CN1405361A - Magnesium alloy ultrasonic anode oxidation method - Google Patents
Magnesium alloy ultrasonic anode oxidation method Download PDFInfo
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- CN1405361A CN1405361A CN 02137751 CN02137751A CN1405361A CN 1405361 A CN1405361 A CN 1405361A CN 02137751 CN02137751 CN 02137751 CN 02137751 A CN02137751 A CN 02137751A CN 1405361 A CN1405361 A CN 1405361A
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- magnesium alloy
- ultrasonic
- anode oxidation
- oxidation method
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Abstract
The invention is an Mg-alloy ultrasonic anode-oxidizing method. It adds stabilizing agent to existing electrolyte and during the oxidizing course, exerts ultrasonic field used to produce OH-1 and H2O2, and utilizes ultrasonic to raise reacting speed and provide atom O for the oxidizing reaction. After alkali-washing and acid-washing, the Mg-alloy workpiece is placed in the electrobath.
Description
Technical field:
The present invention relates to a kind of magnesium alloy ultrasonic anode oxidation method, is a kind of anode oxidation method that produces oxide ceramic coating on magnesium alloy, belongs to technical field of magnesium alloy surface treatment.
Background technology:
In numerous surface treatment method of Mg alloy, anode oxidation method be performance and effect better and have one of important method of the market competitiveness.Traditional anodic oxidation is a kind of electrochemistry oxygen metallization processes.Needs are carried out the anode of anodised workpiece connection direct supply and make anode, another kind of nullvalent metal (for example, stainless steel) negative terminal that connects direct current (D.C.) power supply is done in the suitable electrolytic solution of negative electrode immersion, when electric current passes through electrolyte solution, the negatively charged ions anode moves and at anode discharge, this process is followed the generation of atomic oxygen and formed oxide coating.Anode oxidation process can adopt direct current (D.C.) now, exchange (A.C.); Perhaps stack of AC and DC (A.C+D.C.) and pulsed current (P.C.).When the curtage that is applied during greater than certain value, on anodized workpiece, will produce spark (" spark ") or little electric arc (" micro arc "), therefore, people are called differential arc oxidation (" microarc oxidation ") or micro-plasma oxidation (" microplasma oxidation ") with anodic oxidation (anodizing) again.Only important reaction is to produce hydrogen on negative electrode.Metal anode is consumed and changes into a kind of oxide coating of self.This coating begins to form attached on the metal from metal one side near solution.Metal ion in the oxide ceramic layer results from metal, and oxygen results from the anodic reaction in the Water-Electrolyte solution.The plasma temperature that measuring produced is about 7000 ℃, and under this plasma body temperature, oxide ceramics is liquid.On the one side near metal, the time that produces plasma body is enough to allow the fused oxide ceramics produce suitably contraction, thereby forms a kind of sintered ceramic oxide layer with hole.Near one side of electrolyte solution, the fused oxide ceramics is cooled off rapidly by electrolyte solution, just at escaping gas, especially oxygen and water vapor, make the oxide ceramic layer of formation have by kapillary link to each other mesh-structured.For example, the pore diameter of aluminium alloy anode oxide coating adopts scanning electron microscope to be measured as 0.1um～30um (Wirtz, G.P., et al., Materials and Manufacturing Proceees, 1991, " Ceramic Coatings by anodic SparkDeposition " 6 (1): 87-115).
Existing anodic oxidation of magnetism alloy method adopts strong oxidizer, superoxide usually or change into the material of superoxide (e.g.Canadian Patent No.568,653) during anodic polarization.It is generally acknowledged, oxidation and the Sauerstoffatom that in the superoxide dissociation processes, produces, and subsequently in the hole of magnesium alloy insulating coating, the Sauerstoffatom that produces when recombinating under high current density is relevant.When adopting such as the such strong oxidizer of chromic salt, vanadate and permanganate, no matter be the reduction reaction that is present in the element in the oxygenant with highest oxidation state, still reoxidizing reaction and all will produce atomic oxygen subsequently.When oxygenant that adopts in the anodic oxidation of magnetism alloy process or superoxide contain transition element such as chromium, vanadium, manganese; the compound of these transition element can produce obvious color in the supercoat of Mg alloy surface, the painted or reduction coating performance of influence coating subsequently.Although now occurred not containing the anodic oxidation of magnetism alloy technology of above-mentioned transition element, but, the pore diameter of its coating, the speed of growth of coating and coating smooth finish are similar to the aluminium alloy anode oxide coating, depend primarily on the prescription and the electrical parameter of used solution.
Summary of the invention:
The objective of the invention is at the deficiencies in the prior art, a kind of magnesium alloy ultrasonic anode oxidation method is provided, except trying every possible means to improve the performance of anodic oxidation of magnetism alloy coating in prescription and electrical parameter aspect from solution, the method of further seeking other is improved the performance of magnesium alloy, to reduce the pore diameter of anodic oxidation of magnetism alloy coating, improve the speed of growth and the coating smooth finish of anodic oxidation of magnetism alloy coating, and then improve the corrosion resisting property of magnesium alloy.
For realizing such purpose, in the technical scheme of the present invention, in the electrolytic solution that existing anodic oxidation of magnetism alloy method adopts, add stablizer, and in the magnesium alloy ultrasonic anode oxidation process, apply ultrasonic field, utilize ultrasonic wave to improve speed of response, and provide required atomic oxygen for oxidizing reaction.Pending magnesium alloy workpiece is put into electrolyzer again and is carried out ultrasonic anode oxidation after alkali cleaning, pickling process.
Method of the present invention comprises following concrete steps:
1, pending magnesium alloy workpiece is carried out washing again after the alkali cleaning earlier in basic solution.
Basic solution can be used the conventional basic solution of using in the prior art.
The present invention is preferably by sodium hydroxide 40～60g/l, sodium phosphate 5～15g/l, the basic solution that artificial soap lye wetting agent 20ml/l forms.
2, magnesium alloy workpiece is carried out washing after the pickling in acidic solution again.
Acidic solution can be used the conventional acidic solution of using in the prior art.
The present invention is preferably by phosphoric acid (85%) 250～450ml/l, sulfuric acid (98%) 12～20ml/l, the acidic solution that water 550～650ml/l forms.
3, magnesium alloy workpiece is put into electrolyzer, in applying the electrolytic solution of ultrasonic field, carry out ultrasonic anode oxidation.
Magnesium alloy ultrasonic anode oxidation adopts the related process parameter of the effective anodic oxidation of magnetism alloy method of practical application, for example, and solution formula, solution pH value, electrical parameter etc.In electrolytic solution, add 260～460g/l stablizer on this basis, for example, ethylene glycol, glycerine, urea, hexamethylenetetramine, hexamethylene diamine etc.In used electrolyte solution, apply the ultrasonic field that the ultrasonic frequency scope is 25～600KHz, preferential range of choice is 80～300KHz.In the oxidation that begins to switch on, start the ultrasonic field that is applied.
The present invention can adopt direct current (D.C.), exchange the stack (D.C.+P.C.) of stack (A.C+D.C.), pulsed current (P.C.) and the direct current and the pulse of (A.C.) or AC and DC.
The present invention has applied ultrasonic field in anode oxidation process, in the magnesium alloy ultrasonic anode oxidation process, ultrasonic field can play the effect of stirred solution, reduces the concentration gradient at metal/gas/electrolyte solution phase interface place, increase ion diffusion speed, improve speed of response.Simultaneously, in the magnesium alloy ultrasound anode oxidation process, ultrasonic field can play and produce OH
-1Ion and oxydol H
2O
2Effect, for anodic oxidation reactions provides required atomic oxygen.
Magnesium alloy ultrasonic anode oxidation method of the present invention can reduce the pore diameter of anodized coating, improves the speed of growth and the coating smooth finish of anodic oxidation of magnetism alloy coating, and then has improved the corrosion resisting property of magnesium alloy.
The present invention is suitable for the diecast magnesium alloy of the pure magnesium and the following trade mark: AS41; AM60, AZ61, AZ81, AZ91, AZ92, HK31, QE22, ZE41, ZH62, ZK51, ZK61, EZ33, the wrought magnesium alloy of the HZ32 and the following trade mark: AZ31, AZ61, AZ80, M1, ZK60, ZK40.Also be suitable for AlSi5Mg; AlSi8C3; AlMgSi; Aluminium alloys such as AlMg1.
Description of drawings:
Fig. 1 is the ultrasonic field applying method synoptic diagram of anodic oxidation of magnetism alloy of the present invention.
As shown in the figure, electrolytic solution 2 is arranged in electrolyzer 1, be placed on the positive and negative electrode that two electrodes 4 in the electrolytic solution 2 connect power supply respectively, the ultrasonic wave 3 that ultrasonic generator sends is applied in the electrolytic solution.
Embodiment:
Below in conjunction with drawings and Examples technical scheme of the present invention is further described
Embodiment 1:
Earlier magnesium alloy is carried out alkali cleaning in the alkaline solution of following composition: in following acid solution, carry out pickling after the NaOH 50g/l sodium phosphate 10g/l wetting agent 1g/l washing: after phosphoric acid (85%) 380ml/l sulfuric acid (98%) the 16ml/l water 600ml/l washing, in the electrolyte solution of following composition, carry out anodic oxidation: hydrofluoric acid (HF) 30g/l phosphoric acid (H3PO
4) 60g/l boric acid (H
3PO
3) 70g/l
Present embodiment adds 100g/l hexamethylenetetramine stablizer in anodic oxidation solution; It is 1.4A/dm that current density is adopted in anodic oxidation
2Direct current to be superimposed with watt current density be 0.3A/dm
2, frequency is the alternating-current of 50Hz; The setting end voltage is 240V; In electrolyte solution, apply the ultrasonic field that frequency is 40Hz; Anodic oxidation continues 15min..The pore diameter of resulting anodized coating reduces when not applying ultrasonic field over half, and coat-thickness is the 20um when not adding ultrasonic field also.
Embodiment 2:
Adopt the solution of embodiment 1 to carry out alkali cleaning and pickling in the AZ91 magnesium alloy.In following electrolyte solution, carry out anodic oxidation then.(KF, 40%) 28g/l (K
3PO
4) 58g/l (K
3BO
3) 35g/l hexamethylenetetramine 360g/l
Use NH
4OH (25%) regulates pH value to 7.3.The employing current density is 1.4A/dm
2Direct current; Final voltage is 325V; Solution temperature is 15 ℃, and added ultrasonic frequency is 25KHz, and the treatment time is 15min., and the pore diameter of resulting anodized coating reduces when not applying ultrasonic field over half, and coat-thickness is the 21um when not adding ultrasonic field also.
Embodiment 3:
Adopt the solution of embodiment 1 to carry out alkali cleaning and pickling in the AZ91 magnesium alloy.In following electrolyte solution, carry out anodic oxidation then.K
3SiO
3(30Be’) 75mlNaOH 25gHF.H
2O(10％conc.) 10mlH
2O 1L
The employing current density is 1.4A/dm
2Direct current; Final voltage is 300V; Solution temperature is 20-40 ℃, and added ultrasonic frequency is 25KHz, and the treatment time is 15min., and the pore diameter of resulting anodized coating reduces when not applying ultrasonic field over half, the coat-thickness of coat-thickness when not adding ultrasonic field.
Embodiment 4:
Adopt the solution of example one to carry out alkali cleaning and pickling in the AZ91 magnesium alloy.In following electrolyte solution, carry out anodic oxidation then.Na
3SiO
3(25Be’) 50mlNaOH 30gH
2SiF
6 7gH
2O 1L
The employing current density is 1.4A/dm
2Direct current; Final voltage is 300V; Solution temperature is 20-40 ℃, and added ultrasonic frequency is 250KHz, and the treatment time is 15min., and the pore diameter of resulting anodized coating reduces when not applying ultrasonic field over half, the coat-thickness of coat-thickness when not adding ultrasonic field.
Claims (6)
1, a kind of magnesium alloy ultrasonic anode oxidation method is characterized in that comprising following concrete steps:
1) pending magnesium alloy workpiece is carried out washing again after the alkali cleaning earlier in basic solution;
2) magnesium alloy workpiece is carried out washing after the pickling in acidic solution again;
3) magnesium alloy workpiece is put into electrolyzer, in electrolytic solution, add 260～460g/l stablizer, apply the ultrasonic field that the ultrasonic frequency scope is 25～600KHz, in the oxidation that begins to switch on, start the ultrasonic field that is applied, carry out ultrasonic anode oxidation.
2,, it is characterized in that the preferential 80～300KHz of selection of the ultrasonic frequency scope that applies as the said magnesium alloy ultrasonic anode oxidation method of claim 1.
3,, it is characterized in that the stablizer that adds is an ethylene glycol in electrolytic solution, glycerine, urea, hexamethylenetetramine, hexamethylene diamine as the said magnesium alloy ultrasonic anode oxidation method of claim 1.
4,, it is characterized in that reacting power supply and adopt direct current, interchange, stack, pulsed current or the direct current of AC and DC and the stack of pulse as the said magnesium alloy ultrasonic anode oxidation method of claim 1.
5, as the said magnesium alloy ultrasonic anode oxidation method of claim 1, it is characterized in that basic solution by sodium hydroxide 40～60g/l, sodium phosphate 5～15g/l, artificial soap lye wetting agent 20ml/l forms.
6, as the said magnesium alloy ultrasonic anode oxidation method of claim 1, it is characterized in that acidic solution by phosphoric acid (85%) 250～450ml/l, sulfuric acid (98%) 12～20ml/l, water 550～650ml/l forms.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02137751 CN1405361A (en) | 2002-10-31 | 2002-10-31 | Magnesium alloy ultrasonic anode oxidation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02137751 CN1405361A (en) | 2002-10-31 | 2002-10-31 | Magnesium alloy ultrasonic anode oxidation method |
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|---|---|
| CN1405361A true CN1405361A (en) | 2003-03-26 |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100336937C (en) * | 2004-12-28 | 2007-09-12 | 哈尔滨工业大学 | Composite processing method for increasing corrosion resistance for magnesium alloys |
| CN100381615C (en) * | 2004-11-04 | 2008-04-16 | 上海交通大学 | Two-step pigmenting method for green oxidation film layer on magnesium alloy surface |
| CN101928976A (en) * | 2010-08-20 | 2010-12-29 | 上海交通大学 | Ion exchange membrane electrolytic bath for anodic oxidation of magnetism alloy and oxidation method thereof |
| CN102140664A (en) * | 2011-04-22 | 2011-08-03 | 北京交通大学 | Surface thin layer thickness equalizing method of AZ91 magnesium alloy |
| CN102140665A (en) * | 2011-04-22 | 2011-08-03 | 北京交通大学 | AM60 magnesium alloy surface thin layer thickness uniformity treatment method |
| CN101186989B (en) * | 2007-12-10 | 2011-08-31 | 南昌大学 | Method for preparing AZ61 magnesium alloy half-solid blank using ultrasonic wave |
| CN102181909A (en) * | 2011-04-22 | 2011-09-14 | 北京交通大学 | Thin layer treatment method for surface of AZ91 magnesium alloy |
| CN102181910A (en) * | 2011-04-22 | 2011-09-14 | 北京交通大学 | Thin-layer thickness uniform treatment method for surface of MB8 magnesium alloy |
| CN102181906A (en) * | 2011-04-22 | 2011-09-14 | 北京交通大学 | Method for processing thin layer on surface of MB8 magnesium alloy |
| CN102181908A (en) * | 2011-04-22 | 2011-09-14 | 北京交通大学 | Method for treating thick protective layer on surface of AZ91 magnesium alloy |
| CN102181907A (en) * | 2011-04-22 | 2011-09-14 | 北京交通大学 | Method for treating thin layer on surface of AM60 magnesium alloy |
| CN101899700B (en) * | 2009-05-25 | 2011-12-07 | 佳木斯大学 | Preparation method of ultrasonic microarc oxidation silver-carrying antibiotic bioactive coating on magnesium and titanium surface |
| CN102424998A (en) * | 2011-11-27 | 2012-04-25 | 西北有色金属研究院 | Method for reducing surface roughness of micro arc oxidized ceramic layer |
| CN103014802A (en) * | 2012-12-20 | 2013-04-03 | 广州中国科学院先进技术研究所 | Ultrasonic micro-arc oxidation device and ultrasonic micro-arc oxidation method thereof |
| CN105177668A (en) * | 2012-11-07 | 2015-12-23 | 马鞍山市天睿实业有限公司 | Anode polarization and coloration treatment method of aluminum alloy extinguisher valve body |
| CN108588790A (en) * | 2017-11-24 | 2018-09-28 | 广灵县尚镁科技有限公司 | The method for oxidation of magnesium and magnesium alloy |
| CN108745826A (en) * | 2017-11-24 | 2018-11-06 | 广灵县尚镁科技有限公司 | Magnesium and magnesium alloy hub coating process |
| CN111778536A (en) * | 2020-07-22 | 2020-10-16 | 中山市三美高新材料技术有限公司 | Aluminum alloy surface compact oxidation process under constant ion gradient |
-
2002
- 2002-10-31 CN CN 02137751 patent/CN1405361A/en active Pending
Cited By (27)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100381615C (en) * | 2004-11-04 | 2008-04-16 | 上海交通大学 | Two-step pigmenting method for green oxidation film layer on magnesium alloy surface |
| CN100336937C (en) * | 2004-12-28 | 2007-09-12 | 哈尔滨工业大学 | Composite processing method for increasing corrosion resistance for magnesium alloys |
| CN101186989B (en) * | 2007-12-10 | 2011-08-31 | 南昌大学 | Method for preparing AZ61 magnesium alloy half-solid blank using ultrasonic wave |
| CN101899700B (en) * | 2009-05-25 | 2011-12-07 | 佳木斯大学 | Preparation method of ultrasonic microarc oxidation silver-carrying antibiotic bioactive coating on magnesium and titanium surface |
| CN101928976A (en) * | 2010-08-20 | 2010-12-29 | 上海交通大学 | Ion exchange membrane electrolytic bath for anodic oxidation of magnetism alloy and oxidation method thereof |
| CN101928976B (en) * | 2010-08-20 | 2012-05-30 | 上海交通大学 | Ion exchange membrane electrolytic bath for anodic oxidation of magnetism alloy and oxidation method thereof |
| CN102181908B (en) * | 2011-04-22 | 2012-08-08 | 北京交通大学 | Method for treating thick protective layer on surface of AZ91 magnesium alloy |
| CN102140664A (en) * | 2011-04-22 | 2011-08-03 | 北京交通大学 | Surface thin layer thickness equalizing method of AZ91 magnesium alloy |
| CN102181906A (en) * | 2011-04-22 | 2011-09-14 | 北京交通大学 | Method for processing thin layer on surface of MB8 magnesium alloy |
| CN102181908A (en) * | 2011-04-22 | 2011-09-14 | 北京交通大学 | Method for treating thick protective layer on surface of AZ91 magnesium alloy |
| CN102181907A (en) * | 2011-04-22 | 2011-09-14 | 北京交通大学 | Method for treating thin layer on surface of AM60 magnesium alloy |
| CN102181909A (en) * | 2011-04-22 | 2011-09-14 | 北京交通大学 | Thin layer treatment method for surface of AZ91 magnesium alloy |
| CN102181910A (en) * | 2011-04-22 | 2011-09-14 | 北京交通大学 | Thin-layer thickness uniform treatment method for surface of MB8 magnesium alloy |
| CN102140665A (en) * | 2011-04-22 | 2011-08-03 | 北京交通大学 | AM60 magnesium alloy surface thin layer thickness uniformity treatment method |
| CN102140664B (en) * | 2011-04-22 | 2012-07-11 | 北京交通大学 | Surface thin layer thickness equalizing method of AZ91 magnesium alloy |
| CN102181910B (en) * | 2011-04-22 | 2012-07-11 | 北京交通大学 | Thin-layer thickness uniform treatment method for surface of MB8 magnesium alloy |
| CN102181909B (en) * | 2011-04-22 | 2012-07-11 | 北京交通大学 | Thin layer treatment method for surface of AZ91 magnesium alloy |
| CN102181906B (en) * | 2011-04-22 | 2012-08-08 | 北京交通大学 | Method for processing thin layer on surface of MB8 magnesium alloy |
| CN102424998A (en) * | 2011-11-27 | 2012-04-25 | 西北有色金属研究院 | Method for reducing surface roughness of micro arc oxidized ceramic layer |
| CN105177668A (en) * | 2012-11-07 | 2015-12-23 | 马鞍山市天睿实业有限公司 | Anode polarization and coloration treatment method of aluminum alloy extinguisher valve body |
| CN105177668B (en) * | 2012-11-07 | 2018-05-29 | 马鞍山市天睿实业有限公司 | A kind of anode polarization of Aluminium alloy fire extinguisher valve body and coloring treatment process |
| CN103014802A (en) * | 2012-12-20 | 2013-04-03 | 广州中国科学院先进技术研究所 | Ultrasonic micro-arc oxidation device and ultrasonic micro-arc oxidation method thereof |
| CN103014802B (en) * | 2012-12-20 | 2016-02-03 | 陈贤帅 | A kind of ultrasonic microarc oxidation device and ultrasonic microarc oxidation method thereof |
| CN108588790A (en) * | 2017-11-24 | 2018-09-28 | 广灵县尚镁科技有限公司 | The method for oxidation of magnesium and magnesium alloy |
| CN108745826A (en) * | 2017-11-24 | 2018-11-06 | 广灵县尚镁科技有限公司 | Magnesium and magnesium alloy hub coating process |
| CN111778536A (en) * | 2020-07-22 | 2020-10-16 | 中山市三美高新材料技术有限公司 | Aluminum alloy surface compact oxidation process under constant ion gradient |
| CN111778536B (en) * | 2020-07-22 | 2022-05-13 | 中山市三美高新材料技术有限公司 | Aluminum alloy surface compact oxidation process under constant ion gradient |
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