CN101210336A - Surface treatment method for light metal material - Google Patents
Surface treatment method for light metal material Download PDFInfo
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- CN101210336A CN101210336A CNA2006101674007A CN200610167400A CN101210336A CN 101210336 A CN101210336 A CN 101210336A CN A2006101674007 A CNA2006101674007 A CN A2006101674007A CN 200610167400 A CN200610167400 A CN 200610167400A CN 101210336 A CN101210336 A CN 101210336A
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Abstract
A surface treatment method of a light metal material comprises the following steps of forming a micro-arc oxide film on the surface of the light metal material, and sequentially subjecting the surface of the light metal material with the micro-arc oxide film to laser etching and anode oxidization. The light metal material obtained by the method in the invention has the advantages of very high hardness, abrasion resistance, corrosion resistance and electrical insulation, strong appearance decoration, bright and diversified color and three-dimensional pattern, thus greatly improving the additional value of the light metal material.
Description
Technical field
The present invention relates to a kind of surface treatment method of light metal material.
Background technology
At present, light metal material, for example aluminium and aluminium alloy, magnesium, titanium and alloy thereof, in light weight with it, specific tenacity is high, rolling property, 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.Therefore in order to overcome the defective of light metal surface aspect of performance, the broadened application scope increases the service life, and need carry out surface treatment to light metal material, in order to solve or to improve protective, ornamental and function.At present, the processing for the light metal material surface mainly is plating, anodic oxidation etc.
Because the physics-chem characteristic of light metal material, especially aluminium and alloy itself thereof makes that the plating on the light metal base material is more much more difficult than the plating on steel substrate, and must carry out some particular processing that therefore, technology is very complicated.
Anodic oxidation is with light metal to light metal material, and for example the aluminum or aluminum alloy material places the process that suitable electrolytic solution is switched on and handled as anode.Through anodic oxidation, it is several microns oxide films to the hundreds of micron that the aluminium surface energy generates thickness.This oxide film is a porous layer, and adsorptivity is very strong, is easy to dyeing or painted, and is painted bright-coloured and be difficult for decorporating, and very strong decoration function is arranged.And the surface of this oxide film is a porous honeycomb, and than the natural oxide film of aluminium alloy, solidity to corrosion, wear resistance are improved.
But on the surface that needs high rigidity, high-wearing feature, for example spool, valve pocket, oil cylinder, cylinder, the surface that needs anti-attrition, for example automobile, power tool, machinery need the higher surface of erosion resistance, for example the preservative coat of chemical industry, ship's fitting, need the higher surface of electrical insulating property, need thermostability, thermal insulation, heat insulation top layer, for example heat-resisting, the heat insulating member of engine just can not meet the demands far away to the light metal material anodic oxidation.
Summary of the invention
The objective of the invention is to overcome the handled light metal surface hardness of above-mentioned prior art, scratch resistance, wear resistance, erosion resistance, defective that electrical insulating property is lower, provide a kind of hardness, wear resistance, erosion resistance, electrical insulating property of light metal surface of both can making higher, and can make light metal surface be easy to painted and have the surface treatment method of the light metal material of aesthetic pattern.
The invention provides a kind of surface treatment method of light metal material, wherein, this surface treatment method comprises light metal material surface formed micro-arc oxidation films, and successively laser sculpture and anodic oxidation carried out in the surface of the light metal material that is formed with micro-arc oxidation films.
Differential arc oxidization technique is a kind of emerging process for treating surface, can form one deck micro-arc oxidation films on various metallic surfaces, and this rete has good wear resistance and erosion resistance, the surface treatment of the material that therefore be used for corrosion-resistant, wears no resistance.According to method provided by the invention, in described differential arc oxidation method, can make light metal material obtain to have the micro-arc oxidation films of excellent surface hardness, scratch resistance, wear resistance, erosion resistance and electrical insulating property, but adopt this method painted relatively poor, also can't realize pattern attractive in appearance.And can obtain pattern attractive in appearance by the laser carving method among the present invention, and carrying out anodic oxidation again, that light metal surface is easy to is painted, and can catch lovely luster and the diversified color of color.
By method provided by the invention, differential arc oxidation is carried out on the light metal material surface earlier handles, carries out then laser sculpture, carries out anodic oxidation treatment again, can so that to the light metal material surface both had hardness, wear resistance, scratch resistance, erosion resistance, the equal advantage of higher of electrical insulating property, and the light metal surface decorative appearance after the dyeing is very strong, bright in luster and diversified, pattern has certain stereoscopic sensation, thereby has promoted its value added greatly.
Embodiment
The surface treatment method of a kind of light metal material provided by the invention comprises light metal material surface is formed micro-arc oxidation films, and successively laser sculpture and anodic oxidation is carried out in the surface of the light metal material that is formed with micro-arc oxidation films.
According to treatment process provided by the invention, of the present invention light metal material surface is formed micro-arc oxidation films is that method by differential arc oxidation forms.The formation method of described micro-arc oxidation films comprises light metal material is placed the electrolyzer that fills electrolyte solution, with the light metal material is anode, electrolyzer is as negative electrode, it is the 5-300 micron that micro-arc discharge oxidation under high pressure, the condition of differential arc oxidation make the thickness of the micro-arc oxidation films of light metal material surface formation.
According to treatment process provided by the invention, the condition of differential arc oxidation comprises that current density is a 0.5-10 peace/decimetre
2, voltage for from 0 volt to 700-800 volt, the temperature of electrolyte solution is 10-50 ℃, the time of differential arc oxidation is 5-50 minute.
According to method provided by the invention, in described differential arc oxidation method, used electrolyte solution is the aqueous solution that contains alkali metal compound, described alkali metal compound is selected from one or more in alkali metal hydroxide, alkali-metal silicate, alkali-metal phosphoric acid salt, alkali-metal borate, alkali-metal aluminate, the alkali-metal fluorochemical, with described electrolyte solution is benchmark, and the content of alkali metal compound is the 5-100 grams per liter.
According to method provided by the invention, in described differential arc oxidation method, described electrolyte solution also preferably contains organic additive and/or inorganic additives, described inorganic additives is selected from described alkali metal compound and does not form the inorganic salt of sedimentary Fe, Cu, V, Ni, W, Mo, Sn and Co and in the sulfide one or more, organic additive is glycerol and/or quadrol, the content of described organic additive be the 0.1-30 milliliter/liter, the content of described inorganic additives is the 0.1-20 grams per liter.Add described organic additive and/or inorganic additives and can improve compactness, homogeneity, resistance to soiling and the scratch resistance of micro-arc oxidation films.
According to method provided by the invention, in described differential arc oxidation method, can make light metal material obtain to have the micro-arc oxidation films of excellent surface hardness, scratch resistance, wear resistance, erosion resistance and electrical insulating property, but adopt this method painted relatively poor, also can't realize pattern attractive in appearance.And can obtain pattern attractive in appearance by the laser carving method among the present invention, and carrying out anodic oxidation again, that light metal surface is easy to is painted, and can catch lovely luster and the diversified color of color.
According to method provided by the invention, described laser carving method is as well known to those skilled in the art.The condition of described laser sculpture makes the surface of the light metal material that is formed with micro-arc oxidation films form clear pattern.The condition of described laser sculpture comprises that the electric current of engraving equipment is the 2-20 peace, and frequency is the 2000-50000 hertz, and wavelength is the 5-1000 nanometer, and intermediate retardation is the 2-30 millisecond.The employed equipment of laser sculpture can be various laser engraving machine well known by persons skilled in the art, for example HSLE-SP, the laser engraving machine of HSLE-XP series, laser marking machine.
According to method provided by the invention, described anode oxidation method is conventionally known to one of skill in the art.Described anodic oxidation comprises sulphuric acid anodizing, oxalic acid and chromic acid anodizing or hard anodizing.Wherein, in the sulphuric acid anodizing method, the composition of electrolytic solution is simple, simple and convenient operation and maintenance, and general only the need gets final product Dilution of sulphuric acid to certain concentration, need not to add other pharmaceutical chemicals, so cost is very low; Sulphuric acid oxidation coating is transparent, and the porous layer adsorptivity is strong, is easy to dyeing and painted, and is painted bright-coloured and be difficult for decorporating, and very strong decoration function is arranged, so anode oxidation method preferably adopts sulphuric acid anodizing.
According to the preferred embodiment of the present invention, the method of this sulphuric acid anodizing comprises that the light metal material that will carry out behind the laser sculpture places the electrolyzer that fills sulphuric acid soln, with the light metal material is anode, electrolyzer is as negative electrode, carry out oxidation, the concentration of sulphuric acid soln is the 140-220 grams per liter, and voltage is the 10-12 volt, temperature is 18-22 ℃, and the time is 20-60 minute.
According to method provided by the invention, described surface treatment method comprises also the light metal material after the anodic oxidation is contacted with dye solution that in the surface colour of light metal material, described method of colouring is conventionally known to one of skill in the art.In the preferred case, the temperature that light metal material contacts with dye solution is 40-80 ℃, and the time is 0.5-10 minute, and the concentration of dye solution is the 0.5-10 grams per liter, and the pH value is 5.0-7.0, and the consumption of dye solution is a 0.1-20 gram/rice
2Base material.
According to method provided by the invention, described dyestuff can adopt any known inorganic dyestuff or organic dye, and organic dye is one or more in matching stain, acidic complex dye, acid mordant dye, substantive dyestuff, weak acid dye, dispersed dye, solubilized vat dye, reactive dyestuffs, basic dyestuff, spirit dyestuff and the oil-soluble dyes for example; Inorganic dyestuff is potassium permanganate solution or iron salt solutions for example.
Method provided by the invention is applicable to various light metal materials, for example can be aluminium, magnesium, titanium, aluminium alloy, magnesium alloy and titanium alloy etc.
According to a kind of preferred implementation of the present invention, the preparation method of light metal material provided by the invention comprises successively: 1. to the light metal base material polish, polishing, degreasing, alkali cleaning; 2. differential arc oxidation is handled; 3. laser sculpture; 4. throwing is stung, changed to degreasing, change throwing, alkali; 5. sulphuric acid anodizing; 6. painted; 7. sealing of hole, oven dry.
The following examples will the present invention is further illustrated.
Embodiment 1
Present embodiment illustrates the surface treatment method of light metal material provided by the invention.
(1) aluminum alloy base material is polished, polishing, degreasing, alkali cleaning.
Adopt the method for artificial polishing that aluminum alloy base material is polished, remove unnecessary stub bar of aluminum alloy base material and burr, polish with sand paper again, up to smoothly getting final product with 1200 purpose sand paperings, aluminum alloy base material after process being polished, polished as degreasing solvent with acetone then cleans 2 times repeatedly.Degreasing finishes, and to adopt sodium hydrate content be that 30 grams per liters, sodium phosphate content are that 40 grams per liters, water glass are that the basic solution of 20 grams per liters cleans aluminum alloy base material in the back.The temperature of cleaning is 85 ℃, and the time of cleaning is 10 minutes.Washed then 5 minutes.
(2) differential arc oxidation is handled
To immerse in the electrolyte solution that contain 1 milliliter/liter of tripoly phosphate sodium STPP 10 grams per liter, sodium phosphate 20 grams per liters, water glass 10 grams per liters, sodium metavanadate 10 grams per liters, rose vitriol 10 grams per liters, glycerol through the Al alloy parts of above processing, with the Al alloy parts is anode, adopts current density 2 peace/decimetres
2, 40 ℃ of temperature, voltage is risen to 700 volts from 0 volt carry out the differential arc oxidation processing, with pneumatic blending electrolyte solution to be stirred therebetween, the treatment time is 12 minutes.Clean up with pure water afterwards and dry up, obtain the Al alloy parts of black differential arc oxidation film layer with air pressure gun.The thickness of micro-arc oxidation films (with German PHYNIX company, the coated layer thickness tester of Pocket-Surfix is measured) is 20 microns.
(3) laser sculpture
The Al alloy parts that above-mentioned differential arc oxidation was handled is 5 peaces with laser engraving machine (model is HSLE-SP) at electric current, and frequency is 5000 hertz, and wavelength is 50 nanometers, and intermediate retardation is a laser carved pattern under 5 milliseconds of conditions.
(4) throwing is stung, changed to degreasing, change throwing, alkali
The Al alloy parts that laser sculpture is good carries out degreasing (R100:45 grams per liter successively; 70 ℃; 5 minutes), change throwing (phosphoric acid 85-95 weight %, surplus is a nitric acid; Normal temperature; 0.2 minute), alkali stings that (concentration is the NaOH of 10 weight %; Normal temperature; 0.1-2 minute) handle, after finishing, the per pass operation all needs to clean up with pure water.
(5) sulphuric acid anodizing
To immerse through the Al alloy parts after the above-mentioned processing and fill in the electrolyzer that concentration is 180 grams per liter aqueous sulfuric acids, with this Al alloy parts as anode, at voltage is that 12 volts, temperature are anodic oxidation 50 minutes under 22 ℃ the condition, takes out and cleans up after finishing anodic oxidation.
(6) painted
With middle the dyeing 10 minutes of the green matching stain aqueous solution (Japan is difficult to understand wild) that the immersion of the Al alloy parts after the anodic oxidation has prepared, the concentration of this matching stain solution is 5 grams per liters, and pH value is 5.6, and the consumption of this matching stain solution is 8 gram/rice
2Base material, painted temperature is 50 ℃, takes out and cleans up after finishing.
(7) sealing of hole, oven dry
Al alloy parts after painted was immersed in the pore-sealing liquid of nickel ion 5 grams per liters sealing 10 minutes, temperature is 85 ℃, finishes that the pure water with 90 ℃ cleans up behind the sealing of hole, and toasts 15 minutes under 60 ℃ of conditions.
Through Al alloy parts is carried out above-mentioned processing, resulting Al alloy parts with the coated layer thickness tester (German PHYNIX company, Pocket-Surfix) recording institute's film forming thickness of shape is 20 microns, substrate is a black, pattern be a green.
Embodiment 2
Present embodiment illustrates the surface treatment method of light metal material provided by the invention.
(1) aluminum alloy base material is polished, polishing, degreasing, alkali cleaning.
Adopt the method for artificial polishing that aluminum alloy base material is polished, remove unnecessary stub bar of aluminum alloy base material and burr, polish with sand paper again, up to smoothly getting final product with 1200 purpose sand paperings, aluminum alloy base material after process being polished, polished as degreasing solvent with acetone then cleans 2 times repeatedly.Degreasing finishes, and to adopt sodium hydrate content be that 30 grams per liters, sodium phosphate content are that 40 grams per liters, water glass are that the basic solution of 20 grams per liters cleans aluminum alloy base material in the back.The temperature of cleaning is 85 ℃, and the time of cleaning is 10 minutes.Washed then 5 minutes.
(2) differential arc oxidation is handled
The above-mentioned Al alloy parts handled well is immersed in the electrolytic solution that contains 25 milliliters/liter of Sodium hexametaphosphate 99 20 grams per liters, sodium hydroxide 5 grams per liters, water glass 5 grams per liters, quadrol, with this Al alloy parts as anode.Adopt current density 1.5 peace/decimetres
2, 35 ℃ of temperature, voltage is risen to 800 volts from 0 volt carry out the differential arc oxidation processing, with pneumatic blending electrolytic solution to be stirred therebetween, the treatment time is 10 minutes.Processing cleans up and dries up with air pressure gun with pure water after finishing, and obtains being formed with the Al alloy parts of white micro-arc oxidation films.The thickness of micro-arc oxidation films (with German PHYNIX company, the coated layer thickness tester of Pocket-Surfix is measured) is 10 microns.
(3) laser sculpture
With laser engraving machine (model is HSLE-SP), is 5 to pacify at electric current with the above-mentioned Al alloy parts of handling through differential arc oxidation, and frequency is 10000 hertz, and wavelength is 100 nanometers, and intermediate retardation is that laser sculpture goes out pattern under 2 milliseconds the condition.
(4) throwing is stung, changed to degreasing, change throwing, alkali
The Al alloy parts that laser sculpture is good carries out degreasing (grease-removing agent R100:45 grams per liter successively; 70 ℃; 10 minutes), change throwing (phosphoric acid 85-95 weight %, surplus is a nitric acid; Normal temperature; 2 minutes), alkali stings that (concentration is the NaOH of 10 weight %; Normal temperature; 2 minutes) handle, all need after the per pass operation to clean up with pure water.
(5) sulphuric acid anodizing
To immerse through the Al alloy parts after the above-mentioned processing and fill in the electrolyzer of aqueous sulfuric acid that concentration is 180 grams per liters, with this Al alloy parts as anode, at voltage is that 12 volts, temperature are that anodic oxidation 35 minutes is taken out after finishing and cleaned up with pure water under 20 ℃ the condition.
(6) painted
Al alloy parts after the anodic oxidation is immersed the middle dyeing of the carmoisine aqueous solution (heavy light) 8 minutes, workpiece is dyed light red, the concentration that is used for painted matching stain solution is 1 grams per liter, and pH value is 5.0, and the consumption of matching stain solution is 12 gram/rice
2Base material, painted temperature is 80 ℃, finishes painted back and takes out and clean up with pure water.
(7) sealing of hole, oven dry
Al alloy parts after painted immersed in the pore-sealing liquid contain nickel ion 5 grams per liters sealing 10 minutes, temperature is 85 ℃, finishes that the pure water with 90 ℃ cleans up behind the sealing of hole, and toasts 15 minutes under 60 ℃ of conditions.
Through Al alloy parts is carried out above-mentioned processing, resulting Al alloy parts with the coated layer thickness tester (German PHYNIX company, Pocket-Surfix) recording institute's film forming thickness of shape is 20 microns, substrate be a white, pattern is a redness.
With the coated layer thickness tester (German PHYNIX company, Pocket-Surfix) recording through the resulting film thickness of above-mentioned treatment process is 10 microns, substrate be white, pattern is a light red.
Performance test
(1) neutral salt spray test
The aluminum alloy materials sample is placed in the salt fog cabinet, sodium chloride brine with 5 ± 0.5 weight % under 35 ℃ sprayed sample after 8 hours, taking-up is observed, and the corroded area of record sample surfaces accounts for the percentage composition (the coating total area is pressed metal coating and calculated) of the coating total area.
(2) the wear-resisting test of RCA paper tape
Use the RCA paper tape wear resistant instrument of model as F350008, friction aluminum alloy material surface coating under 175 gram forces, aluminum alloy material surface coating are milled to when show-through, 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: ASTM D3363, load: 750 grams, pencil: the UNI of Mitsubishi
(4) scratch resistance
Carry out the scratch resistance test with scratching instrument, gauge head is the diamond of 0.75 millimeter of diameter, and test angle is 90 °, apply 1N, 2N, 3N respectively ... power in the sample surface, if apply the following power sample surfaces no marking of 3N (containing), then sample scratch resistance performance is qualified, otherwise is defective.
(5) electrical insulating property
With two test resistance of volt ohm-milliammeter to sample surfaces.
Embodiment 1 and embodiment 2 aluminum alloy materials that obtains of handling are carried out neutral salt spray test, the wear-resisting test of RCA paper tape, pencil hardness test, scratch resistance test and electrical insulating property test respectively, and test result is listed in table 1.
Table 1
| Salt spray corrosion area (area %) | RCA paper tape wear resistance (circle) | Pencil hardness (H) | Scratch resistance (N) | Electrical insulating property (ohm) | |
| Embodiment 1 | ＞1000H (＞9.8 grades) | ＞20000 circles | ＞5H | ＞15 | ＞1000Ω |
| Embodiment 2 | ＞1000H (＞9.8 grades) | ＞20000 circles | ＞5H | ＞15 | ＞1000Ω |
| The permission standard | ＞24H (＞9 grades) | ＞3000 circles | ＞HB | ＞3 | -- |
Claims (11)
1. the surface treatment method of a light metal material is characterized in that, this surface treatment method comprises light metal material surface is formed micro-arc oxidation films, and successively laser sculpture and anodic oxidation is carried out in the surface of the light metal material that is formed with micro-arc oxidation films.
2. method according to claim 1, wherein, the formation method of described micro-arc oxidation films comprises light metal material is placed the electrolyzer that fills electrolyte solution, with the light metal material is anode, electrolyzer is as negative electrode, with the light metal material oxidation, it is the 5-300 micron that the condition of differential arc oxidation makes the thickness of the micro-arc oxidation films of light metal material surface formation.
3. method according to claim 2, wherein, the condition of differential arc oxidation comprises that current density is a 0.5-10 peace/decimetre
2, voltage for from 0 volt to 700-800 volt, the temperature of electrolyte solution is 10-50 ℃, the time of differential arc oxidation is 5-50 minute.
4. method according to claim 2, wherein, used electrolyte solution is the aqueous solution that contains alkali metal compound, described alkali metal compound is selected from one or more in alkali metal hydroxide, alkali-metal silicate, alkali-metal phosphoric acid salt, alkali-metal borate, alkali-metal aluminate, the alkali-metal fluorochemical, with described electrolyte solution is benchmark, and the content of alkali metal compound is the 1-100 grams per liter.
5. method according to claim 2, wherein, used electrolyte solution also contains organic additive and/or inorganic additives, described inorganic additives is selected from described alkali metal compound and does not form the inorganic salt of sedimentary Fe, Cu, V, Ni, W, Mo, Sn and Co and in the sulfide one or more, organic additive is glycerol and/or quadrol, the content of described organic additive be the 0.1-30 milliliter/liter, the content of described inorganic additives is the 0.1-20 grams per liter.
6. method according to claim 1, wherein, the condition of described laser sculpture makes the surface of the light metal material that is formed with micro-arc oxidation films form clear pattern.
7. method according to claim 6, wherein, the condition of described laser sculpture comprises that the electric current of engraving equipment is the 2-20 peace, and frequency is the 2000-50000 hertz, and wavelength is the 5-1000 nanometer, and the intermediate retardation during engraving is the 2-30 millisecond.
8. method according to claim 1, wherein, described anodic oxidation is a sulphuric acid anodizing, and the method for this sulphuric acid anodizing comprises that the light metal material that will carry out behind the laser sculpture places the electrolyzer that fills sulphuric acid soln, is anode with the light metal material, electrolyzer is as negative electrode, carry out oxidation, the concentration of sulphuric acid soln is the 140-220 grams per liter, and voltage is the 10-12 volt, temperature is 18-22 ℃, and the time is 20-60 minute.
9. method according to claim 1, wherein, described surface treatment method also comprises the light metal material after the anodic oxidation is contacted with dye solution, surface colour at light metal material, the temperature of contact is 40-80 ℃, and the time is 0.5-10 minute, and the concentration of dye solution is the 0.5-10 grams per liter, the pH value is 5.0-7.0, and the consumption of dye solution is a 0.1-20 gram/rice
2Base material.
10. method according to claim 9, wherein, described dyestuff is one or more in matching stain, acidic complex dye, acid mordant dye, substantive dyestuff, weak acid dye, dispersed dye, solubilized vat dye, reactive dyestuffs, basic dyestuff, spirit dyestuff and the oil-soluble dyes.
11. method according to claim 1, wherein, described light metal is magnesium, aluminium, titanium, magnesium alloy, aluminium alloy or titanium alloy.
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