CN101445949A - 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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Abstract
The invention provides a micro-arc oxidation electrolyte which is aqueous solution containing phosphate and silicate and has the pH value of 6-12, wherein, the electrolyte also contains color toner which comprises one or a plurality of sodium sulfate, rose vitriol, ammonium metavanadate, copper sulphate and potassium permanganate. The micro-arc oxidation electrolyte and a micro-arc oxidation method provided by the invention can lead a micro-arc oxidation film made of light metal materials to obtain multiple colors which are very even to ensure the light metal products to have beautiful decorative effects. Meanwhile, the stain resistance and compactness of the micro-arc oxidation film obtained on the light metal materials are excellent; therefore, the added value and actual use value of aluminium alloy are greatly enhanced.
Description
Technical field
The present invention relates to a kind of electrolytic solution of differential arc oxidation, also relate to a kind of method of differential arc oxidation.
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 blemish in an otherwise perfect thing is soft, not wear-resistant, the non-refractory of surperficial matter of light metal, and especially the corrosion potential of 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 therefore need carry out oxidation to the light metal material surface, makes its surface generate layer protecting film, in order to solve or raising surface property and ornamental function.
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.
For the micro-arc oxidation films that makes the light metal material surface has decorative effect more attractive in appearance, hope can make micro-arc oxidation films possess chromatic effect.
In order to make micro-arc oxidation films possess chromatic effect, someone directly adds pigment or dyestuff under study for action 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 objective of the invention is to overcome that the irregular colour that makes the micro-arc oxidation films surface in the above-mentioned prior art is even, the defective of poor adhesive force, 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, a kind of method of differential arc oxidation also is provided.
The invention provides a kind of electrolytic solution of differential arc oxidation, this electrolytic solution is the aqueous solution that contains phosphoric acid salt and silicate, and the pH value of electrolytic solution is 6-12, and wherein, described electrolytic solution also contains one or more in sodium sulfate, rose vitriol, ammonium meta-vanadate, copper sulfate and the potassium permanganate.
The present invention also provides 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, under the condition of differential arc oxidation, make the light metal material surface form micro-arc oxidation films, wherein, described electrolytic solution is the electrolytic solution of colored differential arc oxidation provided by the invention.
Method according to the electrolytic solution and the differential arc oxidation of differential arc oxidation provided by the invention, can make the micro-arc oxidation films of light metal material obtain black, white, yellow, brown, blue or green brown, grey, reach tens kinds of colors such as being with spot in the shades of colour, and color is very even, makes the light metal product have decorative effect attractive in appearance.Simultaneously, the resistance to soiling and the compactness of the micro-arc oxidation films that light metal material surface obtains are all fine, thereby, promoted the value added and the actual use value of aluminium alloy greatly.
Embodiment
The electrolytic solution of colored differential arc oxidation provided by the invention is the aqueous solution that contains phosphoric acid salt and silicate, and the pH value of electrolytic solution is 6-12, wherein, described electrolytic solution also contains toning agent, and described toning agent is one or more in sodium sulfate, rose vitriol, ammonium meta-vanadate, copper sulfate and the potassium permanganate.
According to electrolytic solution provided by the invention, described phosphoric acid salt and silicate are the main membrane-forming agent in the described electrolytic solution, mainly influence the film forming speed 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 electrolytic solution provided by the invention, sodium sulfate, rose vitriol, ammonium meta-vanadate, copper sulfate and potassium permanganate are all as toning agent, by selecting toning agent or changing the composition of these toning agents in solution, can change the color of light metal material surface by micro-arc oxidation film, obtain having the micro-arc oxidation films of different color.For example, use potassium permanganate can obtain yellow, use rose vitriol can obtain brown etc.
According to electrolytic solution provided by the invention, the pH value of electrolytic solution is 6-12, 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 adopt one or more in sodium hydroxide, yellow soda ash and the potassium hydroxide, the content of described alkali in electrolytic solution is 0.1-10g/L, is preferably 1-6g/L.
According to electrolytic solution provided by the invention, in the preferred case, phosphatic content is 5-50g/L, is preferably 20-40g/L in the described electrolytic solution, and the content of described silicate is 5-50g/L, be preferably 5-10g/L, and the content of toning agent is 0.1-20g/L, be preferably 1-8g/L.In described electrolytic solution, the content of various toning agents is, the content of described sodium sulfate is 0.1-10g/L, be preferably 0.1-2g/L, the content of described rose vitriol is 0.1-10g/L, be preferably 4-8g/L, the content of described ammonium meta-vanadate is 0.1-10g/L, be preferably 4-10g/L, the content of described copper sulfate is 0.1-10g/L, be preferably 1-6g/L, and the content of described potassium permanganate is 0.1-10g/L, be preferably 1-5g/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 and the sodium phosphate; Described silicate is water glass and/or potassium silicate.
According to electrolytic solution provided by the invention, in the preferred case, described electrolytic solution also contains additive, and described additive is one or more in single nickel salt, Sodium orthomolybdate, sodium wolframate, iron(ic) chloride, borax, glycerol and the quadrol.Wherein, single nickel salt, sodium wolframate, Sodium orthomolybdate, iron(ic) chloride and borax can improve the surface property of light metal surface micro-arc oxidation films, for example hardness, fineness, homogeneity and resistance to soiling, and glycerol and/or ethylene glycol can play the effect of stabilizing solution, make in the electrolytic process to be difficult for producing solution and to splash.
According to electrolytic solution provided by the invention, in the preferred case, in described electrolytic solution, various content of additive are, the content of described single nickel salt is 0.1-10g/L, be preferably 1-3g/L, the content of Sodium orthomolybdate is 0.1-10g/L, be preferably 0.1-2g/L, the content of sodium wolframate is 0.1-10g/L, be preferably 0.1-1g/L, the content of iron(ic) chloride is 0.1-10g/L, be preferably 0.1-2g/L, the content of borax is 0.1-10g/L, be preferably 6-10g/L, the content of glycerol is 0.1-10g/L, be preferably 1-2g/L, the content of quadrol is 0.1-10g/L, be preferably 1-2g/L.
The method of differential arc oxidation 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 the electrolytic solution of differential arc oxidation 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 0.5-10A/dm
2, voltage is 0-800V, and the temperature of electrolytic solution is 15-60 ℃, and the time of differential arc oxidation is 2-30 minute.
Can obtain thickness under these conditions is the colored micro-arc oxidation films of 2-100 micron.
The detailed process of differential arc oxidation is, Al alloy parts is immersed in the electrolytic solution as anode, with the electrolyzer of stainless steel plate as negative electrode, voltage is raise gradually from 0, when rising to 5-50V, workpiece surface produces anodic oxidation, generates the porousness aluminum oxide film that certain resistivity is arranged, i.e. anode oxide film.Voltage continues to raise, and when rising to the 300V left and right sides, workpiece surface produces the halation discharge, and this moment, workpiece surface formed ceramic membrane.When voltage is elevated to the 400V left and right sides, the ceramic membrane that workpiece surface forms is promptly punctured by high-voltage and forms the spark discharge passage, goes out when rising when becoming red one by one spark bright spot, when voltage further is elevated to 500-600V, the spark color is white by red stain, and bright spot is changed from small to big.But the voltage promotion constantly produces spark discharge to 800V.So, under effects such as electrochemistry, chemistry, plasma physics, grow one deck Al at the Al alloy parts surface in situ
2O
3Ceramic membrane.
According to method provided by the invention, in the preferred case, described light metal material can be aluminum or aluminum alloy, and for example aluminum alloy materials can be that the trade mark is 2024,5052,6061,6063 aluminum alloy materials.
According to method provided by the invention, in the preferred case, the micropore of the colored micro-arc oxidation films that light metal surface is formed seals, and is dry then.
The method that the micropore of the colored 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 methods such as water seal method, nickel envelope, 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 colored micro-arc oxidation films.
After the micropore of the colored micro-arc oxidation films that light metal surface is formed seals, then dry.Drying can adopt 10-50 ℃ wind to do.
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 5-10 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 for containing sodium hydroxide 20-50 grams per liter, the aqueous solution of sodium phosphate 30-50 grams per liter and water glass 10-30 grams per liter, and the temperature of skim soln is 60-85 ℃.
Adopt the mode of embodiment that the present invention is described in further detail below.
Embodiment 1
Handle workpiece: aluminium alloy battery of mobile phone lid; Material model: A16061
1, pre-treatment
Above-mentioned Al alloy parts was soaked in the skim soln 10 minutes, and water is rinsed well then.Skim soln is for containing sodium hydroxide 30 grams per liters, the aqueous solution of sodium phosphate 40 grams per liters and water glass 20 grams per liters, and the temperature of skim soln is 70 ℃.
2, differential arc oxidation
Al alloy parts after the degreasing is immersed in the differential arc oxidation electrolytic solution, is anode with the Al alloy parts, and stainless steel plate is a negative electrode, adopts the voltage of 0-600 volt under the condition about 25 ℃, 5A/dm
2Current density carried out differential arc oxidation 10 minutes, take out after finishing and clean up with pure water.This differential arc oxidation electrolytic solution is for containing Sodium hexametaphosphate 99 20g/L, Trisodium trimetaphosphate 15g/L, water glass 8g/L, the aqueous solution of potassium permanganate 1g/L and sodium hydroxide 6g/L.
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 to dry up.
Finally obtain being attached with the alloy product that thickness is 9 microns yellow micro-arc oxidation films.Through visual observation, color is very even.
Comparative Examples 1
According to the method for describing among the embodiment 1 Al alloy parts is carried out differential arc oxidation, different is, does not contain potassium permanganate in the electrolytic solution, obtains being attached with the alloy product that thickness is 9 microns micro-arc oxidation films.
Then the above-mentioned alloy product that is attached with micro-arc oxidation films is immersed that to carry out painted, painted temperature in the staining trough of having placed staining agent be 60 ℃, the time is 3 minutes, and staining agent is that the trade mark is the browning agent of light K213 forever.Through visual observation, irregular colour is even, and washing easily comes off.
Embodiment 2
According to the method for describing among the embodiment 1 Al alloy parts is carried out differential arc oxidation, different is that differential arc oxidation electrolytic solution is for containing Sodium hexametaphosphate 99 10g/L, Trisodium trimetaphosphate 12.5g/L, the aqueous solution of rose vitriol 6g/L; The time of differential arc oxidation is 7 minutes.
Final acquisition is attached with the alloy product that thickness is 8 microns brown 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 is carried out differential arc oxidation, different is that electrolytic solution is for containing Sodium hexametaphosphate 99 10g/L, Trisodium trimetaphosphate 12.5g/L, the aqueous solution of rose vitriol 4g/L; The time of differential arc oxidation is 4 minutes.
Final obtain to be attached with the alloy product of micro-arc oxidation films that thickness is 6 microns blue or green brown band spot.Through visual observation, color is very even.
Embodiment 4
According to the method for describing among the embodiment 1 Al alloy parts is carried out differential arc oxidation, different is that electrolytic solution is for containing Sodium hexametaphosphate 99 20g/L, Trisodium trimetaphosphate 20g/L, water glass 6g/L, copper sulfate 5g/L, the aqueous solution of sodium wolframate 0.5g/L; The time of differential arc oxidation is 20 minutes.
Final obtain to be attached with the alloy product of micro-arc oxidation films that thickness is 15 microns greyish white colour band spot.Through visual observation, color is very even.
Embodiment 5
According to the method for describing among the embodiment 1 Al alloy parts is carried out differential arc oxidation, different is that electrolytic solution is for containing Sodium hexametaphosphate 99 20g/L, Trisodium trimetaphosphate 15g/L, water glass 8g/L, copper sulfate 0.5g/L, the aqueous solution of potassium permanganate 1.2g/L and sodium hydroxide 6g/L.
Final acquisition is attached with the alloy product that thickness is 9 microns gray micro-arc oxidation films.Through visual observation, color is very even.
Performance test
(1) resistance to soiling test
After picking test solvent Virahol, artificial perspiration, gasoline with cotton respectively, product surface friction 2 minutes, product surface should not have variable color, nothing comes off; Again that test solvent lipstick, hand lotion, foundation cream, edible oil, sterilant, sun screen is even in product surface coating respectively, place water flushing after 24 hours, product surface should not have variable color, no stains are qualified.
Wherein, artificial perspiration's prescription is urea 1g/L, sodium-chlor 5g/L, and lactic acid 1.14g/L, surplus is a water, the pH value is 6.5.
(2) surfaceness test
Testing tool: the 3D contourgraph (Beijing GermanTech Co., Ltd., KLOCKE)
The Ra value on test products surface (arithmetical av of roughness value, testing method: instrument autoscan, display result).
(3) the wear-resisting test of RCA paper tape
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;
(4) pencil hardness test (ASTMD3363-74)
Instrument: pencil hardness meter F130027
The method of inspection: according to ASTM D3363, load: 750 grams, pencil: the UNI of Mitsubishi
(5) 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 8 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.
(6) electrical insulating property
With two test resistance of volt ohm-milliammeter to sample surfaces.
With the product of the resulting Al alloy parts that is formed with micro-arc oxidation films of embodiment 1-4 respectively according to above-mentioned performance test methods carry out that resistance to soiling, scratch resistance, surfaceness, RCA paper tape are wear-resisting, the test of pencil hardness, neutral salt spray corrosion and electrical insulating property, the results are shown in Table 1 in test.
Table 1
| The resistant test | The surface roughness Ra value | RCA paper tape wear resistance (circle) | Pencil hardness (H) | Salt air corrosion ratio (area %) | Electrical insulating property (ohm) | |
| Embodiment 1 | Qualified | 0.578 | 3000 circles | >3H | <5％ | >1000000 |
| Embodiment 2 | Qualified | 0.612 | 3000 circles | >3H | <5％ | >1000000 |
| Embodiment 3 | Qualified | 0.566 | 3000 circles | >3H | <5％ | >1000000 |
| Embodiment 4 | Qualified | 0.604 | 3000 circles | >3H | <5％ | >1000000 |
| Embodiment 5 | Qualified | 0.589 | 3000 circles | >3H | <5％ | >1000000 |
From the result of table 1 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 colored micro-arc oxidation films on the light metal material surface, and the performance of various surface propertys that should the colour micro-arc oxidation films such as resistance to soiling, wear resistance, erosion resistance, surface compact degree is all very high, and hardness is very high.
Claims (10)
1, a kind of electrolytic solution of differential arc oxidation, this electrolytic solution is the aqueous solution that contains phosphoric acid salt and silicate, and the pH value of electrolytic solution is 6-12, it is characterized in that, described electrolytic solution also contains toning agent, and described toning agent is one or more in sodium sulfate, rose vitriol, ammonium meta-vanadate, copper sulfate and the potassium permanganate.
2, electrolytic solution according to claim 1, wherein, phosphatic content is 5-50g/L, and the content of described silicate is 5-50g/L, and the content of described toning agent is 0.1-20g/L.
3, electrolytic solution according to claim 2, wherein, phosphatic content is 20-40g/L, and the content of described silicate is 5-10g/L, and the content of described toning agent is 1-8g/L.
4, according to any described electrolytic solution among the claim 1-3, wherein, described phosphoric acid salt is one or more in Trisodium trimetaphosphate, Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, sodium polyphosphate and the sodium phosphate; Described silicate is water glass and/or potassium silicate.
5, electrolytic solution according to claim 1 and 2, wherein, described electrolytic solution also contains additive, and described additive is one or more in single nickel salt, Sodium orthomolybdate, sodium wolframate, iron(ic) chloride, borax, glycerol and the quadrol.
6, electrolytic solution according to claim 5, wherein, described content of additive is 0.1-20g/L.
7, electrolytic solution according to claim 6, wherein, described content of additive is 1-10g/L.
8, a kind of method of colored 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, 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 1-7.
9, method according to claim 8, wherein, the condition of described differential arc oxidation comprises that current density is 0.5-10A/dm
2, voltage is 0-800V, and the temperature of electrolytic solution is 15-60 ℃, and the time of differential arc oxidation is 2-30 minute.
10, method according to claim 8, wherein, described light metal material is an aluminum or aluminum alloy.
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