CN101985768A - Micro-arc oxidation electrolyte and micro-arc oxidation method - Google Patents
Micro-arc oxidation electrolyte and micro-arc oxidation method Download PDFInfo
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- CN101985768A CN101985768A CN2009101090659A CN200910109065A CN101985768A CN 101985768 A CN101985768 A CN 101985768A CN 2009101090659 A CN2009101090659 A CN 2009101090659A CN 200910109065 A CN200910109065 A CN 200910109065A CN 101985768 A CN101985768 A CN 101985768A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
Abstract
The invention belongs to the field of micro-arc oxidation, and relates to micro-arc oxidation electrolyte. The electrolyte comprises the aqueous solution of film former and toner, and has the pH value of 6.0 to 12, wherein the film former is phosphate and/or silicate; the toner is a titanium compound; and the film former content is 5 to 50 g/L, and the toner content is 5 to 30 g/L. When used for performing micro-arc oxidation on light metals, the micro-arc oxidation electrolyte provided by the invention can form blue ceramic films on the surfaces of the light metals so as to break the limitation of the conventional micro-arc oxidation technology to colors, expand grey-black and grey-white tones to colorful fields with uniform colors and achieve the decoration effect of a light-metallic product. Moreover, by the invention, the erosion resistance, the pollution resistance and the compactability of the micro-arc oxidized film are enhanced, and the surface of the micro-arc oxidized film has a ceramic texture. The invention further discloses a micro-arc oxidation method.
Description
Technical field
The present invention relates to a kind of differential arc oxidation electrolytic solution and differential arc oxidation method.
Background technology
At present, light metal material, for example aluminium, magnesium, titanium and alloy thereof, in light weight with it, specific tenacity is high, rolling property and ductility are good, be easy to machining characteristics is widely used in space flight, aviation, automobile, building and electron trade.But the surperficial matter of light metal corrosion potential soft, not wear-resistant, non-refractory, especially aluminium is lower, and general corrosion is more serious.In order to overcome the defective of light metal surface aspect of performance, the broadened application scope increases the service life, and often need carry out oxidation to the surface of light metal material, makes its surface generate layer protecting film, in order to the surface property that improves light metal and ornamental.
Carry out differential arc oxidation acquisition micro-arc oxidation films on the light metal material surface and have lot of advantages: pre-treatment is simple, coating growth speed is fast, hardness is high, electrolytic solution is free from environmental pollution.Thereby the application of differential arc oxidization technique more and more widely.But the rete color of existing micro-arc oxidation films is single, is confined to tones such as white, black, grey black look usually.In order to make it have decorative effect more attractive in appearance, require micro-arc oxidation films to possess chromatic effect.
In order to make micro-arc oxidation films possess chromatic effect, someone directly adds pigment or dyestuff in the electrolytic solution of differential arc oxidation, still, can make the sticking power variation of micro-arc oxidation films on the light metal material surface like this, and it is inhomogeneous to paint, and does not reach desirable effect.
The light metal material that the somebody will form micro-arc oxidation films under study for action from the teeth outwards immerse carry out in the staining trough placed staining agent painted.But, to carry out painted micro-arc oxidation films irregular colour like this and spare, poor adhesive force comes off easily, and is difficult to reach the Color of expection.
Summary of the invention
The technical problem to be solved in the present invention be make the irregular colour on micro-arc oxidation films surface even in the prior art, the defective of poor adhesive force, thereby a kind of electrolytic solution that can form colored micro-arc oxidation films and color even that should colour micro-arc oxidation films surface, differential arc oxidation that sticking power is good is provided.
The invention provides a kind of differential arc oxidation electrolytic solution, wherein, comprise that the aqueous solution of membrane-forming agent and toning agent and the Ph of electrolytic solution are 6.0-12; Described membrane-forming agent is phosphoric acid salt and/or silicate, and described toning agent is a titanium compound; The content of described membrane-forming agent is 5-50g/L, and the content of described toning agent is 5-30g/L.
Another technical problem that the present invention will solve be make the irregular colour on micro-arc oxidation films surface even in the prior art, the defective of poor adhesive force, can form colored micro-arc oxidation films and color even that should colour micro-arc oxidation films surface, the differential arc oxidation method that sticking power is good thereby provide a kind of.
A kind of differential arc oxidation method also is provided, a kind of method of differential arc oxidation, this method comprises light metal material is placed the electrolyzer that fills electrolytic solution, with the light metal material is anode, with the stainless steel plate is negative electrode, make the light metal material surface form micro-arc oxidation films under the condition of differential arc oxidation, wherein, described electrolytic solution is the electrolytic solution of differential arc oxidation of the present invention.
Adopt differential arc oxidation electrolytic solution provided by the invention and electrolysis process that light metal is carried out differential arc oxidation, can obtain blue ceramic membrane at light metal surface, changed the limitation of differential arc oxidization technique in the past aspect color, greyish black and greyish white tone is expanded to colored field, and color is very even, makes the light metal product have decorative effect attractive in appearance.The solidity to corrosion of the formed micro-arc oxidation films of the present invention, resistance to soiling and compactness also all increase in addition, and the surface has ceramic texture.It is peculiar functional that differential arc oxidation electrolytic solution of the present invention and differential arc oxidation method had both been strengthened differential arc oxidation, enriched the ornamental of aluminum alloy differential arc oxidation film again, therefore expand the Application Areas of differential arc oxidization technique, promoted the value added and the actual use value of aluminium alloy workpiece greatly.
Embodiment
The invention provides a kind of differential arc oxidation electrolytic solution, this electrolytic solution comprises that the aqueous solution of membrane-forming agent and toning agent and the Ph of electrolytic solution are 6.0-12; Described membrane-forming agent is phosphoric acid salt and/or silicate, and described toning agent is a titanium compound; The content of described membrane-forming agent is 5-50g/L, and the content of described toning agent is 5-30g/L.
According to electrolytic solution provided by the invention, described phosphoric acid salt or silicate are the main membrane-forming agent in the described electrolytic solution, mainly influence the film forming speed and the rete density of micro-arc oxidation films.In certain scope, along with the increase of phosphoric acid salt or silicate concentration, the differential arc oxidation film forming speed is accelerated.
According to differential arc oxidation electrolytic solution provided by the present invention, described titanium compound is a toning agent, change the composition of its content in solution, can change the depth of micro-arc oxidation films color, obtain the micro-arc oxidation films of blue series, the compound of described titanium is one or more in titanium potassium oxalate(T.P.O.), the titanium dioxide.
According to differential arc oxidation electrolytic solution provided by the present invention, in preferable case, described membrane-forming agent is the mixture of phosphoric acid salt and silicate.Described phosphatic content is 5-50g/L, be preferably 10-30g/L, and the content of described silicate is 5-50g/L, be preferably 8-15g/L, and the content of toning agent is 5-30g/L, be preferably 10-20g/L.
According to electrolytic solution provided by the invention, in the preferred case, described phosphoric acid salt is one or more in Trisodium trimetaphosphate, Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, sodium polyphosphate, sodium phosphate, the potassium polyphosphate; Described silicate is one or more in water glass, potassium silicate, the water glass.
According to differential arc oxidation electrolytic solution provided by the present invention, in the preferred case, described electrolytic solution also comprises additive, and described content of additive is 0-30g/L, more elects 5-15g/L as; Described additive is one or more in sodium wolframate, Sodium orthomolybdate, borax, ammonium molybdate, boric acid, potassium wolframate, the potassium molybdate.Described additive can improve the surface property of light metal surface micro-arc oxidation films, for example hardness, fineness, homogeneity and resistance to soiling.
According to electrolytic solution provided by the invention, for the pH value that makes electrolytic solution is 6-12, electrolytic solution of the present invention also comprises the Ph conditioning agent, the pH value of described electrolytic solution can be regulated by well known to a person skilled in the art method, for example regulate by adding alkali, described alkali can be sodium hydroxide and/or potassium hydroxide, and the content of described alkali in electrolytic solution is 0-10g/L, is preferably 0-5g/L.
According to differential arc oxidation electrolytic solution provided by the present invention, in the preferred case, described electrolytic solution also comprises stablizer, and the content of described stablizer is 0-10ml/L, and described stablizer is one or more in glycerol, ethylene glycol, the butyleneglycol.Described stablizer can play the effect of stabilizing solution, makes in the electrolytic process to be difficult for producing solution and to splash.
Differential arc oxidation method provided by the invention comprises light metal material is placed the electrolyzer that fills electrolytic solution, with the light metal material is anode, with the stainless steel plate is negative electrode, under the condition of differential arc oxidation, make the light metal material surface form micro-arc oxidation films, wherein, described electrolytic solution is differential arc oxidation electrolytic solution provided by the invention.
According to method provided by the invention, in the preferred case, the condition of described differential arc oxidation comprises that current density is 3-30A/dm
2, voltage is 300-600V, and the temperature of electrolytic solution is 15-60 ℃, and the time of differential arc oxidation is 5-80 minute.
According to method provided by the invention, can obtain attached to light metal surface thickness is 1-100 micron micro-arc oxidation films.
According to method provided by the invention, in the preferred case, described light metal material can be aluminum or aluminum alloy, for example aluminum alloy materials can be the trade mark be 2024,5052,6061,6063, aluminum alloy materials.
The present invention also comprises pre-treatment to the concrete steps that light metal carries out differential arc oxidation, promptly light metal material is carried out degreasing.The method of light metal material being carried out degreasing is for well known to a person skilled in the art the whole bag of tricks, and for example this method comprises, light metal material was soaked in the skim soln 2-5 minute, and water is rinsed well then.The component of skim soln and formulation content are for well known to a person skilled in the art various components and formulation content, for example the selected skim soln of the present invention is the aqueous solution that contains yellow soda ash 15-25g/L, sodium phosphate 10-20g/L, tripoly phosphate sodium STPP 2-5g/L, sodium hydroxide 0-0.5g/L, and the temperature of skim soln is 35-45 ℃.
According to method provided by the invention, in the preferred case, the micropore of the micro-arc oxidation films that light metal surface is formed seals, and is dry then.
The method that the micropore of the micro-arc oxidation films that light metal surface is formed seals can adopt the whole bag of tricks known in those skilled in the art, for example method such as water seal method, organosilicon sealing of hole.The present invention preferably adopts the water seal method, and this method comprises that the pure water with 70-90 ℃ soaked light metal 0.5-10 minute that is attached with micro-arc oxidation films.
After the micropore of the colored micro-arc oxidation films that light metal surface is formed seals, then dry.The exsiccant method can adopt the whole bag of tricks known in those skilled in the art, and for example drying can adopt 20-50 ℃ wind to do.
Adopt the mode of embodiment that the present invention is described in further detail below.
Embodiment 1
1, pre-treatment
Al alloy parts (6061) was soaked in the skim soln 3 minutes, and water is rinsed well then.Skim soln is for containing sodium hydroxide 0.01 grams per liter, the aqueous solution of sodium phosphate 15 grams per liters, yellow soda ash 20 grams per liters and tripoly phosphate sodium STPP 3 grams per liters, and the temperature of skim soln is 40 ℃.
2, differential arc oxidation
Al alloy parts after the degreasing is immersed in the differential arc oxidation electrolytic solution, with the Al alloy parts is anode, stainless steel plate is a negative electrode, under 25 ℃ condition, adopt the pulse mao power source to carry out differential arc oxidation, supply frequency is 500HZ, dutycycle is 20%, and voltage is 300 volts, and current density is 5A/dm
2, differential arc oxidation 30 minutes, taking-up cleans up with pure water after finishing.This differential arc oxidation electrolytic solution is for containing tripoly phosphate sodium STPP 20g/L, and titanium potassium oxalate(T.P.O.) 15g/L, the PH of electrolytic solution are 6.5.
It is sealing 5 minutes in 85 ℃ the hot pure water that the above-mentioned Al alloy parts that carries out behind the differential arc oxidation is immersed temperature, takes out then in 20 ℃ of hot blast dryings.
Finally obtain being attached with the alloy product that thickness is 10 microns blue micro-arc oxidation films.Through visual observation, color is very even.
Embodiment 2
According to the method for describing among the embodiment 1 Al alloy parts (2024) is carried out differential arc oxidation, different is that differential arc oxidation electrolytic solution is for containing tripoly phosphate sodium STPP 20g/L, water glass 8g/L, sodium hydroxide 2g/L, titanium potassium oxalate(T.P.O.) 15g/L, the aqueous solution of glycerol 5ml/L, the PH of electrolytic solution is 10.The supply frequency of differential arc oxidation is 800HZ, and dutycycle is 20%, and current density is 3A/dm
2, voltage is 300V, the time of differential arc oxidation is 30 minutes.
Final acquisition is attached with the alloy product that thickness is 12 microns blue micro-arc oxidation films.Through visual observation, color is very even.
Embodiment 3
According to the method for describing among the embodiment 1 Al alloy parts (6061) is carried out differential arc oxidation, different is that differential arc oxidation electrolytic solution is for containing Sodium hexametaphosphate 99 15g/L, Trisodium trimetaphosphate 15g/L, sodium hydroxide 4g/L, titanium potassium oxalate(T.P.O.) 25g/L, the solution of sodium wolframate 4g/L, the PH of electrolytic solution are 12.The supply frequency of differential arc oxidation is 3000HZ, and dutycycle is 25%, and current density is 10A/dm
2, voltage is 500V, the time of differential arc oxidation is 40 minutes.
Final acquisition is attached with the alloy product that thickness is 15 microns mazarine micro-arc oxidation films.Through visual observation, color is very even.
Embodiment 4
According to the method for describing among the embodiment 1 aluminium alloy (6063) workpiece is carried out differential arc oxidation, different is, differential arc oxidation electrolytic solution is for containing Sodium hexametaphosphate 99 5g/L, Trisodium trimetaphosphate 5g/L, sodium hydroxide 4g/L, titanium potassium oxalate(T.P.O.) 5g/L, ethylene glycol 7ml/L, the aqueous solution of sodium wolframate 12g/L, the Ph of electrolytic solution is 12.The supply frequency of differential arc oxidation is 1000HZ, and dutycycle is 40%, and current density is 15A/dm
2, voltage is raised to 460V, and the time of differential arc oxidation is 40 minutes.
Final acquisition is attached with the alloy product that thickness is 10 microns light blue micro-arc oxidation films.Through visual observation, color is very even.
Embodiment 5
According to the method for describing among the embodiment 1 aluminium alloy 5052 workpiece are carried out differential arc oxidation, different is, differential arc oxidation electrolytic solution is for containing Sodium hexametaphosphate 99 20g/L, Trisodium trimetaphosphate 20g/L, water glass 10g/L, sodium hydroxide 4g/L, titanium potassium oxalate(T.P.O.) 10g/L, ethylene glycol 10ml/L, the aqueous solution of Sodium Tetraborate 20g/L, the Ph of electrolytic solution is 12.The frequency of the power supply of differential arc oxidation is 1500HZ, and dutycycle is 15%, and current density is 8A/dm
2, voltage is raised to 480V, and the time of differential arc oxidation is 30 minutes.
Final acquisition is attached with the alloy product that thickness is 16 microns blue micro-arc oxidation films.Through visual observation, color is very even.
Embodiment 6
According to the method for describing among the embodiment 1 aluminium alloy 5052 workpiece are carried out differential arc oxidation, different is, differential arc oxidation electrolytic solution is for containing Sodium hexametaphosphate 99 20g/L, Trisodium trimetaphosphate 10g/L, water glass 5g/L, sodium hydroxide 10g/L, titanium potassium oxalate(T.P.O.) 30g/L, the aqueous solution of Sodium Tetraborate 30g/L, the Ph of electrolytic solution is 13.The frequency of the power supply of differential arc oxidation is 3000HZ, and dutycycle is 5%, and current density is 30A/dm
2, voltage is raised to 600V, and the time of differential arc oxidation is 30 minutes.
Final acquisition is attached with the alloy product that thickness is 14 microns blue micro-arc oxidation films.Through visual observation, color is very even.
Embodiment 7
According to the method for describing among the embodiment 1 aluminium alloy 6061 workpiece are carried out differential arc oxidation, different is, differential arc oxidation electrolytic solution is for containing Sodium hexametaphosphate 99 5g/L, water glass 6g/L, and titanium potassium oxalate(T.P.O.) 10g/L, the aqueous solution of Sodium Tetraborate 5g/L, the Ph of electrolytic solution is 7.The frequency of the power supply of differential arc oxidation is 2000HZ, and dutycycle is 15%, and current density is 20A/dm
2, voltage is raised to 480V, and the time of differential arc oxidation is 30 minutes.
Final acquisition is attached with the alloy product that thickness is 11 microns blue micro-arc oxidation films.Through visual observation, color is very even.
Comparative Examples 1
According to the method for describing among the embodiment 1 aluminium alloy 6061 workpiece are carried out anodic oxidation, different is that differential arc oxidation electrolytic solution is Sodium hexametaphosphate 99 20g/L, Trisodium trimetaphosphate 20g/L, water glass 6g/L, sodium hydroxide 4g/L, the aqueous solution of Sodium Tetraborate 5g/L, the Ph of electrolytic solution is 12 the aqueous solution.The current density of differential arc oxidation is 8A/dm
2, voltage is raised to 480V, and the time of differential arc oxidation is 30 minutes.Then sample being put into blue organic dye solution placed 5 minutes.
Final acquisition is attached with the alloy product that thickness is 12 microns light blue uneven micro-arc oxidation films.
Performance test
(1), sticking power test
The surface treated sample for preparing is measured the method for fusible method (ASTM D3359-02) according to tape test, carry out the sticking power test.
(2) the wear-resisting test of RCA paper tape (F2357-04)
Use the RCA paper tape wear resistant instrument of model as F350008, the differential arc oxidation film layer of friction product surface is milled to when exposing aluminum alloy material surface under 175 gram forces, the number of turns that the record rubber wheel rotates.
(3) pencil hardness test (ASTMD 3363-74)
Instrument: pencil hardness meter F130027
The method of inspection: according to ASTM D3363, load: 750 grams, pencil: the UNI of Mitsubishi
(4) neutral salt spray corrosion test
Product sample is placed salt-mist corrosion tester (the positive laboratory apparatus in source, Shanghai company limited, FQY050) in, at 35 ℃ is that the sodium chloride aqueous solution of 5 ± 0.5 weight % was sprayed 48 hours continuously on the product sample surface with concentration down, take out then and observe, and the corroded area of record product sample surfaces accounts for the percentage composition of the rete total area as the salt air corrosion ratio.
Table 1
From the result of table 2 as can be seen, adopt the electrolytic solution of differential arc oxidation provided by the invention and the method for differential arc oxidation that Al alloy parts is carried out differential arc oxidation, adopt the electrolytic solution of differential arc oxidation provided by the invention and the method for differential arc oxidation not only can form blue micro-arc oxidation films on the light metal material surface, and the performance of various surface property wear resistancies that should the blueness micro-arc oxidation films, erosion resistance sticking power is all very high, and hardness is very high.
Claims (9)
1. a differential arc oxidation electrolytic solution is characterized in that, comprises that the aqueous solution of membrane-forming agent and toning agent and the Ph of electrolytic solution are 6.0-12; Described membrane-forming agent is phosphoric acid salt and/or silicate, and described toning agent is a titanium compound;
The content of described membrane-forming agent is 5-50g/L, and the content of described toning agent is 5-30g/L.
2. differential arc oxidation electrolytic solution according to claim 1, described phosphoric acid salt are one or more in Trisodium trimetaphosphate, Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, sodium polyphosphate, sodium phosphate, the potassium polyphosphate; Described silicate is one or both in water glass, the potassium silicate.
3. differential arc oxidation electrolytic solution according to claim 1, the compound of described titanium are one or both in titanium potassium oxalate(T.P.O.), the titanium dioxide.
4. differential arc oxidation electrolytic solution according to claim 1 also comprises additive, and described content of additive is 0-30g/L; Described additive is one or more in sodium wolframate, Sodium orthomolybdate, borax, ammonium molybdate, boric acid, potassium wolframate, the potassium molybdate.
5. differential arc oxidation electrolytic solution according to claim 1 also comprises the Ph conditioning agent, and described Ph conditioning agent is 0-10g/L, and described Ph conditioning agent is sodium hydroxide and/or potassium hydroxide.
6. differential arc oxidation electrolytic solution according to claim 1 also comprises stablizer, and the content of described stablizer is 0-10ml/L, and described stablizer is one or more in glycerol, ethylene glycol, the butyleneglycol.
7. differential arc oxidation method, this method comprises light metal material is placed the electrolyzer that fills electrolytic solution, with the light metal material is anode, with the stainless steel plate is negative electrode, under the condition of differential arc oxidation, make the light metal material surface form micro-arc oxidation films, it is characterized in that described electrolytic solution is the electrolytic solution of any described differential arc oxidation among the claim 1-6.
8. method according to claim 7, wherein, the condition of described differential arc oxidation comprises, adopts the pulse mao power source to carry out differential arc oxidation, and supply frequency is 500-3000HZ, and dutycycle is 5-40%, and current density is 3-30A/dm
2, voltage is 300-600V, and the temperature of differential arc oxidation is 15-60 ℃, and the time of differential arc oxidation is 5-80 minute.
9. method according to claim 7, wherein, described light metal material is an aluminum or aluminum alloy.
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