CN102230205A - 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 is a kind of aluminum alloy differential arc oxidation black ceramic membrane and preparation method thereof.
Background technology
Premium propertiess such as aluminium alloy has the specific tenacity height, heat-conductivity conducting is good, shaping processability is good, nonmagnetic and easy to be recycled and obtained widely using, especially along with manufacturing fast development, aluminium and alloy thereof have become the main raw that lightweight is made, and the amount of being to use is only second to second metalloid material of iron and steel.Yet, the electropotential of aluminium alloy is extremely low, is exposed in the wet environment, especially in acid or alkaline atmosphere, aluminium alloy very easily corrodes makes its application be restricted, and aluminium alloy is low owing to matrix hardness, wearing no resistance makes that its range of application is narrower.Therefore aluminium alloy needs could satisfy through corresponding surface treatment the requirement of environment for use before use, improve aluminium alloy surface hardness, wear resistance, solidity to corrosion and ornamental just become current aluminium alloy use in urgent problem.
Differential arc oxidation (MAO) claims anode spark deposition (A SD) again, this technology is that non-ferrous metal (A l, T i, Ta, M g etc.) and alloy thereof are placed electrolytic solution, ionization of gas, oxidation on metal surface produce plasma body in the solution under the highfield effect, make matrix surface produce microcell spark discharge spot, under the acting in conjunction of a series of complex reactions such as thermochemistry, plasma chemistry, electrochemistry, diffusion reaction, high-temperature phase-change, generate have high rigidity, the insulativity oxide film of high bond strength, characteristics such as wear-resisting, anti-corrosion.
Eighties of last century the '30s, people's reported first such as Gunterschules aluminum alloy anode spark discharge phenomenon, found afterwards that this phenomenon also can be used for preparing oxide film, it is anticorrosion to be applied to magnesium alloy at first.From eighties of last century seventies, the U.S., Germany and USSR (Union of Soviet Socialist Republics) all begin 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 on the fine aluminium surface
2O
3Hard film layer, differential arc oxidization technique has had remarkable progress.Middle and later periods eighties differential arc oxidization technique just really becomes the research focus and begins to enter industrial production to be used.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 ornamental demand, because rete color dullness (mostly being grey), wish that differential arc oxidization technique can realize the diversification of color and luster, wherein black ceramic membrane all is being widely used aspect protection, optical property and the decoration of material because of having unique optical function and ceramic performance.
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, have in addition reach 100min; As Wuhan University of Technology at Na
3PO
4, Na
2WO
4, KOH, HBO
3Electrolytic solution in handle 110min and obtain black film (the big processing parameter of Kuang Chun is to the 2008 Wuhan University of Technology's master thesis that influence of aluminum alloy differential arc oxidation black ceramic membrane film forming rule); (3) complex process, pre-treatment need oil removing, alkaline etching, pickling oven dry etc., also need differential arc oxidation to generate ceramics based basement membrane layer before painted; Is 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 thereof are studied 2005 University Of Chongqing's master thesis) in LC4, LY12 aluminum alloy surface to second oxidation as University Of Chongqing with Fe-Cr-Co.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of aluminum alloy differential arc oxidation black ceramic membrane and preparation method thereof is provided, the black ceramic membrane process of prepared of the present invention is simple, cost is low, environmental pollution is little, and the black ceramic membrane solidity to corrosion that generates in aluminum alloy surface is good, color and luster is even.
Realize the technical scheme that the object of the invention adopted:
A kind of preparation method of aluminum alloy differential arc oxidation black ceramic membrane comprises the steps:
(1) configuration electrolytic solution: take by weighing water glass 5～30g, sodium phosphate 10～30g, vanadate 3～10g, sodium wolframate 5～30g, sodium hydroxide 1～5g and hexamethylenetetramine 1～10g, mix in the back adding 1L distilled water being configured to electrolytic solution;
(2) differential arc oxidation: as anode, stainless steel substrates is a negative electrode with aluminium alloy, and is immersed in fully in the electrolytic solution in the step (1), after adopting the alternating-current 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 the described step (2) also passes through polishing, cleaning and exsiccant pre-treatment before using.
The pH value of electrolytic solution is 8.0～11.0 in the described step (1).
The parameter of alternating-current pulse power supply is respectively in the described step (2): 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 is that scope is-128～+ 128 by the color change of indigo plant to Huang.
Adopt the color of spectrophotometric determination rete, under white background, carry out colourimetric number with spectrophotometer and measure, 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 in aluminum alloy surface by interpolation hexamethylenetetramine in the composite electrolytic solution of phosphoric acid salt-silicate and all becomes the black ceramic layer that color and luster is even, aberration is little, solidity to corrosion is good, adding the differential arc oxidation film layer blackness and the increase of color and luster homogeneity, the aberration that are obtained behind the hexamethylenetetramine reduces, roughness reduces, membrane uniformity and solidity to corrosion significantly improve, and the present invention also has advantages such as efficient height, technology is simple, environmental pollution is little.
Description of drawings
Fig. 1 is the square section sem photograph of the differential arc oxidation black film that makes in not adding hexamethylenetetramine electrolytic solution of the embodiment of the invention 2 aluminium alloys; Wherein (a) is for amplifying 1000 times of photos, (b) for amplifying 5000 times of photos;
The square section sem photograph of the differential arc oxidation black film that Fig. 2 embodiment of the invention 2 aluminium alloys make in adding hexamethylenetetramine electrolytic solution; 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 the neutralization of hexamethylenetetramine electrolytic solution to have added the differential arc oxidation for preparing in the hexamethylenetetramine electrolytic solution, and with the electrokinetic potential polarization curve comparison diagram of aluminum matrix alloy; Wherein curve 1 is an 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 done further concrete detailed description the in detail, but embodiments of the present invention are not limited thereto, 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 comprises the steps:
(1) pre-treatment: from model is 6063 aluminium alloy extrusions (thickness 2mm) intercepting 4x4cm
2Sample, SiC sand paper with 220#, 600#, 800# polishes smooth specimen surface to surface scratch direction unanimity successively, then with washed with de-ionized water, dry up standbyly, it is to remove the oxide compound and the grease of aluminum alloy surface that aluminium alloy is carried out pretreated purpose.
(2) preparation electrolytic solution: at room temperature take by weighing water glass 10g, sodium phosphate 10g, sodium wolframate 15g, vanadate 5g, sodium hydroxide 2g, mix the back and add in the 1l distilled water, it is fully dissolved with magnetic stirrer.
(3) aluminum alloy differential arc oxidation is painted
With the pretreated aluminum alloy specimen of above-mentioned process as anode, and immerse fully in the above-mentioned electrolytic solution for preparing, stainless steel substrates is as negative electrode, with anchor clamps be fixed on anode apart from the 10cm place, and with it over against, adopt the alternating-current pulse power supply that aluminium alloy is carried out differential arc oxidation and handle; Power supply adopts the operator scheme of constant current, and each power parameter is: forward voltage 550V, negative voltage 350V, current density 6A/dm
2, frequency 150HZ, dutycycle 30%, oxidization time 20min, behind the parameter setting sample is carried out differential arc oxidation and handles.
(4) cleaning, drying
After disposing, take out aluminum alloy specimen,, in distilled water, soaked ten minutes, take out air-dryly, can obtain the aluminum alloy differential arc oxidation black ceramic membrane with the tap water flushing.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 by weighing water glass 10g, sodium phosphate 20g, sodium wolframate 15g, vanadate 8g, sodium hydroxide 2g, mix the back and add in the 1l distilled water, it is fully dissolved with magnetic stirrer.
(3) aluminum alloy differential arc oxidation is painted
With the pretreated aluminum alloy specimen of above-mentioned process as anode, and immerse fully in the above-mentioned electrolytic solution for preparing, stainless steel substrates is as negative electrode, with anchor clamps be fixed on anode apart from the 10cm place, and with it over against, adopt the alternating-current pulse power supply that aluminium alloy is carried out differential arc oxidation and handle; Power supply adopts the operator scheme of constant current, and each power parameter is: forward voltage 550V, negative voltage 350V, current density 6A/dm
2, frequency 150HZ, dutycycle 30%, oxidization time 20min, behind the parameter setting sample is carried out differential arc oxidation and handles.
(4) cleaning, drying
After disposing, take out aluminum alloy specimen,, in distilled water, soaked ten minutes, take out air-dryly, can obtain the aluminum alloy differential arc oxidation black ceramic membrane with the tap water flushing.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 by weighing water glass 10g, sodium phosphate 20g, sodium wolframate 15g, vanadate 8g, sodium hydroxide 2g, hexamethylenetetramine (C
6H
12N
4) 4g, mix the back and add in the 1l distilled water, with magnetic stirrer it is fully dissolved.
(3) aluminum alloy differential arc oxidation is painted
With the pretreated aluminum alloy specimen of above-mentioned process as anode, and immerse fully in the above-mentioned electrolytic solution for preparing, stainless steel substrates is as negative electrode, with anchor clamps be fixed on anode apart from the 10cm place, and with it over against, adopt the alternating-current pulse power supply that aluminium alloy is carried out differential arc oxidation and handle; Power supply adopts the operator scheme of constant current, and each power parameter is: forward voltage 550V, negative voltage 350V, current density 9A/dm
2, frequency 150HZ, dutycycle 30%, oxidization time 15min, behind the parameter setting sample is carried out differential arc oxidation and handles.
(4) cleaning, drying
After disposing, take out aluminum alloy specimen,, in distilled water, soaked ten minutes, take out air-dryly, can obtain the aluminum alloy differential arc oxidation black ceramic membrane with the tap water flushing.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 by weighing water glass 10g, sodium phosphate 20g, sodium wolframate 15g, vanadate 8g, sodium hydroxide 2g, hexamethylenetetramine (C
6H
12N
4) 6g, mix the back and add in the 1l distilled water, with magnetic stirrer it is fully dissolved.
(3) aluminum alloy differential arc oxidation is painted
With the pretreated aluminum alloy specimen of above-mentioned process as anode, and immerse fully in the above-mentioned electrolytic solution for preparing, stainless steel substrates is as negative electrode, with anchor clamps be fixed on anode apart from the 10cm place, and with it over against, adopt the alternating-current pulse power supply that aluminium alloy is carried out differential arc oxidation and handle; Power supply adopts the operator scheme of constant current, and each power parameter is: forward voltage 550V, negative voltage 350V, current density 6A/dm
2, frequency 150HZ, dutycycle 30%, oxidization time 20min, behind the parameter setting sample is carried out differential arc oxidation and handles.
(4) cleaning, drying
After disposing, take out aluminum alloy specimen,, in distilled water, soaked ten minutes, take out air-dryly, can obtain the aluminum alloy differential arc oxidation black ceramic membrane with the tap water flushing.。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.
Carry out interpretation of result with aluminium alloy as an example at the differential arc oxidation that does not add hexamethylenetetramine and added in the electrolytic solution of hexamethylenetetramine below, analytical results is as follows:
(1) sem analysis
Shown in Fig. 1 (a) and Fig. 2 (a), there are a large amount of molten materials in the black micro-arc oxidation films laminar surface that aluminium alloy generates in not adding the electrolytic solution of hexamethylenetetramine, and covered the discharge micropore, make rete rough and uneven in surface, and discharge micropore skewness.The black micro-arc oxidation films microcosmic that aluminium alloy generates in the electrolytic solution that adds hexamethylenetetramine has taken place than obvious variation (as Fig. 1 (b), Fig. 2 (b)), micropore on the rete is evenly distributed, stores around the micropore disappears, and the homogeneity and the compactness of rete are significantly improved.
(2) chemical property analysis
Utilize electrokinetic potential polarization to investigate the black micro-arc oxidation films that black micro-arc oxidation films that alloy matrix aluminum, aluminium alloy generate and aluminium alloy generate in not adding the electrolytic solution of hexamethylenetetramine in the electrolytic solution that adds hexamethylenetetramine, corrosion resisting property in the NaCl of the 3.5wt% aqueous solution respectively, the result is shown in Fig. 3 and table 1, compare the corrosion electric current density (i of the black micro-arc oxidation films that aluminium alloy generates in not adding the electrolytic solution of hexamethylenetetramine with alloy matrix aluminum
Corr) reduced by 1 order of magnitude; Corrosion electric current density (the i of the black micro-arc oxidation films that aluminium alloy generates in the electrolytic solution that adds hexamethylenetetramine
Corr) having reduced by 3 orders of magnitude, corrosion electric current density is more little, and the solidity to corrosion of rete is good more.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/ |
| 1 | Aluminum substrate | 5.248 | -0.761 |
| 2 | |
0.165 | -0.782 |
| 3 | Embodiment 4 | 0.0063 | -0.870 |
The foregoing description is a preferred implementation 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 the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (4)
1. the preparation method of an aluminum alloy differential arc oxidation black ceramic membrane is characterized in that, comprises the steps:
(1) configuration electrolytic solution: take by weighing water glass 5～30g, sodium phosphate 10～30g, vanadate 3～10g, sodium wolframate 5～30g, sodium hydroxide 1～5g and hexamethylenetetramine 1～10g, mix in the back adding 1L distilled water being configured to electrolytic solution;
(2) differential arc oxidation: as anode, stainless steel substrates is a negative electrode with aluminium alloy, and is immersed in fully in the electrolytic solution in the step (1), after adopting the alternating-current 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 the described step (2) also passes through polishing, cleaning and exsiccant pre-treatment before using.
3. preparation method according to claim 1 and 2 is characterized in that, the pH value of electrolytic solution is 8.0～11.0 in the described step (1).
4.. preparation method according to claim 3 is characterized in that, the parameter of alternating-current pulse power supply is respectively in the described step (2): 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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