CN107893250A - A kind of preparation technology of golden oxidized aluminum alloy layer - Google Patents
A kind of preparation technology of golden oxidized aluminum alloy layer Download PDFInfo
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- CN107893250A CN107893250A CN201711295229.2A CN201711295229A CN107893250A CN 107893250 A CN107893250 A CN 107893250A CN 201711295229 A CN201711295229 A CN 201711295229A CN 107893250 A CN107893250 A CN 107893250A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/12—Anodising more than once, e.g. in different baths
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/14—Producing integrally coloured layers
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/16—Pretreatment, e.g. desmutting
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Abstract
The invention discloses a kind of preparation technology of golden oxidized aluminum alloy layer, including:S01, pre-treatment:6063 aluminium alloys are subjected to degreasing, alkali cleaning, washing, neutralization, washing;S02:Active oxidation:Aluminium alloy after S01 is handled inserts progress electrolysis, activation oxidation in active oxidation liquid;S03, re-electrolysis processing:Aluminium alloy after pre-treatment is subjected to electrolytic oxidation in the electrolytic solution;S04, removal of impurities:The oxide-film being prepared is soaked in removal of impurities liquid and carries out removal of impurities processing.The configuration of adaptability has been carried out to pre-treating technology and activating process in electrolysis process in the present invention, make pre-treating technology and activating process more reasonable, it can promote the generation of micro-arc oxidation process, and make it that ceramic layer caused by electrolysis is uniform, fine and close, wear-resisting and nondiscoloration.
Description
Technical field
The invention belongs to aluminum alloy surface process technology, and in particular to a kind of preparation technology of golden oxidized aluminum alloy layer.
Background technology
Aluminum alloy surface color plasma electrolytic oxidation technology(Plasma Electrolytic Oxidation)Also known as
Micro-arc discharge aoxidizes(Microarc Discharge Oxidation)Or differential arc oxidation(Microarc Oxidation), it is
Combination by electrolyte with corresponding electrical parameter, TRANSIENT HIGH TEMPERATURE high pressure caused by arc discharge is relied on to make in aluminum alloy surface
With growing the process for treating surface of the ceramic film based on oxidized aluminum alloy thing.Utilize plasma electrolytic oxidation technology
The good oxide ceramic membrane of output wear resistance and corrosion resistance can be grown in aluminum alloy surface original position, between the ceramic membrane and alloy matrix aluminum
Adhesion is strong, film thickness range is wider and controllability is strong, and the composite bed formed has high rigidity, corrosion-resistant, wear-resistant, anti-thermal shock
Deng excellent properties.
The plasma electrolytic oxidation technology of aluminium alloy has obtained expanded application in many fields, such as the change that the trade mark is 6063
Shape aluminium alloy is just widely used in the industries such as building decoration, instrument and meter, light industry.In order to obtain appearance attractive in appearance, eliminate or
Reflective, lifting wear resistance and corrosion resistance is reduced, needs 6063 wrought aluminium alloys to be prepared into black, indigo plant in many application processes
The oxidation film layer of the different tones such as color, yellow, although common anodizing technology can realize film forming and coloring, it
Chromatograph is thin, cause in especially 6063 al alloy components containing impurity elements such as silicon, magnesium the dyed layer quality of anode oxide film compared with
Low, dye layer is thin and easily comes off, and easily fades and change colour under ultraviolet irradiation, compared with plasma electrolytic oxidation
Film gap is very remote.
Following key technology main points be present in the preparation of 6063 aluminium alloy plasma electrolytic oxidation films:1st, pre-treatment works,
Degreasing, cleaning step in pre-treatment work are related to the surface state of follow-up electrolytic process;2nd, plasma electrolysis is being carried out
Before oxidizing process, a kind of technique of activation need to be provided, it is in state of activation film forming easy to process to enable aluminum alloy to surface;3rd, it is different
Electrolyte and electrolytic condition have different coloring effects to the ceramic film produced, and the color that ceramic film shows is
By the metal oxide ions formed in oxide-film and the color reaction of its complex compound, it need to strictly control electrolytic cell tank liquor and add
The composition concentration of agent and corresponding magnitude of voltage is added to obtain the colored film of setting thickness.
The coloured ceramic film formed at present in aluminum alloy surface is mostly blueness, black or deeper cool colour, in electricity
Sub- product market is well received by the public golden because color matching is difficult, has an aptitude to dark and can not obtain bright during electrolysis
Gold, so as to can not carry out it is commercially use.
The content of the invention
In order to solve the deficiencies in the prior art, the invention provides a kind of aluminium alloy oxygen that can obtain bright golden color
Change the preparation technology of layer, the technique obtains the high presentation bright golden color of hardness by strictly controlling the composition and concentration of electrolyte
Aluminum alloy ceramic layer.Meanwhile adaptability is carried out to pre-treating technology and activating process in the electrolysis process in the present invention
Configuration, makes pre-treating technology and activating process more reasonable, can promote the generation of micro-arc oxidation process, and electrolysis is produced
Ceramic layer is uniform, fine and close, wear-resisting and nondiscoloration.
The technique effect of the invention to be reached is realized by following scheme:
The preparation technology of the golden oxidized aluminum alloy layer provided in the present invention, comprises the following steps:
S01, pre-treatment:6063 aluminium alloys are subjected to degreasing, alkali cleaning, washing, neutralization, washing;
S02:Active oxidation:Aluminium alloy after S01 is handled inserts progress electrolysis, activation oxidation, the activation in active oxidation liquid
Oxidation solution is 14-15wt% aqueous solution of nitric acid, and the temperature of active oxidation is 25-30 DEG C, current density 1.0-1.2A/dm2, place
A length of 20-30s during reason, the canescence active oxidation film that thickness is 1-3 μm is prepared;
S03, re-electrolysis processing:Aluminium alloy after pre-treatment is subjected to electrolytic oxidation, the electrolyte prescription in the electrolytic solution
For potassium permanganate 5-6g/L, ammonium metavanadate 0.2-0.4 g/L, concentrated sulfuric acid 32-33 g/L, sodium metasilicate 6-8g/L, tartaric acid 16-
18g/L, EDTA0.2-0.3 g/L, leaf-alcohol 0.02-0.03 g/L, surplus are water, voltage 260-265V, a length of during oxidation processes
30-35min, the golden oxide-film that thickness is 120-122 μm is prepared;
S04, removal of impurities:The oxide-film being prepared is soaked in removal of impurities liquid and carries out removal of impurities processing, the composition of the removal of impurities liquid is
Triethanolamine 20-30mL/L, malic acid 18-20g/L, sodium persulfide 0.01-0.02 g/L, surplus are water, and removal of impurities liquid temperature degree is
40-45 DEG C, a length of 8-10s during immersion, aluminum alloy surface noresidue is washed to after immersion.
Further, in S01, defatting step is:Pending aluminium alloy is placed in the degreaser circulated, it is described de-
Fat liquid component and constituent content are sodium carbonate 15-18wt%, sodium phosphate 5-6wt%, surfactant 3-5wt%, anhydrosorbitol
Fatty acid ester 3-5wt%, sapindoside 0.5-0.7wt%, surplus are water, and degreaser temperature is 35-40 DEG C in processing procedure, is taken off
A length of 3-5 minutes during fat;The surfactant is the acyl glucose acid amides and alkyl glucose ester that HLB value is 7-8, both
Mass ratio is 1:1.2.
The purpose of degreasing is that the grease complete liquidation of aluminum alloy surface is clean, in actual production, it is contemplated that production effect
Rate and the hidden danger that anticaustic can not be remained to aluminum alloy surface, are cleaned using surfactant method in the present invention, are led to
The surfactant for adding suitable HLB value and high efficiency infiltration foaming agent sorbitan fatty ester and sapindoside are crossed,
The alloy product in defatting step is rapidly removed the grease on surface, especially have for the heavier alloy product of greasy dirt
Effect.
The golden oxide-film surface that re-electrolysis process is prepared often is covered and has a little variegated loose colour residual, needs to utilize
The removal of impurities liquid for having elimination effect to loose colour but not having corrosion function to oxide-film surface is handled, and three second are utilized in the present invention
Hydramine and malic acid, which eliminate, causes variegated ion, and sodium persulfide will corrode the precipitation by metallic ion separated out, and collective effect eliminates
It is variegated.
Further, in S01, alkali wash water that caustic scrubbing step uses is 48-52wt% sodium hydroxides, 4-5wt% sodium alginates,
Surplus is water, and 55-60 DEG C of alkali cleaning temperature, the alkali cleaning time is 4-5min.
Further, in S01, water-washing step is to be sprayed aluminum alloy surface to noresidue using water purification.
Further, in S01, the neutralizer used in neutralization procedure is 8-12wt% aqueous solution of nitric acid.
Alkali cleaning directly is carried out using high-concentration alkali liquor in the present invention, is neutralized using low concentration acid, in alkali washing process
Sodium alginate is added as corrosion-inhibiting material, while controls alkali cleaning temperature and time, reduces the corrosion for building industry team alloy matrix aluminum.
Further, in S03, the compound method of the electrolyte is:Sodium metasilicate is poured into pure water, the bar being stirred continuously
Under part, tartaric acid, cysteine vanadyl, EDTA are sequentially added, after stirring, ammonium metavanadate is eventually adding, stirs.
Further, in S03, to adjust the viscosity and permeance property of electrolyte, 0.2-0.3g/ is added in the electrolyte
L Arabic gum.
Further, it is described in S03 to obtain more darker red in order to adjust oxidation film layer color
0.002-0.004g/L sodium metavanadate is added in electrolyte.
Further, in S03,0.01-0.02g/L sodium persulfide is added in the electrolyte, for precipitating electrolyte
Middle excessive foreign ion.
Further, in S03, the electrolyte is in acidity.Electrolyte can must normally make in acid condition
With.
The present invention has advantages below:
The invention provides a kind of preparation technology for the oxidized aluminum alloy layer that can obtain bright golden color, the technique is by strictly controlling
The composition and concentration of electrolyte processed, obtain the aluminum alloy ceramic layer of the high presentation bright golden color of hardness.Meanwhile the electricity in the present invention
The configuration of adaptability has been carried out to pre-treating technology and activating process in solution technique, has made pre-treating technology and activating process more adduction
Reason, can promote the generation of micro-arc oxidation process, and make it that ceramic layer caused by electrolysis is uniform, fine and close, wear-resisting and nondiscoloration.
Embodiment
With reference to embodiment, the present invention will be described in detail.
The aluminium alloy plate that 15 × 15cm is made in 6063 aluminium alloy punching presses, thickness is 0.8cm is carried out as embodiment sample
The preparation of oxide layer.
Embodiment 1
Specific preparation process is as follows:
S01, pre-treatment:
Sample is placed in the degreaser circulated, the degreaser component and constituent content are sodium carbonate 18wt%, sodium phosphate
6.0wt%, surfactant 4.4wt%, sorbitan fatty ester 4.5wt%, sapindoside 0.7wt%, surplus is water,
Degreaser temperature is 40 DEG C in processing procedure, a length of 4 minutes during degreasing.Surfactant is the acyl glucose acyl that HLB value is 8
Amine and alkyl glucose ester, both mass ratioes are 1:1.2.
It is above-mentioned be disposed after sample inserted into gap also middle carry out alkali cleaning, the alkali wash water that caustic scrubbing step uses is 48wt%
Sodium hydroxide, 5wt% sodium alginates, surplus are water, and alkali cleaning temperature 60 C, the alkali cleaning time is 5min.Sprayed after alkali cleaning using water purification
Aluminum alloy surface is rinsed to noresidue.
It is above-mentioned be disposed after sample inserted in neutralizer neutralized, the neutralizer used in neutralization procedure is 8wt%
Aqueous solution of nitric acid, processing time 15-20s, aluminum alloy surface is sprayed to noresidue with water purification after neutralization.
S02, active oxidation:Aluminium alloy after S01 is handled inserts progress electrolysis, activation oxidation in active oxidation liquid(It is stainless
Steel negative electrode), active oxidation liquid is 14.5wt% aqueous solution of nitric acid, and the temperature of active oxidation is 30 DEG C, current density 1.2A/
dm2, handling duration 20s, the canescence active oxidation film that average thickness is 3 μm is prepared.
S03, re-electrolysis processing(Normal temperature):Aluminium alloy after pre-treatment is subjected to electrolytic oxidation in the electrolytic solution, is electrolysed
Formula of liquid is potassium permanganate 5.8g/L, the g/L of ammonium metavanadate 0.24, the g/L of the concentrated sulfuric acid 32, sodium metasilicate 6g/L, tartaric acid 17.5g/
L, EDTA0.25 g/L, the g/L of leaf-alcohol 0.025, surplus are water, voltage 260V, a length of 32min during oxidation processes, thickness are prepared
Spend the golden oxide-film for 120.5 μm.
The compound method of above-mentioned electrolyte is:Sodium metasilicate is poured into pure water, under conditions of being stirred continuously, is sequentially added dense
Sulfuric acid, tartaric acid, EDTA, leaf-alcohol, after stirring, potassium permanganate and ammonium metavanadate are eventually adding, is stirred.
S04, removal of impurities:The oxide-film being prepared is soaked in removal of impurities liquid and carries out removal of impurities processing, the group of the removal of impurities liquid
It is water as triethanolamine 25mL/L, malic acid 18g/L, the g/L of sodium persulfide 0.012, surplus, removal of impurities liquid temperature degree is 42 DEG C, leaching
A length of 8s during bubble, is washed to aluminum alloy surface noresidue after immersion.
Embodiment 2
Other conditions are same as Example 1 in the present embodiment, and 0.3g/L Arabic gum is with the addition of in S03 electrolyte, is made
The course of reaction of re-electrolysis is more steady.
The golden oxide-film that average thickness is 122 μm is finally prepared.
Embodiment 3
Other conditions are same as Example 1 in the present embodiment, and 0.002g/L sodium metavanadate is with the addition of in S03 electrolyte,
The golden red oxide-film that average thickness is 120 μm is finally prepared.
Embodiment 4
Other conditions are same as Example 1 in the present embodiment, 0.02g/L sodium persulfide with the addition of in S03 electrolyte, most
The golden oxide-film that average thickness is 120 μm is prepared afterwards.Circulation in S03 in the cycle ratio embodiment 1 of electrolyte
Number is lifted 2-3 times.
The hardness on the aluminum alloy specimen surface obtained in embodiment 1-4 is respectively:1392HV(HV10)、1401HV
(HV10)、1365HV(HV10)、1344HV(HV10).Hardness is very high.
As seen from the above-described embodiment, the oxidized aluminum alloy layer preparation technology in the present invention is by strictly controlling the group of electrolyte
Into and concentration, obtain hardness it is high presentation bright golden color aluminum alloy ceramic layer.Meanwhile to preceding in the electrolysis process in the present invention
Handling process and activating process have carried out the configuration of adaptability, make pre-treating technology and activating process more reasonable, can promote
The generation of micro-arc oxidation process, and make it that ceramic layer is uniform, fine and close, wear-resisting and nondiscoloration caused by electrolysis.
It is last it should be noted that above example is only illustrating the technical scheme of the embodiment of the present invention rather than it is entered
Row limitation, although the embodiment of the present invention is described in detail with reference to preferred embodiment, one of ordinary skill in the art
It should be understood that can still be modified to the technical scheme of the embodiment of the present invention or equivalent substitution, and these modifications or wait
The scope of amended technical scheme disengaging technical scheme of the embodiment of the present invention can not also be made with replacement.
Claims (9)
1. a kind of preparation technology of golden oxidized aluminum alloy layer, it is characterised in that comprise the following steps:
S01, pre-treatment:6063 aluminium alloys are subjected to degreasing, alkali cleaning, washing, neutralization, washing;
S02:Active oxidation:Aluminium alloy after S01 is handled inserts progress electrolysis, activation oxidation, the activation in active oxidation liquid
Oxidation solution is 14-15wt% aqueous solution of nitric acid, and the temperature of active oxidation is 25-30 DEG C, current density 1.0-1.2A/dm2, place
A length of 20-30s during reason, the canescence active oxidation film that thickness is 1-3 μm is prepared;
S03, re-electrolysis processing:Aluminium alloy after pre-treatment is subjected to electrolytic oxidation, the electrolyte prescription in the electrolytic solution
For potassium permanganate 5-6g/L, ammonium metavanadate 0.2-0.4 g/L, concentrated sulfuric acid 32-33 g/L, sodium metasilicate 6-8g/L, tartaric acid 16-
18g/L, EDTA0.2-0.3 g/L, leaf-alcohol 0.02-0.03 g/L, surplus are water, voltage 260-265V, a length of during oxidation processes
30-35min, the golden oxide-film that thickness is 120-122 μm is prepared.
2. the preparation technology of golden oxidized aluminum alloy layer as claimed in claim 1, it is characterised in that:In S01, defatting step is:
Pending aluminium alloy is placed in the degreaser circulated, the degreaser component and constituent content are sodium carbonate 15-
18wt%, sodium phosphate 5-6wt%, surfactant 3-5wt%, sorbitan fatty ester 3-5wt%, sapindoside 0.5-
0.7wt%, surplus are water, and degreaser temperature is 35-40 DEG C in processing procedure, a length of 3-5 minutes during degreasing;The surface-active
Agent is the acyl glucose acid amides and alkyl glucose ester that HLB value is 7-8, and both mass ratioes are 1:1.2.
3. the preparation technology of golden oxidized aluminum alloy layer as claimed in claim 1, it is characterised in that:In S01, caustic scrubbing step uses
Alkali wash water be 48-52wt% sodium hydroxides, 4-5wt% sodium alginates, surplus be water, 55-60 DEG C of alkali cleaning temperature, the alkali cleaning time is
4-5min。
4. the preparation technology of golden oxidized aluminum alloy layer as claimed in claim 1, it is characterised in that:In S01, water-washing step is profit
Aluminum alloy surface is sprayed to noresidue with water purification.
5. the preparation technology of golden oxidized aluminum alloy layer as claimed in claim 1, it is characterised in that:In S01, make in neutralization procedure
Neutralizer is 8-12wt% aqueous solution of nitric acid.
6. the preparation technology of golden oxidized aluminum alloy layer as claimed in claim 1, it is characterised in that:In S03, the electrolyte
Compound method is:Sodium metasilicate is poured into pure water, under conditions of being stirred continuously, sequentially adds the concentrated sulfuric acid, tartaric acid, EDTA, leaf
Alcohol, after stirring, potassium permanganate and ammonium metavanadate are eventually adding, is stirred.
7. the preparation technology of golden oxidized aluminum alloy layer as claimed in claim 1, it is characterised in that:In S03, in the electrolyte
Add 0.2-0.3g/L Arabic gum.
8. the preparation technology of golden oxidized aluminum alloy layer as claimed in claim 1, it is characterised in that:In S03, in the electrolyte
Add 0.002-0.004g/L sodium metavanadate.
9. the preparation technology of golden oxidized aluminum alloy layer as claimed in claim 1, it is characterised in that:In S03, in the electrolyte
Add 0.01-0.02g/L sodium persulfide.
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Citations (6)
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JPS6210298A (en) * | 1985-07-06 | 1987-01-19 | Kinki Yakuhin Kogyo Kk | Electrolytic coloring method for chromium alloy |
CN1594668A (en) * | 2004-07-15 | 2005-03-16 | 张秋声 | Imitation gold electrolytic coloring agent for aluminium and aluminium alloy products |
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 |
CN102808208A (en) * | 2012-08-29 | 2012-12-05 | 广东豪美铝业有限公司 | Method for putting gold color on aluminum material |
CN103255463A (en) * | 2012-02-17 | 2013-08-21 | 苏州铭德铝业有限公司 | Golden yellow electrolytic coloring technology |
CN105734639A (en) * | 2016-03-25 | 2016-07-06 | 北京石油化工学院 | Micro-arc oxidation electrolyte and method for preparing golden yellow ceramic layer on surface of matrix |
-
2017
- 2017-12-08 CN CN201711295229.2A patent/CN107893250A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6210298A (en) * | 1985-07-06 | 1987-01-19 | Kinki Yakuhin Kogyo Kk | Electrolytic coloring method for chromium alloy |
CN1594668A (en) * | 2004-07-15 | 2005-03-16 | 张秋声 | Imitation gold electrolytic coloring agent for aluminium and aluminium alloy products |
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 |
CN103255463A (en) * | 2012-02-17 | 2013-08-21 | 苏州铭德铝业有限公司 | Golden yellow electrolytic coloring technology |
CN102808208A (en) * | 2012-08-29 | 2012-12-05 | 广东豪美铝业有限公司 | Method for putting gold color on aluminum material |
CN105734639A (en) * | 2016-03-25 | 2016-07-06 | 北京石油化工学院 | Micro-arc oxidation electrolyte and method for preparing golden yellow ceramic layer on surface of matrix |
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