-11 | 2018-03-23 | 深圳瑞之谷医疗科技有限公司 | Substrate, heating plate, humidification machine and its processing method are used in one kind heating |
| CN107904647A (en) * | 2017-11-30 | 2018-04-13 | 北京石油化工学院 | A kind of Micro-arc Oxidized Ceramic Coatings on Magnesium Alloy hole sealing agent and method for sealing |
| CN112064091A (en) * | 2020-08-21 | 2020-12-11 | 广东机电职业技术学院 | Hole sealing method for micro-arc oxidation film layer |
| CN112410848A (en) * | 2019-08-23 | 2021-02-26 | 华孚精密科技(马鞍山)有限公司 | Method for preventing magnesium piece from being polluted during encapsulation |
| CN115478269A (en) * | 2022-10-11 | 2022-12-16 | 山西聚星辰新材料科技有限公司 | Preparation method of flexible aluminum-based ceramic insulating foil |
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Cited By (17)
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| CN103147109A (en) * | 2013-03-26 | 2013-06-12 | 西北工业大学 | Method for sealing aluminum alloy micro-arc oxidation film layer |
| CN103421997A (en) * | 2013-08-30 | 2013-12-04 | 山东大学 | Degradable Mg-Zn-Si-Ca magnesium-based biological ceramic composite implant material and preparation method thereof |
| CN103421997B (en) * | 2013-08-30 | 2015-12-02 | 山东大学 | A kind of degradable Mg-Zn-Si-Ca magnesium base bioceramic compound implant material and preparation method thereof |
| CN103469280A (en) * | 2013-09-24 | 2013-12-25 | 重庆研镁科技有限公司 | Magnesium alloy micro-arc oxidation electrolyte and technology for carrying out black ceramic processing on magnesium alloy surface by using electrolyte |
| CN103526251A (en) * | 2013-10-15 | 2014-01-22 | 北京星航机电装备有限公司 | Method for preparing micro-arc oxidation film with photocatalysis function |
| CN104651908A (en) * | 2013-11-25 | 2015-05-27 | 中国兵器科学研究院宁波分院 | Preparation method and hole sealing method of magnesium alloy surface ceramic coating |
| CN104131324A (en) * | 2014-08-12 | 2014-11-05 | 广西玉柴机器股份有限公司 | Aluminum alloy piston for internal combustion engine |
| CN106112818A (en) * | 2016-06-29 | 2016-11-16 | 重庆铁马工业集团有限公司 | A kind of metallic element decontamination process |
| CN107779930A (en) * | 2016-08-31 | 2018-03-09 | 昆山汉鼎精密金属有限公司 | The surface decorating method and its products formed of magnesium alloy encapsulated products |
| CN106521602A (en) * | 2016-10-25 | 2017-03-22 | 中国兵器科学研究院宁波分院 | Preparing method of magnesium alloy surface composite ceramic film layer |
| CN106521602B (en) * | 2016-10-25 | 2018-11-20 | 中国兵器科学研究院宁波分院 | The preparation method of Mg alloy surface composite ceramics film layer |
| CN107829125A (en) * | 2016-11-11 | 2018-03-23 | 深圳瑞之谷医疗科技有限公司 | Substrate, heating plate, humidification machine and its processing method are used in one kind heating |
| CN107904647A (en) * | 2017-11-30 | 2018-04-13 | 北京石油化工学院 | A kind of Micro-arc Oxidized Ceramic Coatings on Magnesium Alloy hole sealing agent and method for sealing |
| CN112410848A (en) * | 2019-08-23 | 2021-02-26 | 华孚精密科技(马鞍山)有限公司 | Method for preventing magnesium piece from being polluted during encapsulation |
| CN112064091A (en) * | 2020-08-21 | 2020-12-11 | 广东机电职业技术学院 | Hole sealing method for micro-arc oxidation film layer |
| CN112064091B (en) * | 2020-08-21 | 2021-10-26 | 广东机电职业技术学院 | Hole sealing method for micro-arc oxidation film layer |
| CN115478269A (en) * | 2022-10-11 | 2022-12-16 | 山西聚星辰新材料科技有限公司 | Preparation method of flexible aluminum-based ceramic insulating foil |
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