CN100457981C - Method for plasma micro arc oxidizing of light metal surface - Google Patents
Method for plasma micro arc oxidizing of light metal surface Download PDFInfo
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- CN100457981C CN100457981C CNB2004100356915A CN200410035691A CN100457981C CN 100457981 C CN100457981 C CN 100457981C CN B2004100356915 A CNB2004100356915 A CN B2004100356915A CN 200410035691 A CN200410035691 A CN 200410035691A CN 100457981 C CN100457981 C CN 100457981C
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 10
- 239000002184 metal Substances 0.000 title claims abstract description 10
- 230000001590 oxidative effect Effects 0.000 title abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000010891 electric arc Methods 0.000 claims abstract description 4
- 239000008151 electrolyte solution Substances 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 claims description 13
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 12
- 229910021538 borax Inorganic materials 0.000 claims description 6
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 239000011775 sodium fluoride Substances 0.000 claims description 6
- 235000013024 sodium fluoride Nutrition 0.000 claims description 6
- 239000004328 sodium tetraborate Substances 0.000 claims description 6
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 229940045641 monobasic sodium phosphate Drugs 0.000 claims description 5
- 235000019353 potassium silicate Nutrition 0.000 claims description 5
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 150000004760 silicates Chemical class 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 2
- 229920003023 plastic Polymers 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 17
- 238000007254 oxidation reaction Methods 0.000 abstract description 13
- 239000003792 electrolyte Substances 0.000 abstract description 12
- 230000003647 oxidation Effects 0.000 abstract description 12
- 229910000838 Al alloy Inorganic materials 0.000 abstract description 6
- 239000008367 deionised water Substances 0.000 abstract description 2
- 229910021641 deionized water Inorganic materials 0.000 abstract description 2
- 230000007935 neutral effect Effects 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001463 metal phosphate Inorganic materials 0.000 abstract 1
- 229910052914 metal silicate Inorganic materials 0.000 abstract 1
- 239000004411 aluminium Substances 0.000 description 15
- 229910045601 alloy Inorganic materials 0.000 description 12
- 239000000956 alloy Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- 229910000737 Duralumin Inorganic materials 0.000 description 5
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 4
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 3
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 3
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005474 detonation Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
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- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The present invention relates to plasma micro arc oxidizing process of light metal surface, and is especially surface oxidizing technological process for aluminum and aluminum alloy. The technological process adopts asymmetrical positive and negative pulse electric sources with continuously adjustable peak voltage, continuously adjustable pulse duty factor and frequency continuously adjustable in 20-2000 Hz; the pre-treated workpiece hung to anode and set inside electrolyte; stainless sheet suspended inside the electrolyte tank as cathode; neutral or alkaline electrolyte comprising metal silicate or metal phosphate and deionized water; and gas-liquid scanning treatment process, in which the workpiece to be oxidized is made to move back and forth in homogeneous speed inside the electrolyte for plasma micro arc discharge in the gas-liquid interface to form oxide film. The process is reliable, high in oxidation efficiency, high in metal surface treating performance and low in power consumption.
Description
Technical field:
The present invention relates to a kind of method of light metal surface being carried out plasma micro-arc oxidation; the oxide treatment technical matters is carried out on particularly a kind of surface to aluminium and alloy thereof; promptly carry out the plasma micro-arc oxidation treating processes at aluminium and alloy surface thereof; make its surface generate ceramic coating, can be widely used in processing is protected in fields such as machinery, electronics, aviation, automobile, engineering to magnesium, titanium and alloy thereof especially aluminium and alloy accessory thereof method.
Technical background:
Aluminium and alloy thereof have good mechanical property and physicals, and it can be widely used in fields such as machinery, electronics, aviation, automobile, engineering, plays an important role in national economy.Though there is the natural oxide film of one deck on the aluminium surface, it has only about 10-100nm, does not have provide protection.So, aluminium material surface is handled, making it the surface, to generate surface hardness and the corrosion resisting property that layer oxide film can improve aluminum be very important.At present, the method for aluminium material surface oxidation mainly contains: chemical oxidation, anodic oxidation and differential arc oxidation etc. are several.Differential arc oxidation has many good qualities than chemical oxidation and anodic oxidation: pre-treatment is simple, coating growth speed is fast, hardness is high, and electrolytic solution is difficult for contaminate environment etc., thereby the application of differential arc oxidization technique more and more widely.Existing many patent documentations or article record, in the Chinese patent application number 011022620 file record of announcing, adopt the pulse power, pulse waveform is a square wave, its frequency is 25-300Hz, and applying voltage is the positive pulse voltage of 300-800V and the negative pulse voltage of 0-300V; In the file record that Chinese patent application number 031571735 is announced, employing be the symmetric alternating current pulse, its voltage is 180-270V, frequency is 20-200Hz, dutycycle is 0.1-0.7.The said pulse-repetition of above-mentioned patent is below the 300Hz, does not point out how many peak impulse voltages is and whether stacking factor is distinguished adjustable continuously.Adopt the method that from molten electrolyte, shifts out sample anodes gradually to optimize processing parameter in the record of Russ P RU2110624 file, but this patent does not point out to put into gradually electrolytic solution again, comes and goes repeatedly.In the document record of Chinese patent application number 022220631, set forth the device that a kind of part bore surface is handled, but need be than complicated apparatus, and can only handle internal surface of hole, and can not handle simultaneously by the hole surfaces externally and internally.In addition, also have Chinese patent application number be 998168645,021115214,971824800 and the 138th page of " Xi'an University of Technology's journal " second phase in 2000 in all descriptions and put down in writing the method and apparatus of oxide treatment aluminium and alloy surface thereof from the same principle method frame such as " aluminum alloy differential arc oxidation technology " document of etc.ing, all exist the shortcoming that some are difficult for raising the efficiency and increasing handling property in these methods in varying degrees.
Summary of the invention:
The objective of the invention is to adopt conventional technical matters that metal is particularly carried out the method for oxide treatment in the surface of aluminium and alloy thereof, it mainly is in order to overcome the shortcoming of the parameter condition aspect that exists in the prior art, raising the efficiency and increasing under the handling property condition, a kind of novel method of using the plasma micro-arc oxidation method to handle aluminium and alloy surface thereof is provided, promptly adopts a kind of asymmetric positive and negative pulse power to carry out plasma micro-arc oxidation and handle aluminium and alloy thereof.
Its plasma micro-arc oxidation process of method for oxidation involved in the present invention is: will hang over through the workpiece of pre-treatment and put into electrolytic solution on the anode, negative electrode is the stainless steel substrates that hangs in stainless steel electrolytic liquid bath or the plastics electrolytic bath; Adopt the asymmetric positive and negative pulse power, applying the pulse forward voltage is 0-650V, and negative voltage is 0-100V, and current density is 3-60A/dm
2, oxidation temperature is 10-65 ℃, the treatment time can be 5-360min.Wherein, pulse-repetition is that 20-2000Hz is adjustable continuously; Positive and negative peak impulse voltage is adjustable continuously: peak forward voltage 0-700V, negative peak voltage 0-100V; Positive and negative pulse duty factor is adjustable continuously in 0-100% respectively.Used electrolytic solution is made up of chemical substance such as metal-salt and deionized water, is divided into silicate series and series of phosphate, is neutral or alkaline, and the pH value is 7-12.Silicate series electrolytic solution wherein comprises water glass (2.5-60g/L), sodium hydroxide (0.5-10g/L), additive (organic or inorganic things such as Sodium hexametaphosphate 99, Seignette salt, sodium wolframate, Trisodium Citrate) 0.5-5g/L.And series of phosphate electrolytic solution comprises SODIUM PHOSPHATE, MONOBASIC (30-160g/L), sodium tetraborate (10-80g/L), Sodium Fluoride (8-25g/L) and additive (organic or inorganic things such as Seignette salt, sodium wolframate, Sodium Fluoride, ammonium fluoride) 0.5-5g/L.
The plasma micro-arc oxidation method that the present invention adopts is handled aluminium and alloy surface thereof, except that workpiece being immersed in carry out in the electrolytic solution, also can adopt gas-liquid scan mode (liquid-gas interface scanning method) to carry out, make oxidized workpiece at the uniform velocity little by little immerse electrolytic solution with the speed of 0.04-0.4mm/s, at the uniform velocity little by little leave electrolytic solution with identical speed again, and come and go repeatedly, this can make the plasma micro-arc discharge take place at the liquid-gas interface place, make discharge energy concentrated relatively, micro-arc discharge carries out line sweep to sample, helps the generation of the oxide film of workpiece.
The present invention uses the plasma micro-arc oxidation method that aluminium with holes and alloy workpiece surfaces externally and internally thereof are handled simultaneously, because the internal surface of hole of Al alloy parts with holes is because electric field is subjected to partly shielding effect, so the oxidation film layer of internal surface is difficult for growing, employing (minimum-value aperture is Φ 18mm) in workpiece hole increases auxiliary cathode makes the workpiece hole surfaces externally and internally obtain good oxidation film layer simultaneously.
The present invention is when adopting the plasma micro-arc oxidation method to handle aluminium and alloy surface thereof, insulation processing is carried out on used hanger surface, adopt the anode hanger, position on hanger is from the workpiece to electrolytic solution is twined the insulation processing that stretches tight with the insulating material of insulation tape or insulating coating, reduce scattered current and avoid producing the gas detonation and electrolytic solution splashes at liquid level of electrolyte.The present invention compares with existing several different methods, on same principle and frame foundation, parameters such as frequency are adjusted, adopt the liquid-gas interface scanning method, the workpiece surfaces externally and internally is handled simultaneously, increased auxiliary cathode and take technical measures such as insulation processing, its result of implementation shows, it is reliable that present method has principle, oxide treatment efficient height, the metallic surface performance is good, outstanding advantage such as conserve energy.
Specific embodiment:
In the enforcement of the present invention, to hang on the anode through the workpiece of pre-treatment and put into the electrolytic solution that is mixed with respectively, its negative electrode is the stainless steel electrolytic liquid bath, get the pending aluminum alloy part of different quality models respectively, under various different conditions, carry out oxide treatment, its conditional parameter such as each embodiment, its oxide treatment result all reaches the ideal effect.
Embodiment 1:
Handle workpiece: the survey meter aluminum alloy part
Material model: duralumin LY12
Electrolyte prescription: water glass 10g/L
Sodium hydroxide 2.5g/L
Sodium hexametaphosphate 99 1.5g/L
PH value 12
Oxidizing condition: frequency 400Hz
Voltage: positive pulse crest voltage 400V
Negative-going peaks threshold voltage 30V
Stacking factor 50%
Current density 8A/dm
2
Time 10min
The result: rete is Dark grey, and is uniform and smooth, and thicknesses of layers is that 8 μ m reach service requirements
Embodiment 2:
Material model: duralumin LY12
Electrolyte prescription: water glass 10g/L
Sodium hydroxide 2.5g/L
Sodium Tetraborate 5g/L
Sodium wolframate 2g/L
PH value 12
Oxidizing condition: frequency 400Hz
Voltage: positive pulse peak electricity 500V
Negative-going peaks threshold voltage 40V
Stacking factor 50%
Current density 15A/dm
2
Time 360min
Result: thicknesses of layers 200 μ m
Film hardness HV 2200
Embodiment 3:
Select for use inner hole part (Φ 18mmx50mm) as handling workpiece.
Material model: distortion aluminium 8011
Electrolyte prescription: water glass 15g/L
Sodium hydroxide 5g/L
Sodium hexametaphosphate 99 2g/L
Seignette salt 1g/L
PH value 13
Oxidizing condition: frequency 400Hz
Voltage: positive pulse crest voltage 300V
Negative-going peaks threshold voltage 65V
Stacking factor 30%
Current density 8A/dm
2
The auxiliary cathode diameter is the 3mm Stainless Steel Wire
Time 10min
The result: the surfaces externally and internally rete is light grey, color even, smooth surface thicknesses of layers 6 μ m
Embodiment 4:
Aluminium alloy cigarette machine part is as handling workpiece.
Material model: duralumin LY12
Electrolyte prescription: SODIUM PHOSPHATE, MONOBASIC 60g/L
Sodium tetraborate 40g/L
Sodium Fluoride 20g/L
Neutral ammonium fluoride 3g/L
Sodium wolframate 3g/L
PH value 7
Oxidizing condition: frequency 100Hz
Voltage: positive pulse crest voltage 180V
Current density 10A/dm
2
Stacking factor 50%
Time 10min
The result: the rete color is a white, and the surface is moist
Thicknesses of layers 9 μ m
Film hardness HV 1200
Embodiment 5:
Material model: duralumin LY12
Electrolyte prescription: SODIUM PHOSPHATE, MONOBASIC 80g/L
Sodium tetraborate 40g/L
Sodium Fluoride 20g/L
Neutral ammonium fluoride 3.5g/L
PH value 7
Oxidizing condition: frequency 100Hz
Voltage positive pulse crest voltage 170V
Current density 10A/dm
2
Stacking factor 10%
Time 7min
The result: the rete color is a white, the smooth surface exquisiteness, and thicknesses of layers 10 μ m are under scanning electron microscope
Observe, it is the micropore of 5-10 μ m that film surface has diameter
Embodiment 6:
Material model: duralumin LY12
Electrolyte prescription: SODIUM PHOSPHATE, MONOBASIC 80g/L
Sodium tetraborate 40g/L
Sodium Fluoride 20g/L
Neutral ammonium fluoride 3.5g/L
PH value 7
Oxidizing condition: frequency 100Hz
Voltage positive pulse crest voltage 170V
Current density 10A/dm
2
Stacking factor 50%
Time 7min
The result: the rete color is a white, and the surface is more smooth, and thicknesses of layers 10 μ m observe under scanning electron microscope, and it is the micropore of 15-25 μ m that diameter is arranged on the film surface.
By sample result as can be known, when other condition was identical, pulse duty factor was more little, and the gained rete is fine and close more, and when stacking factor reduced to 10% by 50%, the micro-pore diameter of film surface had dropped to 5-10 μ m by 15-25 μ m.
Claims (4)
1. method of light metal surface being carried out plasma micro-arc oxidation, to hang over through the workpiece of pre-treatment and put into electrolytic solution on the anode, negative electrode is the stainless steel substrates that hangs in stainless steel electrolytic liquid bath or the plastics electrolytic bath, adopt the asymmetric positive and negative pulse power, it is characterized in that pulse-repetition is that 20-2000Hz is adjustable continuously, the positive negative pulse stuffing crest voltage is adjustable continuously, and the positive negative pulse stuffing stacking factor is adjustable continuously in 0-100%; Adopt the liquid-gas interface scanning method that workpiece is carried out oxide treatment, this liquid-gas interface scanning method is to make workpiece at the uniform velocity little by little enter electrolytic solution, at the uniform velocity little by little leave electrolytic solution with identical speed again, and come and go repeatedly, the plasma micro-arc discharge is taken place at the liquid-gas interface place.
2. according to claim 1 light metal surface is carried out the method for plasma micro-arc oxidation, it is characterized in that used electrolytic solution is divided into silicate series electrolytic solution and series of phosphate electrolytic solution; Wherein said silicate series electrolytic solution comprises water glass, sodium hydroxide and additive, and described series of phosphate electrolytic solution comprises SODIUM PHOSPHATE, MONOBASIC, sodium tetraborate, Sodium Fluoride and additive.
3. according to claim 1 light metal surface is carried out the method for plasma micro-arc oxidation, it is characterized in that workpiece surfaces externally and internally with holes is handled simultaneously, in workpiece hole, increase auxiliary cathode.
4. according to claim 1 light metal surface is carried out the method for plasma micro-arc oxidation, it is characterized in that insulation processing is carried out with insulation tape or insulating coating in the position on hanger is from the workpiece to electrolytic solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100356915A CN100457981C (en) | 2004-09-14 | 2004-09-14 | Method for plasma micro arc oxidizing of light metal surface |
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| CNB2004100356915A CN100457981C (en) | 2004-09-14 | 2004-09-14 | Method for plasma micro arc oxidizing of light metal surface |
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| CN100457981C true CN100457981C (en) | 2009-02-04 |
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