CN102230205B - Aluminum alloy micro-arc oxidation black ceramic membrane and preparation method thereof - Google Patents
Aluminum alloy micro-arc oxidation black ceramic membrane and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a method for preparing an aluminum alloy micro-arc oxidation black ceramic membrane, which comprises the following steps of: preparing electrolyte solution by using 5 to 30 grams of sodium silicate, 10 to 30 grams of sodium phosphate, 3 to 10 grams of vanadate, 5 to 30 grams of sodium tungstate, 1 to 5 grams of sodium hydroxide and 1 to 10 grams of hexamethylenetetramine and by mixing, and adding 1 liter of distilled water; performing micro-arc oxidation, namely immersing aluminum alloy serving as an anode and a stainless steel sheet serving as a cathode in the electrolyte solution, after performing the micro-arc oxidation by using an alternating-current pulse power supply, taking the aluminum alloy out, and cleaning and drying to prepare the required micro-arc oxidation black ceramic membrane. By the method, a black ceramic layer which is high in corrosion resistance and uniform in colors and luster is formed on the surface of the aluminum alloy; and the method is high in efficiency, low in cost and small in environment pollution.
Description
Technical field
The present invention relates to the aluminum alloy surface processing technology field, specifically a kind of aluminum alloy micro-arc oxidation black and preparation method thereof.
Background technology
Aluminium alloy has that specific tenacity is high, heat-conductivity conducting good, shaping processability is good, nonmagnetic and the premium properties such as easy to be recycled and being widely used, especially along with manufacturing fast development, aluminium and alloy thereof have become the main raw that lightweight is manufactured, are the Equations of The Second Kind metallic substance that usage quantity is only second to iron and steel.Yet, the electropotential of aluminium alloy is extremely low, is exposed in wet environment, especially in acid or alkaline atmosphere, aluminium alloy very easily corrosion makes its application be restricted, and aluminium alloy is because matrix hardness is low, wearing no resistance makes its range of application narrower.Therefore aluminium alloy needs could meet through corresponding surface treatment the requirement of environment for use before use, improves the surface hardness, wear resistance, solidity to corrosion of aluminium alloy and ornamentally just becomes in current aluminium alloy application urgent problem.
Differential arc oxidation (MAO) claims again anodic spark deposition (A SD), this technology is that non-ferrous metal (A l, T i, Ta, M g etc.) and alloy thereof are placed in to electrolytic solution, in solution, ionization of gas, oxidation on metal surface produce plasma body under the highfield effect, make matrix surface produce microcell spark discharge spot, under the acting in conjunction of the series of complexes such as thermochemistry, plasma chemistry, electrochemistry, diffusion reaction, high-temperature phase-change reaction, generate have high rigidity, the insulativity oxide film of high bond strength, the characteristics such as wear-resisting, anti-corrosion.
Eighties of last century the '30s, people's reported first such as Gunterschules the aluminum alloy anode Spark Discharges, found afterwards that this phenomenon also can be used for preparing oxide film, was applied to magnesium alloy anticorrosion at first.From eighties of last century seventies, the U.S., Germany and USSR (Union of Soviet Socialist Republics) all start the research of this respect in succession, and to the eighties in 20th century, German scholar P.Kurze utilizes spark discharge successfully to obtain Al at surface of pure aluminum
2O
3Hard film layer, differential arc oxidization technique has had remarkable progress.Middle and later periods eighties differential arc oxidization technique just really becomes study hotspot and starts to enter the industrial production application.China pays close attention to this technology since the nineties in 20th century, at present oneself moves towards the practical stage aspect wear-resisting, decorative coating.
Along with being gradually improved and the expansion of Application Areas of aluminum alloy differential arc oxidation process for treating surface, the aluminum alloy differential arc oxidation process for treating surface has been proposed to ornamental demand, due to Film color dull (mostly being grey), wish that differential arc oxidization technique can realize the diversification of color and luster, wherein black ceramic membrane, because having unique optical function and ceramic performance, all is being widely used aspect protection, optical property and the decoration of material.
Aspect the painted research of aluminum alloy differential arc oxidation, do not find external relevant document; More research has been done to aluminum alloy differential arc oxidation is painted by domestic many units, but few to the preparation research of aluminum alloy differential arc oxidation black film, its research has following characteristics: contain highly toxic substance in (1) solution; As: Wuhan University of Technology is by adding the Tripotassium iron hexacyanide (K
3[Fe (CN)
6]), six cyanogen close the sour potassium (K of iron (II)
4[Fe (CN)
6] 3H
2O) at aluminum alloy surface differential arc oxidation painted (Zhang Wenfan aluminum alloy surface differential arc oxidation coloring process and power supply research [D] .2009 Wuhan University of Technology master thesis thereof).(2) treatment time long, what have even reaches 100min; As Wuhan University of Technology at Na
3PO
4, Na
2WO
4, KOH, HBO
3Electrolytic solution in process 110min and obtain black film (the affect 2008 Wuhan University of Technology master thesis of the big processing parameter of Kuang Chun on aluminum alloy micro-arc oxidation black film forming rule); (3) complex process, pre-treatment need oil removing, alkaline etching, pickling oven dry etc., also need before painted differential arc oxidation to generate ceramics based basement membrane layer; As University Of Chongqing, be that to become embrane method and W-P-Mo be that oxidation step becomes embrane method to prepare black ceramic membrane (Zhang Jinbin aluminum alloy surface micro-plasma oxidation black ceramic membrane preparation technology and membrane formation mechanism research 2005 University Of Chongqing's master thesis) thereof in LC4, LY12 aluminum alloy surface to second oxidation with Fe-Cr-Co.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of aluminum alloy micro-arc oxidation black and preparation method thereof is provided, black ceramic membrane process prepared by technique of the present invention is simple, cost is low, environmental pollution is little, and the black ceramic membrane solidity to corrosion generated in aluminum alloy surface is good, color and luster is even.
Realize the technical scheme that the object of the invention adopts:
A kind of preparation method of aluminum alloy micro-arc oxidation black, comprise the steps:
(1) configuration electrolytic solution: take water glass 5～30g, sodium phosphate 10～30g, vanadate 3～10g, sodium wolframate 5～30g, sodium hydroxide 1～5g and hexamethylenetetramine 1～10g, add after mixing in 1L distilled water and be configured to electrolytic solution;
(2) differential arc oxidation: as anode, stainless steel substrates is negative electrode by aluminium alloy, and is immersed in fully in the electrolytic solution in step (1), after adopting AC pulse power supply to carry out the differential arc oxidation processing, aluminium alloy is taken out, clean, drying, can make required differential arc oxidation black ceramic membrane.
Aluminium alloy in described step (2) is also process polishing, cleaning and dry pre-treatment before using.
In described step (1), the pH value of electrolytic solution is 8.0～11.0.
In described step (2), the parameter of AC pulse power supply is respectively: forward voltage 200～600V, negative voltage 100～400v, current density 3～12A/dm
2, frequency 100HZ～800HZ, dutycycle 10%～50%, oxidization time 5～40min.
" L a b standard colorimetric system " CIE.1976-Lab colorimeter system L, a, b value that the evaluating basis International Commission on Illumination (CIE) of color is recommended show color, and L represents brightness, and scope is 0～100, and black is 0, and white is 100; A be by green to red color change, scope is-128～+ 128; B be by indigo plant to yellow color change, scope is-128～+ 128.
Adopt the color of spectrophotometric determination rete, under white background, carry out colourimetric number mensuration with spectrophotometer, each sample pros and cons is respectively measured 3 times, gets its mean value.The Lab value of ater (0,0,0) aberration
The homogeneity of reaction color.
Compared with prior art, the present invention has following advantage and beneficial effect:
The present invention gives birth to and all becomes the black ceramic layer that color and luster is even, aberration is little, solidity to corrosion is good in aluminum alloy surface by the composite electrolytic solution of phosphoric acid salt-silicate, adding hexamethylenetetramine, adding the differential arc oxidation film layer blackness and the increase of color and luster homogeneity, the aberration that after hexamethylenetetramine, obtain reduces, roughness reduces, membrane uniformity and solidity to corrosion significantly improve, and the present invention also has the advantages such as efficiency is high, technique is simple, environmental pollution is little.
The accompanying drawing explanation
Fig. 1 is the square section scanning electron microscope (SEM) photograph of the differential arc oxidation black film that makes in not adding hexamethylenetetramine electrolytic solution of the embodiment of the present invention 2 aluminium alloys; Wherein (a) is for amplifying 1000 times of photos, (b) for amplifying 5000 times of photos;
The square section scanning electron microscope (SEM) photograph of Fig. 2 embodiment of the present invention 2 aluminium alloys make in adding hexamethylenetetramine electrolytic solution differential arc oxidation black film; Wherein (a) is for amplifying 1000 times of photos, (b) for amplifying 5000 times of photos;
Fig. 3 black film that is aluminium alloy of the present invention after not adding differential arc oxidation prepared in having added hexamethylenetetramine electrolytic solution by the neutralization of hexamethylenetetramine electrolytic solution, and with the electrokinetic potential polarization curve comparison diagram of aluminum matrix alloy; Wherein curve 1 is alloy matrix aluminum; Curve 2 is potential polarization curves of the differential arc oxidation black film for preparing in not adding hexamethylenetetramine electrolytic solution of aluminium alloy; Curve 3 is potential polarization curves of the differential arc oxidation black film for preparing in adding hexamethylenetetramine electrolytic solution of aluminium alloy.
Embodiment
Below in conjunction with specific embodiment, the present invention is more specifically described in detail, but embodiments of the present invention are not limited to this, the processing parameter for not indicating especially, can carry out with reference to routine techniques.
Embodiment 1:
Aluminum alloy differential arc oxidation black film preparation method, comprise the steps:
(1) pre-treatment: the aluminium alloy extrusions (thickness 2mm) that is 6063 from model intercepts 4x4cm
2Sample, with the SiC sand paper of 220#, 600#, 800#, polish smooth to the surface scratch direction specimen surface consistent successively, then by washed with de-ionized water, dry up standbyly, it is to remove oxide compound and the grease of aluminum alloy surface that aluminium alloy is carried out to pretreated purpose.
(2) preparation electrolytic solution: at room temperature take water glass 10g, sodium phosphate 10g, sodium wolframate 15g, vanadate 5g, sodium hydroxide 2g, add after mixing in 1l distilled water, by magnetic stirrer, it is fully dissolved.
(3) aluminum alloy differential arc oxidation is painted
Using the pretreated aluminum alloy specimen of above-mentioned process as anode, and immerse fully in the above-mentioned electrolytic solution prepared, stainless steel substrates, as negative electrode, is fixed on anode apart from the 10cm place with fixture, and with it over against, adopt AC pulse power supply to carry out the differential arc oxidation processing to aluminium alloy; The power acquisition operator scheme of constant current, each power parameter is: forward voltage 550V, negative voltage 350V, current density 6A/dm
2, frequency 150HZ, dutycycle 30%, oxidization time 20min, after parameter setting, sample is carried out to the differential arc oxidation processing.
(4) cleaning, drying
After being disposed, take out aluminum alloy specimen, rinse with tap water, soaked ten minutes in distilled water, take out air-dryly, can obtain aluminum alloy micro-arc oxidation black.Its outward appearance is even, average roughness Ra: 1.72 μ m, Lab mean value (25.76; 0.91; 0.84), Lab standard deviation (0.128; 0.057; 0.008); Aberration △ E=0.140.
Embodiment 2:
(1) pre-treatment: with
Embodiment 1.
(2) preparation electrolytic solution: at room temperature take water glass 10g, sodium phosphate 20g, sodium wolframate 15g, vanadate 8g, sodium hydroxide 2g, add after mixing in 1l distilled water, by magnetic stirrer, it is fully dissolved.
(3) aluminum alloy differential arc oxidation is painted
Using the pretreated aluminum alloy specimen of above-mentioned process as anode, and immerse fully in the above-mentioned electrolytic solution prepared, stainless steel substrates, as negative electrode, is fixed on anode apart from the 10cm place with fixture, and with it over against, adopt AC pulse power supply to carry out the differential arc oxidation processing to aluminium alloy; The power acquisition operator scheme of constant current, each power parameter is: forward voltage 550V, negative voltage 350V, current density 6A/dm
2, frequency 150HZ, dutycycle 30%, oxidization time 20min, after parameter setting, sample is carried out to the differential arc oxidation processing.
(4) cleaning, drying
After being disposed, take out aluminum alloy specimen, rinse with tap water, soaked ten minutes in distilled water, take out air-dryly, can obtain aluminum alloy micro-arc oxidation black.Its outward appearance is even, average roughness Ra: 3.03 μ m, Lab mean value (28.14; 0.62; 1.15); Lab standard deviation (0.076; 0.039; 0.086); Aberration △ E=0.121.
Embodiment 3:
(1) pre-treatment: with
Embodiment 1.
(2) preparation of the painted treatment solution of aluminum alloy differential arc oxidation: at room temperature take water glass 10g, sodium phosphate 20g, sodium wolframate 15g, vanadate 8g, sodium hydroxide 2g, hexamethylenetetramine (C
6H
12N
4) 4g, after mixing, add in 1l distilled water, by magnetic stirrer, it is fully dissolved.
(3) aluminum alloy differential arc oxidation is painted
Using the pretreated aluminum alloy specimen of above-mentioned process as anode, and immerse fully in the above-mentioned electrolytic solution prepared, stainless steel substrates, as negative electrode, is fixed on anode apart from the 10cm place with fixture, and with it over against, adopt AC pulse power supply to carry out the differential arc oxidation processing to aluminium alloy; The power acquisition operator scheme of constant current, each power parameter is: forward voltage 550V, negative voltage 350V, current density 9A/dm
2, frequency 150HZ, dutycycle 30%, oxidization time 15min, after parameter setting, sample is carried out to the differential arc oxidation processing.
(4) cleaning, drying
After being disposed, take out aluminum alloy specimen, rinse with tap water, soaked ten minutes in distilled water, take out air-dryly, can obtain aluminum alloy micro-arc oxidation black.Its outward appearance is even, average roughness Ra: 2.34 μ m, Lab mean value (27.88; 0.27; 0.54); Lab standard deviation (0.065; 0.005; 0.039); Aberration △ E=0.076.
Embodiment 4:
(1) pre-treatment: with
Embodiment 1.
(2) preparation of the painted treatment solution of aluminum alloy differential arc oxidation: at room temperature take water glass 10g, sodium phosphate 20g, sodium wolframate 15g, vanadate 8g, sodium hydroxide 2g, hexamethylenetetramine (C
6H
12N
4) 6g, after mixing, add in 1l distilled water, by magnetic stirrer, it is fully dissolved.
(3) aluminum alloy differential arc oxidation is painted
Using the pretreated aluminum alloy specimen of above-mentioned process as anode, and immerse fully in the above-mentioned electrolytic solution prepared, stainless steel substrates, as negative electrode, is fixed on anode apart from the 10cm place with fixture, and with it over against, adopt AC pulse power supply to carry out the differential arc oxidation processing to aluminium alloy; The power acquisition operator scheme of constant current, each power parameter is: forward voltage 550V, negative voltage 350V, current density 6A/dm
2, frequency 150HZ, dutycycle 30%, oxidization time 20min, after parameter setting, sample is carried out to the differential arc oxidation processing.
(4) cleaning, drying
After being disposed, take out aluminum alloy specimen, rinse with tap water, soaked ten minutes in distilled water, take out air-dryly, can obtain aluminum alloy micro-arc oxidation black.。Its outward appearance is even, average roughness Ra: 1.20 μ m, Lab mean value (27.29; 0.47; 0.33); Lab standard deviation (0.017; 0; 0.012); Aberration △ E=0.021.
Below the differential arc oxidation in not adding hexamethylenetetramine and having added the electrolytic solution of hexamethylenetetramine carries out interpretation of result as an example with aluminium alloy, and analytical results is as follows:
(1) sem analysis
As shown in Fig. 1 (a) and Fig. 2 (a), there are a large amount of molten materials in aluminium alloy generates in not adding the electrolytic solution of hexamethylenetetramine black differential arc oxidation film layer surface, and covered the electric discharge micropore, make rete rough and uneven in surface, and electric discharge micropore skewness.Obvious variation (as Fig. 1 (b), Fig. 2 (b)) has occurred in aluminium alloy generates in the electrolytic solution that adds hexamethylenetetramine black micro-arc oxidation films microcosmic, micropore on rete is evenly distributed, stores around micropore disappears, and homogeneity and the compactness of rete are significantly improved.
(2) chemical property analysis
Utilize electrokinetic potential polarization to investigate alloy matrix aluminum, aluminium alloy generate in not adding the electrolytic solution of hexamethylenetetramine black micro-arc oxidation films and aluminium alloy generate in the electrolytic solution that adds hexamethylenetetramine black micro-arc oxidation films, corrosion resisting property in the NaCl of the 3.5wt% aqueous solution respectively, result as shown in Figure 3 and Table 1, with alloy matrix aluminum, compare the corrosion electric current density (i of aluminium alloy generates in not adding the electrolytic solution of hexamethylenetetramine black micro-arc oxidation films
Corr) reduced by 1 order of magnitude; Corrosion electric current density (the i of aluminium alloy generates in the electrolytic solution that adds hexamethylenetetramine black micro-arc oxidation films
Corr) having reduced by 3 orders of magnitude, corrosion electric current density is less, and the solidity to corrosion of rete is better.Illustrating and add the solidity to corrosion that hexamethylenetetramine can improve rete greatly, is that rete is finer and close because hexamethylenetetramine can make the surface of rete more uniform and smooth, and impurity and corrosive deposit are not easy to enter rete, and corrosion is difficult to carry out.
The electrochemical parameter of table 1 electrokinetic potential polarization curve
| Sequence number | Sample | icorr(μA·cm-2) | Ecorr/V |
| 1 | Aluminum substrate | 5.248 | -0.761 |
| 2 | |
0.165 | -0.782 |
| 3 | |
0.0063 | -0.870 |
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (4)
1. the preparation method of an aluminum alloy micro-arc oxidation black, is characterized in that, comprises the steps:
(1) configuration electrolytic solution: take water glass 5～30g, sodium phosphate 10～30g, vanadate 3～10g, sodium wolframate 5～30g, sodium hydroxide 1～5g and hexamethylenetetramine 1～10g, add after mixing in 1L distilled water and be configured to electrolytic solution;
(2) differential arc oxidation: as anode, stainless steel substrates is negative electrode by aluminium alloy, and is immersed in fully in the electrolytic solution in step (1), after adopting AC pulse power supply to carry out the differential arc oxidation processing, aluminium alloy is taken out, clean, drying, can make required differential arc oxidation black ceramic membrane.
2. preparation method according to claim 1, is characterized in that, the aluminium alloy in described step (2) is also process polishing, cleaning and dry pre-treatment before using.
3. preparation method according to claim 1 and 2, is characterized in that, in described step (1), the pH value of electrolytic solution is 8.0～11.0.
4. preparation method according to claim 3, is characterized in that, in described step (2), the parameter of AC pulse power supply is respectively: forward voltage 200～600V, negative voltage 100～400v, current density 3～12A/dm
2, frequency 100Hz～800Hz, dutycycle 10%～50%, oxidization time 5～40min.
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| CN113622010B (en) * | 2021-08-31 | 2022-12-16 | 日照微弧技术有限公司 | Aluminum alloy surface black ceramic membrane and preparation method thereof |
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| CN114921832B (en) * | 2022-06-07 | 2024-02-13 | 常州大学 | Method for generating black ceramic film on surface of titanium alloy |
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| CN101445949A (en) * | 2007-11-27 | 2009-06-03 | 比亚迪股份有限公司 | Micro-arc oxidation electrolyte and micro-arc oxidation method |
| CN101270495B (en) * | 2008-04-21 | 2010-10-27 | 华南理工大学 | Method for preparing corrosion protection abrasion resistant ceramic coating with alloy surface differential arc oxidization |
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