CN100425740C - Anode oxidating electrolysing liquid under inhibiting arc state of magnesium alloy and process for anode oxidating - Google Patents
Anode oxidating electrolysing liquid under inhibiting arc state of magnesium alloy and process for anode oxidating Download PDFInfo
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- CN100425740C CN100425740C CNB200510032436XA CN200510032436A CN100425740C CN 100425740 C CN100425740 C CN 100425740C CN B200510032436X A CNB200510032436X A CN B200510032436XA CN 200510032436 A CN200510032436 A CN 200510032436A CN 100425740 C CN100425740 C CN 100425740C
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Abstract
The present invention relates to the anode oxidizing electrolyte of magnesium alloy in an arc inhibiting state and a method for anode oxidation. Water is used as a solvent for the anode oxidizing electrolyte and the anode oxidizing electrolyte has the components of organic amine of 75 to 150 g/L, inorganic phosphatic and boron compounds of 6 to 12 g/L, organic carboxylate of 1 to 4 g/L, fluoride of 2 to 5 g/L and metal oxoacid salt of 4 to 10 g/L. The anode oxidizing method has the obvious characteristic that the surface of a magnesium alloy anode does not generate spark discharge under the conditions of high oxidation voltage and a high oxidation peak current parameter. The electrolyzing technology has the advantages of low solution toxicity, fast film forming, simple and safe technological operation, low energy consumption, etc. Anode oxide films obtained by the method have the advantages of smoothness, compactness and high hardness, and can obviously enhance the corrosion resisting property of magnesium and magnesium alloy. The film layer can be singly used as a protective layer for magnesium alloy and can also be used as a substrate for other coating layers.
Description
Technical field:
The present invention relates to a kind of magnesium alloy materials at the anodic oxidation electrolyte and the anode oxidation method that press down under the arcuation attitude.
Technical background:
Magnesium alloy materials is because characteristics such as its excellent physics, chemistry, mechanical property and light specific gravity, specific tenacity and specific rigidity height, heat-conductivity conducting performance be good and in space flight and aviation, electronics, and communication, the application in fields such as automobile making is constantly developed.Especially in recent ten years along with the developing rapidly of automotive industry and electronic industry, a large amount of magnesium alloy component are used to replace plastics even steel-iron components.But the chemical stability of magnesium is low, the standard equilibrium potential very negative (2.34V), solidity to corrosion is relatively poor, has restricted it and has brought into play due advantage, and therefore, the solidity to corrosion that strengthens magnesium has important practical significance.
Because the solidity to corrosion of magnesium alloy materials is poor, therefore must carry out the requirement that surface treatment could be satisfied environment for use to it before using, in numerous surface treatment method of Mg alloy, anode oxidation method is that performance and effect better have one of important method of the market competitiveness, magnesium and alloy thereof are after electrochemical anodic oxidation is handled, its surface can form one deck and the metallic matrix bonding force is strong, electrical insulating property good, and has good heat shock resistance, wear-resistant, corrosion resistant surface conversion coating.
Traditional anodic oxidation of magnetism alloy technology is just possible oxidation filming under higher voltage and electric current only, when the voltage that is applied or electric current during greater than certain value, on oxidized workpiece, will produce spark discharge or little electric arc, therefore people are called anodic oxidation differential arc oxidation or micro-plasma oxidation again, the plasma temperature that measuring is produced in the differential arc oxidation of magnesium alloy is approximately 7000 ℃, under this plasma body temperature, oxide ceramics is liquid, on one side near metal, the time that produces plasma body is enough to allow the fused oxide ceramics produce suitable contraction, thereby produces a kind of sintered ceramic oxide layer with hole.On the one side near electrolyte solution, the fused oxide ceramics is cooled off rapidly by electrolyte solution.Because film surface escaping gas, especially oxygen and water vapor, make the oxide ceramic layer of formation have by kapillary link to each other mesh-structured.
Because mostly be accompanied by intensive spark or little arc-over in the anodic oxidation of magnetism alloy process, temperature is too high, and discharges a large amount of heat, brings hidden danger to safety in production, and needs large-scale cooling apparatus in commercial production, has improved production cost; Simultaneously, the magnesium oxide film of anode spark or little arc-over formation of deposits is rough porous often, influences the use of material.
Summary of the invention:
At the deficiencies in the prior art, purpose of the present invention has aimed to provide a kind of than less energy-consumption, under the state of fast filming, makes the magnesium alloy materials surface generate the anodic oxidation electrolyte of the oxidation film layer of one deck high rigidity, high abrasion and high anti-corrosion.
Another object of the present invention aims to provide the above-mentioned anodic oxidation electrolyte of a kind of use, in the anodic oxidation of magnetism alloy method that presses down under the arc discharge state.
The objective of the invention is to realize by following manner:
Bath composition of the present invention comprises 75～150g/L organic amine, inorganic phosphorated, the boron compound of 6～12g/L, 1～4g/L organic carboxylate, 2～5g/L fluorochemical; Wherein said electrolyte solution all is solvent with water.Bath composition also comprises 4～10g/L metal oxygen-containing hydrochlorate.
Organic amine is saturated fatty amine, contain two keys or triple-linked unsaturated fatty acids amine, in the hydramine two kinds, and the former number of described organic amine carbon is 1～10.
Described inorganic phosphorated, boron compound is phosphorous or contains potassium, sodium or the ammonium salt of boron; Can be primary ammonium phosphate, potassium primary phosphate, Secondary ammonium phosphate, dipotassium hydrogen phosphate, sodium polyphosphate, trisodium phosphate, sodium tetraborate, one or more in the sodium metaborate.
Described organic carboxylate can be sodium acetate, Sodium Propionate, Sodium Benzoate, sebacic acid sodium, hexanodioic acid sodium, one or more in the para-phthalic sodium.
Described fluorochemical can be Potassium monofluoride, Sodium Fluoride, ammonium bifluoride, Sodium tetrafluoroborate, one or more in the Sodium Silicofluoride.
Described metal oxygen-containing hydrochlorate can be sodium aluminate, sodium wolframate, Sodium orthomolybdate, one or more in the sodium metavanadate.
Another object of the present invention realizes by following manner:
Magnesium alloy materials as anode, is placed composite electrolytic solution, with stainless steel as negative electrode, adopt the silicon rectifier direct supply, control voltage was raised to required voltage 80V～160V from 0V in 30 seconds, and remained unchanged, until end, the treatment time is controlled to be 5～15 minutes.
Oxidation current raises with voltage and increases, and reaches peak current density 10～20A/dm
2After, peak point current was kept 5～15 seconds, descended rapidly, reached 2A/dm at last
2, film forming finishes; Oxidation is carried out under no arc light condition all the time; Power supply can adopt the silicon rectifier direct supply, and described voltage can be between 80V～160V.
Peak current density 10～20A/dm
2, continue 5～15 seconds; Electrolyte temperature can be 10～80 ℃ of range.When current density is finally reduced to 2A/dm
2, then film forming finishes.
The control anode oxidation process is under the no arc light condition all the time, adopts the silicon rectifier direct supply, makes the magnesium alloy materials surface generate the oxidation film layer of one deck high rigidity, high abrasion and high anti-corrosion fast, and its Production Flow Chart is:
Degreasing → washing → but electrochemical anodic oxidation film forming → washing → oven dry under the arc condition.
What anodic oxidation electrolyte of the present invention was the contriver in repetition test repeatedly is basic resulting, in electrolytic solution, the organic assembling of organic amine and other component can suppress magnesium alloy materials effectively and produce spark discharge or little electric arc in anode oxidation process, and the anodic oxidation of magnesium alloy is carried out under the state of relatively placidity; Simultaneously, organic amine can also obviously improve anodised film forming speed, improves the compactness of rete, reduces porosity, makes the oxide film of magnesium alloy show as brighter and cleaner on macroscopic view.Anodic oxidation electrolyte of the application of the invention and technology compared with prior art have following advantage:
1. the difference of the present invention and plasma intensified electrochemical surface potteryization method maximum just is can not discharge by flashing in the film process, production safety, noise is little, and nonirritant gaseous volatilization, be fit to the safety in production standard, the film forming required voltage is lower, and current density descends along with film forming carrying out, average current density is low, less energy consumption.
2. electrolytic solution of the present invention is for adopting the novel anodizing composite electrolytic solution of development voluntarily, and its oxidation electrolyte concentration is lower, and toxicity, corrodibility are little.
3. use the magnesium alloy materials that the present invention relates to and press down anode oxidation process under the arcuation attitude, can form specious brown or the uniform and smooth rete of silver gray at Mg alloy surface, this rete has higher hardness, good wear resistance and good solidity to corrosion, and metallic matrix is had good barrier propterty.And this rete has vesicular structure, can provide good substrate as paint, coating etc. for further applying organic film.
4. anode oxidation process of the present invention is simple, and it is constant that electrolyte temperature need not to keep, and can change in 10～80 ℃ of scopes; Anodizing time can be controlled in 5～15min and finishes; The average formation speed of rete is fast, can reach 3～5 μ m/min; Thicknesses of layers can change between 10～40 μ m.
5. the arc electrochemical anodic oxidation film forming process that presses down of the present invention has characteristics such as plant and instrument less investment, production technique is simple, the one-pass film-forming area is big, tooling cost is low.The rete that obtains has the excellent decoration performance, in case product adopts present technique as its process for treating surface, will improve added value of product greatly, makes product have the stronger market competitiveness.
Embodiment:
Embodiment 1:
1 starting material
(sample is diameter 30mm to the AZ91D magnesium alloy materials, the right cylinder of high 9mm.)
2 technical process
Degreasing → washing → but arc electrochemical anodic oxidation film forming → washing → oven dry
3 electrolyte components
| Dimethylamine 30g/L thanomin 60g/L sodium phosphate 10g/L sebacic acid sodium 1.5g/L sodium metavanadate 4g/L Sodium Fluoride 4g/L |
4 press down arc electrochemical anodic oxidation technology
Place electrolyzer to press down the arc anodic oxidation treatment magnesium alloy materials, the control anodizing voltage rises to 120 volts by 0 volt in 30s, and oxidation current raises with voltage and increases, and reaches peak current density 18A/dm
2, and continue 5 seconds, and allow film forming carry out automatically then, finish (in the operating process, until film forming when current density drops to 2A/dm
2During the left and right sides, think that then film process finishes).Time is 8min, and solution temperature need not forced refrigeration, only needs to adopt the recirculated cooling water cooling that tank liquor is not seethed with excitement and gets final product.
5 film qualities
Light brown, even, complete, smooth densification, thicknesses of layers 23 μ m, hardness 290HV.
Embodiment 2:
1 starting material
(sample is diameter 30mm to the AZ91D magnesium alloy materials, the right cylinder of high 9mm.)
2 technical process
Identical with embodiment 1
3 electrolyte components
| Ethamine 50g/L diethylenetriamine 50g/L dipotassium hydrogen phosphate 8g/L sodium wolframate 6g/L sodium acetate 1g/L Sodium Fluoride 5g/L |
4 press down arc electrochemical anodic oxidation technology
Place electrolyzer to press down the arc anodic oxidation treatment magnesium alloy materials, the control anodizing voltage rises to 100 volts by 0 volt in 30s, and oxidation current raises with voltage and increases, and reaches peak current density 15A/dm
2, and continue 10 seconds, and allow film forming carry out automatically then, finish (in the operating process, until film forming when current density drops to 2A/dm
2During the left and right sides, think that then film process finishes).Time is 8min, and solution temperature need not forced refrigeration, only needs to adopt the recirculated cooling water cooling that tank liquor is not seethed with excitement and gets final product.
5 film qualities
Silver gray, even, complete, smooth densification, thicknesses of layers 35 μ m, hardness 300HV.
Embodiment 3:
1 starting material
(sample is diameter 30mm to the AZ91D magnesium alloy materials, the right cylinder of high 9mm.)
2 technical process
Identical with embodiment 1
3 electrolyte components
| Dimethylamine 70g/L thanomin 80g/L sodium phosphate 12g/L sodium wolframate 8g/L Sodium Propionate 4g/L Sodium tetrafluoroborate 5g/L |
4 press down arc electrochemical anodic oxidation technology
Place electrolyzer to press down the arc anodic oxidation treatment magnesium alloy materials, the control anodizing voltage rises to 80 volts by 0 volt in 30s, and oxidation current raises with voltage and increases, and reaches peak current density 16A/dm
2, and continue 8 seconds, and allow film forming carry out automatically then, finish (in the operating process, until film forming when current density drops to 2A/dm
2During the left and right sides, think that then film process finishes).Time is 8min, and solution temperature need not forced refrigeration, only needs to adopt the recirculated cooling water cooling that tank liquor is not seethed with excitement and gets final product.
5 film qualities
Canescence, even, complete, smooth densification, thicknesses of layers 20 μ m, hardness 265HV.
Embodiment 4:
1 starting material
(sample is diameter 30mm to the AZ31 magnesium alloy materials, the right cylinder of high 9mm.)
2 technical process
Identical with embodiment 1
3 electrolyte components
| Amylamine 35g/L quadrol 45g/L trisodium phosphate 6g/L para-phthalic sodium 2g/L fluoroboric acid sodium 4g/L |
4 press down arc electrochemical anodic oxidation technology
Place electrolyzer to press down the arc anodic oxidation treatment magnesium alloy materials, the control anodizing voltage rises to 150 volts by 0 volt in 30s, and oxidation current raises with voltage and increases, and reaches peak current density 20A/dm
2, and continue 5 seconds, and allow film forming carry out automatically then, finish (in the operating process, until film forming when current density drops to 2A/dm
2During the left and right sides, think that then film process finishes).Time is 8min, and solution temperature need not forced refrigeration, only needs to adopt the recirculated cooling water cooling that tank liquor is not seethed with excitement and gets final product.
5 film qualities
Brown, even, complete, smooth densification, thicknesses of layers 25 μ m, hardness 310HV.
Embodiment 5:
1 starting material
(sample is diameter 30mm to the AZ31 magnesium alloy materials, the right cylinder of high 9mm.)
2 technical process
Identical with embodiment 1
3 electrolyte components
| Dimethylamine 50g/L quadrol 45g/L trisodium phosphate 6g/L sodium tetraborate 4g/L hexanodioic acid sodium 1g/L fluoroboric acid sodium 2g/L |
4 press down arc electrochemical anodic oxidation technology
Place electrolyzer to press down the arc anodic oxidation treatment magnesium alloy materials, the control anodizing voltage rises to 120 volts by 0 volt in 30s, and oxidation current raises with voltage and increases, and reaches peak current density 18A/dm
2, and continue 5 seconds, and allow film forming carry out automatically then, finish (in the operating process, until film forming when current density drops to 2A/dm
2During the left and right sides, think that then film process finishes).Time is 8min, and solution temperature need not forced refrigeration, only needs to adopt the recirculated cooling water cooling that tank liquor is not seethed with excitement and gets final product.
5 film qualities
Brown, even, complete, smooth densification, thicknesses of layers 20 μ m, hardness 300HV.
Embodiment 6:
1 starting material
(sample is diameter 30mm to the MB2 magnesium alloy materials, the right cylinder of high 9mm.)
2 technical process
Identical with embodiment 1
3 electrolyte components
| Triethylene tetramine 50g/L trolamine 25g/L sodium polyphosphate 8g/L sebacic acid sodium 1.5g/L Sodium Fluoride 3g/L Sodium Silicofluoride 2g/L |
4 press down arc electrochemical anodic oxidation technology
Place electrolyzer to press down the arc anodic oxidation treatment magnesium alloy materials, the control anodizing voltage rises to 120 volts by 0 volt in 30s, and oxidation current raises with voltage and increases, and reaches peak current density 16A/dm
2, and continue 10 seconds, and allow film forming carry out automatically then, finish (in the operating process, until film forming when current density drops to 2A/dm
2During the left and right sides, think that then film process finishes).Time is 8min, and solution temperature need not forced refrigeration, only needs to adopt the recirculated cooling water cooling that tank liquor is not seethed with excitement and gets final product.
5 film qualities
Brown, even, complete, smooth densification, thicknesses of layers 20 μ m, hardness 260HV.
Embodiment 7:
1 starting material
(sample is diameter 30mm to the MB2 magnesium alloy materials, the right cylinder of high 9mm.)
2 technical process
Identical with embodiment 1
3 electrolyte components
| Dimethylamine 70g/L quadrol 35g/L potassium primary phosphate 12g/L sodium aluminate 10g/L Sodium tetrafluoroborate 5g/L |
4 press down arc electrochemical anodic oxidation technology
Place electrolyzer to press down the arc anodic oxidation treatment magnesium alloy materials, the control anodizing voltage rises to 150 volts by 0 volt in 30s, and oxidation current raises with voltage and increases, and reaches peak current density 20A/dm
2, and continue 15 seconds, and allow film forming carry out automatically then, finish (in the operating process, until film forming when current density drops to 2A/dm
2During the left and right sides, think that then film process finishes).Time is 8min, and solution temperature need not forced refrigeration, only needs to adopt the recirculated cooling water cooling that tank liquor is not seethed with excitement and gets final product.
5 film qualities
Canescence, even, complete, smooth densification, thicknesses of layers 30 μ m, hardness 350HV.
Claims (6)
1. magnesium alloy is at the anodic oxidation electrolyte that presses down under the arcuation attitude, and it is characterized in that: electrolyte component is:
Dimethylamine 30g/L
Thanomin 60g/L
Sodium phosphate 10g/L
Sebacic acid sodium 1.5g/L
Sodium metavanadate 4g/L
Sodium Fluoride 4g/L;
Wherein said electrolyte solution all is solvent with water.
2. magnesium alloy is at the anodic oxidation electrolyte that presses down under the arcuation attitude, and it is characterized in that: electrolyte component is:
Ethamine 50g/L
Diethylenetriamine 50g/L
Dipotassium hydrogen phosphate 8g/L
Sodium wolframate 6g/L
Sodium acetate 1g/L
Sodium Fluoride 5g/L;
Wherein said electrolyte solution all is solvent with water.
3. magnesium alloy is at the anodic oxidation electrolyte that presses down under the arcuation attitude, and it is characterized in that: electrolyte component is:
Dimethylamine 70g/L
Thanomin 80g/L
Sodium phosphate 12g/L
Sodium wolframate 8g/L
Sodium Propionate 4g/L
Sodium tetrafluoroborate 5g/L
Wherein said electrolyte solution all is solvent with water.
4. magnesium alloy is at the anodic oxidation electrolyte that presses down under the arcuation attitude, and it is characterized in that: electrolyte component is:
Amylamine 35g/L
Quadrol 45g/L
Trisodium phosphate 6g/L
Para-phthalic sodium 2g/L
Fluoroboric acid sodium 4g/L;
Wherein said electrolyte solution all is solvent with water.
5. magnesium alloy is at the anodic oxidation electrolyte that presses down under the arcuation attitude, and it is characterized in that: electrolyte component is:
Dimethylamine 50g/L
Quadrol 45g/L
Trisodium phosphate 6g/L
Sodium tetraborate 4g/L
Hexanodioic acid sodium 1g/L
Fluoroboric acid sodium 2g/L
Wherein said electrolyte solution all is solvent with water.
6. magnesium alloy is at the anodic oxidation electrolyte that presses down under the arcuation attitude, and it is characterized in that: electrolyte component is:
Triethylene tetramine 50g/L
Trolamine 25g/L
Sodium polyphosphate 8g/L
Sebacic acid sodium 1.5g/L
Sodium Fluoride 3g/L
Sodium Silicofluoride 2g/L;
Wherein said electrolyte solution all is solvent with water.
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|---|---|---|---|
| CNB200510032436XA CN100425740C (en) | 2005-11-25 | 2005-11-25 | Anode oxidating electrolysing liquid under inhibiting arc state of magnesium alloy and process for anode oxidating |
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| CN1793438A CN1793438A (en) | 2006-06-28 |
| CN100425740C true CN100425740C (en) | 2008-10-15 |
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Families Citing this family (14)
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| KR101195458B1 (en) * | 2009-04-22 | 2012-10-30 | 한양대학교 에리카산학협력단 | Method for treating the surface of metal |
| CN101974711B (en) * | 2010-09-28 | 2012-10-31 | 蔡乐勤 | Preparation method of aluminum magnesium alloy material with wear resistance and corrosion resistance |
| CN102199785B (en) * | 2011-06-29 | 2012-12-12 | 上海理工大学 | Microarc oxidation solution of titanium alloy wear-resistant coating and application thereof |
| CN102828218B (en) * | 2012-09-14 | 2015-04-15 | 戚威臣 | Electrolyte used for magnesium alloy anode oxidation treatment and treatment method |
| CN103938253A (en) * | 2013-01-23 | 2014-07-23 | 汉达精密电子(昆山)有限公司 | Magnesium alloy anodic oxidation electrolyte and method of processing magnesium alloy with the electrolyte |
| CN105101715B (en) * | 2014-04-25 | 2019-04-26 | 华为技术有限公司 | Anti-corrosion magnesium alloy communication device and preparation method thereof |
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| CN105714354A (en) * | 2016-03-21 | 2016-06-29 | 南京工程学院 | Electrolyte used for preparing N-doped micro-arc oxidation ceramic layer |
| WO2018126094A1 (en) * | 2017-01-01 | 2018-07-05 | Henkel Ag & Co. Kgaa | Dark colored electroceramic coatings for magnesium |
| CN107090590A (en) * | 2017-04-24 | 2017-08-25 | 南京邮电大学 | A kind of aluminium alloy anode oxide electrolyte and oxidation technology based on corrosion inhibiter |
| CN108327167A (en) * | 2018-03-07 | 2018-07-27 | 广州凯腾新材料科技有限公司 | The method that metal and plastic cement combine |
| CN111118570A (en) * | 2018-10-31 | 2020-05-08 | 华孚精密科技(马鞍山)有限公司 | Die-casting aluminum alloy micro-arc oxidation electrolyte, method and product thereof |
| CN111162245B (en) * | 2018-11-08 | 2021-08-20 | 四川理工学院 | Magnesium air battery cathode surface modification method and electrolyte |
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