CN108149298A - A kind of pink salt aluminium alloy electrolysis coloring processes - Google Patents
A kind of pink salt aluminium alloy electrolysis coloring processes Download PDFInfo
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- CN108149298A CN108149298A CN201711270207.0A CN201711270207A CN108149298A CN 108149298 A CN108149298 A CN 108149298A CN 201711270207 A CN201711270207 A CN 201711270207A CN 108149298 A CN108149298 A CN 108149298A
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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 pink salt aluminium alloy electrolysis coloring processes, including：S01, pre-treatment：Electrolysis, activation is carried out after aluminum alloy material surface is cleaned up in activating solution；S02, once electrolytic coloring：DC electrolysis coloring is carried out in once electrolytic coloring liquid to aluminium alloy, coloration temperature is 20 25 DEG C, and the constant current density of coloring is 0.6 0.8A/dm2, a length of 1 3min during coloring, using graphite electrode；S03, re-electrolysis coloring：Ac electrolytic coloring is carried out in re-electrolysis coloring liquid to the aluminium alloy for completing S02 steps, coloration temperature is 20 25 DEG C, and the current density of coloring is 0.1 0.4A/dm2, a length of 2 4min during coloring, using graphite electrode.The present invention provides a kind of aluminium alloy electrolysis coloring processes that can be uniformly coloured, the color method utilizes the technical process of electrolytic coloring twice, make dyed layer evenly, stablize, hardness higher, and the black colorant layer of good texture is finally presented in alloy colouring layer, is suitable for the preparation process of high-end aluminum alloy appearance part.
Description
Technical field
The invention belongs to aluminum alloy surface processing technique fields, and in particular to a kind of aluminium alloy electrolytic coloring comprising pink salt
Method.
Background technology
Aluminium alloy density is low, intensity is than high.It is one of most widely used non-ferrous metal structural material in industry, has excellent
Good electric conductivity, thermal conductivity and corrosion stability.Simultaneously as aluminium alloy density is low, cheap, small toxicity, moulding process are ripe,
Compared to stainless steel and titanium alloy is played, there is boundless development space in fields such as medical instrument, food, household appliances.
Aluminium alloy anode oxide electrolytic coloring is one of most commonly used processing method of applicability in aluminum alloy surface processing.
Fine and close, thick and solid oxidation film layer is formed in aluminum alloy surface using the method for anodic oxidation, so as to significantly improve the resistance to of aluminium alloy
Corrosion promotes its hardness, wearability and decoration performance.Aluminium alloy electrocolor process is that oxidation is first generated in general electrolyte
Then film is electrolysed again in metallic salt electrolyte, make the cationic deposition of metal salt in oxidation film vacuum bottom and
Coloring, aluminium alloy electrocolor process liquid are referred to as re-electrolysis colouring.Re-electrolysis colouring is according to power supply type classification point
For direct current method and alternating current method, classify according to electrolytic colouring liquid, single salt, various metals composite salt and double staining can be divided into
Liquid method.
The essence of aluminium alloy electrolytic coloring is similar to plating, is all that the metal ion in metal salt solution is sunk by being electrolysed
The long-pending vacuum stage in anode oxide film, when being mapped on such metallic diffusing scattering occurs for light, so as to which oxidation film is presented
Color.Electrolytic coloring reaction belongs to by metal（Aluminium base）Semiconductor（Oxidation film barrier layer）The electrochemistry that electrolyte is formed is anti-
Should, it is an extremely complex electrochemical reaction process.Method of the prior art is needed after preceding processing, by aluminium alloy
After common sulphuric acid anodizing, then in the electrolytic coloring slot containing metal salt coloured oxidation film.For example, application No. is
201010190868.4 Chinese invention patent " a kind of preparation method of aluminum alloy colored composite film " in propose a kind of aluminium
The preparation method of alloy colored composite film, this method includes pre-treatment and the DC electrolysis of aluminium alloy is coloured, DC electrolysis
Coloring is using by H2SO4、CuSO4, EDTA and water composition composite electrolyte, wherein H2SO4For 1000-1200g/L, CuSO4
For 200-300g/L, EDTA 40-55g/L, surplus is water；0.5=0.6A/cm is kept at a temperature of 20-30 DEG C2 Constant current
Density is coloured, and the ratio between cathode and annode area are（1.5-2）：1.This method preparation process is simple, production operation safety, raw
It produces coloring film at low cost, obtained and not only has good corrosion resistance, but also meet cosmetic requirement.
Aluminium alloy electrolysis coloring processes in the above method actually should although having the advantages that safety, at low cost
With being susceptible in the process, coloring is uneven, easily the problem of aberration occurs with the color of setting.
Invention content
In order to solve the deficiencies in the prior art, the present invention provides it is a kind of can uniformly be coloured include tin
The aluminium alloy electrolysis coloring processes of salt, the color method make dyed layer evenly, surely using the technical process of electrolytic coloring twice
Fixed, hardness higher, and the black colorant layer of good texture is finally presented in alloy colouring layer, is suitable for high-end aluminum alloy appearance part
Preparation process.
Institute of the invention technique effect to be achieved is realized by following scheme：
The aluminium alloy electrolysis coloring processes provided in the present invention, include the following steps：
S01, pre-treatment：Electrolysis, activation is carried out after aluminum alloy material surface is cleaned up in activating solution, the activating solution
Constituent content is concentrated sulfuric acid 2-5g/L, phosphatase 24 0-55g/L, chromic acid 0.2-0.3g/L, and surplus is water；Activation temperature is 65-70
DEG C, electrolysis time 15-30s, current density is 0.1-0.15 A/dm2；
S02, once electrolytic coloring：DC electrolysis coloring, the once electrolytic are carried out in once electrolytic coloring liquid to aluminium alloy
Coloring liquid constituent content is boric acid 28-32g/L, seven water nickel sulfate 35-50 g/L, cobaltous sulfate 25-30 g/L, sulfosalicylic acid 5-
8 g/L, five cobaltammine 2-3g/L of sulfuric acid nitrite anions, surplus is water；PH value is adjusted using 0.1-0.5wt% dilute sulfuric acids and ammonium hydroxide
In the range of 4.0-4.5, coloration temperature is 20-25 DEG C, and the constant current density of coloring is 0.6-0.8A/dm2, a length of 1- during coloring
3min, using graphite electrode；
S03, re-electrolysis coloring：Alternating current electrolysis is carried out in re-electrolysis coloring liquid to the aluminium alloy for completing S02 steps
Color, the re-electrolysis coloring liquid constituent content is stannous sulfate 20-22 g/L, copper sulphate 8-8.5g/L, citric acid 12-13
G/L, concentrated sulfuric acid 5-10 g/L, sulfosalicylic acid 3-4g/L, surplus are water；PH is adjusted using 0.1-0.5wt% dilute sulfuric acids and ammonium hydroxide
For value in the range of 4.2-4.3, coloration temperature is 20-25 DEG C, and the current density of coloring is 0.1-0.4A/dm2, a length of 2- during coloring
4min, using graphite electrode.
The main component of oxidation film is aluminium oxide, and pure aluminium oxide is nonconducting insulator, but made of reality
Oxidation film and impure aluminium oxide, but close to a kind of substance of insulator, more similar to the state of semiconductor.In order to make
Electrolytic coloring process is more uniform, even if metal ion carries out electrolysis precipitation in fenestra is aoxidized, electronics must be to barrier layer table
It moves in face.Other than special coloring liquid, metal is the reason of oxidation film deposits coloring in the air using " gold colloid particle
Light reflection " illustrates.Most metallic plates have argenteous metallic luster, but if the metal are milled to fine-powder
Grain, then become black, as white in the glass plate of water white transparency is milled to fine-powder.It can be seen that the color of object because
Whether its type, state are colloidal particle and variant.
The principle of above-mentioned electrolytic coloring is understood, surface has been generated to the aluminum alloy materials of oxidation film first in the present invention
Surface clean is clean, then its surface is made to form activation point using electrolysis, activation, so that follow-up electrolytic coloring process can be rapid
Carry out.The electrolysis of short time, low current density in the present invention in mix acid liquor are activated, and on the one hand enable aluminum alloy to surface
Oxidation film more even uniform, on the other hand activates surface film oxide, due to processing time is short, to oxidation film almost without any
Substantive influence.
Using electrocolor process twice in the present invention, matched in once electrolytic coloring using nickel sulfate and the double salt of cobaltous sulfate
Fang Jinhang electrolytic colorings coordinate weak acid and five cobaltammine of sulfuric acid nitrite anions to form specific pH environment, while provide electrolysis
Ion buffer environment in coloring process, the speed of control electrolytic coloring process intermediate ion attachment, in oxidized aluminum alloy film surface
Form the colored film of one layer of inclined coppery of light cyan.Stannous sulfate and the double salt formulas of copper sulphate are utilized in re-electrolysis coloring,
Adhere to one layer of more secured, tough and tensile dyed layer on once electrolytic dyed layer, which is black layer, and is showed pale red
Brown gloss is very beautiful.
The selection of electrode material is most important in electrolytic colouring technology, and once electrolytic colours in the present invention and re-electrolysis
Using graphite electrode, other electrodes not can be used for color.
Further, during S01 electrolysis, activations, aluminum alloy materials are hung on hanger, and the hanger is in polishing fluid
Uniform rotation, velocity of rotation 10-30r/min.
Further, the electrolysis, activation process of S01 carries out under ultrasound environments, supersonic frequency 80-120KHz.
During electrolysis, activation, since as electrolyte, certain corrosiveness can be generated to aluminium using Acidic Liquid, when
When voltage rises, the minute bubbles of insulating properties are gathered on anode, quickly form one layer of closely adhesive layer.At this moment, electric current passes through exhausted
If the position of edge is electrolysed, place more than the bubble is difficult to, by the way that electrolysis, activation seldom occurs, to cause due to electric current
Oxidized aluminum alloy layer forms uneven, therefore needs to exclude bubble using the rotation of hanger or ultrasonic technique, while also can
Reaction speed is controlled, acid solution minimizes the erosion degree of aluminum alloy surface, is smoothed out electrolysis, activation process.
Further, the silver nitrate of 0.2-0.3g/L is added in the once electrolytic coloring liquid.
Further, the accelerating agent GKC of 5-10g/L is added in the once electrolytic coloring liquid.
Further, the aluminum sulfate of 5-6g/L is added in the re-electrolysis coloring liquid.
Further, the boric acid of 5-6g/L is added in the re-electrolysis coloring liquid.
Further, the silver nitrate of 0.2-0.3g/L is added in the re-electrolysis coloring liquid.
Further, it is rodlike electricity that the once electrolytic, which is coloured with the electrode shape used in re-electrolysis coloring process,
Pole.
Further, it is tubulose electricity that the once electrolytic, which is coloured with the electrode shape used in re-electrolysis coloring process,
Pole.
The present invention has the following advantages：
The present invention provides a kind of aluminium alloy electrolysis coloring processes for including pink salt that can be uniformly coloured, the coloring sides
Method using electrolytic coloring twice technical process, make dyed layer evenly, stablize, hardness higher, and alloy colouring layer is final
The black colorant layer of good texture is presented, is suitable for the preparation process of high-end aluminum alloy appearance part.
Specific embodiment
With reference to embodiment, the present invention will be described in detail.
6063 wrought aluminium alloys are struck out into 10 × 15cm mobile phone shells in the embodiment of the present invention, and utilize sulphuric acid anodizing
It is 25-30 μm of anode oxide film that thickness is made on its surface for technique, and to the aluminum alloy sample with anode oxide film into
Row electrolytic coloring.
Embodiment 1
The processing of following steps is carried out to the aluminium alloy mobile phone shell sample of above-mentioned 1000PCS：
S01, pre-treatment：
Carry out electrolysis, activation after specimen surface is cleaned up in activating solution, the constituent content of activating solution is concentrated sulfuric acid 4g/L,
Phosphoric acid 55g/L, chromic acid 0.2g/L activation temperatures are 65 DEG C, electrolysis time 20s, current density 0.1A/dm2.Electrolysis, activation
In the process, aluminum alloy specimen is hung on hanger, hanger uniform rotation in polishing fluid, velocity of rotation 20r/min.
It is rinsed 3-5 times using deionized water after activation.
S02, once electrolytic coloring：
DC electrolysis coloring is carried out in once electrolytic coloring liquid to sample, once electrolytic coloring liquid constituent content is boric acid 32g/
L, seven water nickel sulfates, 40 g/L, 30 g/L of cobaltous sulfate, sulfosalicylic acid 8g/L, five cobaltammine 2.5g/L of sulfuric acid nitrite anions.Profit
It is 4.0 to adjust pH value with 0.1wt% dilute sulfuric acids and ammonium hydroxide, and coloration temperature is 25 DEG C, and the constant current density of coloring is 0.7A/dm2,
A length of 1.5min during coloring, using rodlike graphite electrode.
Once electrolytic is rinsed after colouring using deionized water, removes surface loose colour residual.
S03, re-electrolysis coloring：
Ac electrolytic coloring, re-electrolysis coloring liquid group are carried out in re-electrolysis coloring liquid to the sample for completing S02 steps
Divide content for stannous sulfate 21g/L, copper sulphate 8.35g/L, 12.4 g/L of citric acid, 5.5 g/L of the concentrated sulfuric acid, sulfosalicylic acid
3g/L, surplus are water.PH value position 4.2 is adjusted using 0.1wt% dilute sulfuric acids and ammonium hydroxide, coloration temperature is 25 DEG C, the constant current of coloring
Density is 0.2A/dm2, a length of 3min during coloring, using rodlike graphite electrode.
In processing procedure, aluminum alloy sample surface is in canescence after pre-treatment, is presented after the completion of once electrolytic coloring
The inclined coppery of light cyan, surface slightly have unevenness, homogeneous black surface are presented, and show light reddish brown color light after the completion of re-electrolysis coloring
Pool, it is very beautiful.Yield 99.4%.
Embodiment 2
The present embodiment terms and conditions is same as Example 1, is carried out under ultrasound environments in pretreatment process, and supersonic frequency is
100KHz.Electrolysis time extends to 24s.Yield 99.3%.
Embodiment 3
The present embodiment terms and conditions is same as Example 1, and the silver nitrate of 0.25g/L is added in once electrolytic coloring liquid.Primary electricity
After solution coloring, aluminum alloy surface has fairy green gloss, and after re-electrolysis coloring, it is general that shallow gold is presented in aluminium alloy black surface
Red gloss, aesthetics are promoted.
Yield is same as Example 1.
Embodiment 4
The present embodiment terms and conditions is same as Example 1, and the accelerating agent GKC of 6g/L, primary electricity are added in once electrolytic coloring liquid
The process of solution coloring is speeded, and surface is than embodiment 1 more uniformly.
Yield 99.8%.
Embodiment 5
The present embodiment terms and conditions is same as Example 1, and the aluminum sulfate of 5.5g/L is added in re-electrolysis coloring liquid.Re-electrolysis
3-5 μm of thickness in the black film thickness ratio embodiment 1 generated after the completion is coloured, appearance is more hard thick and solid.
Yield 99.0%.
Embodiment 6
The present embodiment terms and conditions is same as Example 1, and the silver nitrate of 0.22g/L is added in re-electrolysis coloring liquid.Secondary electricity
After solution coloring, the general feux rouges pool of shallow gold is presented in aluminium alloy black surface, with more metal-like.
Yield 99.0%.
Embodiment 7
The present embodiment terms and conditions is same as Example 1, and the boric acid of 5.5g/L is added in re-electrolysis coloring liquid.Re-electrolysis
Color liquid cycle-index is promoted 2-3 times.
Yield 99.0%.
Embodiment 8
The present embodiment terms and conditions is same as Example 1, the electrode used in once electrolytic coloring and re-electrolysis coloring process
Shape is tubulose.
Yield is same as Example 1.
Embodiment 1 makes current density be evenly distributed with the electrode shape in embodiment 8, preferably edge can be avoided to imitate
It should.
It can be seen that by above-described embodiment, the technique that the aluminium alloy electrolysis coloring processes in the present invention utilize electrolytic coloring twice
Process, make dyed layer evenly, stablize, hardness higher, and the black colorant layer of good texture is finally presented in alloy colouring layer, fits
It shares in the preparation process of high-end aluminum alloy appearance part.
It is last it should be noted that above example be only to illustrate the embodiment of the present invention technical solution rather than to its into
Row limitation, although the embodiment of the present invention is described in detail with reference to preferred embodiment, those of ordinary skill in the art
It should be understood that the technical solution of the embodiment of the present invention can be still modified or replaced equivalently, and these are changed or wait
The range of modified technical solution disengaging technical solution of the embodiment of the present invention cannot also be made with replacement.
Claims (10)
1. a kind of pink salt aluminium alloy electrolysis coloring processes, it is characterised in that include the following steps：
S01, pre-treatment：Electrolysis, activation is carried out after aluminum alloy material surface is cleaned up in activating solution, the activating solution
Constituent content is concentrated sulfuric acid 2-5g/L, phosphatase 24 0-55g/L, chromic acid 0.2-0.3g/L, and surplus is water；Activation temperature is 65-70
DEG C, electrolysis time 15-30s, current density is 0.1-0.15 A/dm2；
S02, once electrolytic coloring：DC electrolysis coloring, the once electrolytic are carried out in once electrolytic coloring liquid to aluminium alloy
Coloring liquid constituent content is boric acid 28-32g/L, seven water nickel sulfate 35-50 g/L, cobaltous sulfate 25-30 g/L, sulfosalicylic acid 5-
8 g/L, five cobaltammine 2-3g/L of sulfuric acid nitrite anions, surplus is water；PH value is adjusted using 0.1-0.5wt% dilute sulfuric acids and ammonium hydroxide
In the range of 4.0-4.5, coloration temperature is 20-25 DEG C, and the constant current density of coloring is 0.6-0.8A/dm2, a length of 1- during coloring
3min, using graphite electrode；
S03, re-electrolysis coloring：Alternating current electrolysis is carried out in re-electrolysis coloring liquid to the aluminium alloy for completing S02 steps
Color, the re-electrolysis coloring liquid constituent content is stannous sulfate 20-22 g/L, copper sulphate 8-8.5g/L, citric acid 12-13
G/L, concentrated sulfuric acid 5-10 g/L, sulfosalicylic acid 3-4g/L, surplus are water；PH is adjusted using 0.1-0.5wt% dilute sulfuric acids and ammonium hydroxide
For value in the range of 4.2-4.3, coloration temperature is 20-25 DEG C, and the current density of coloring is 0.1-0.4A/dm2, a length of 2- during coloring
4min, using graphite electrode.
2. aluminium alloy electrolysis coloring processes as described in claim 1, it is characterised in that：During S01 electrolysis, activations, aluminium alloy material
Material is hung on hanger, hanger uniform rotation in polishing fluid, velocity of rotation 10-30r/min.
3. pink salt aluminium alloy electrolysis coloring processes as described in claim 1, it is characterised in that：The electrolysis, activation process of S01 is super
It is carried out under acoustic environment, supersonic frequency 80-120KHz.
4. pink salt aluminium alloy electrolysis coloring processes as described in claim 1, it is characterised in that：Add in the once electrolytic coloring liquid
Add the silver nitrate of 0.2-0.3g/L.
5. pink salt aluminium alloy electrolysis coloring processes as described in claim 1, it is characterised in that：Add in the once electrolytic coloring liquid
Add the accelerating agent GKC of 5-10g/L.
6. pink salt aluminium alloy electrolysis coloring processes as described in claim 1, it is characterised in that：Add in the re-electrolysis coloring liquid
Add the aluminum sulfate of 5-6g/L.
7. pink salt aluminium alloy electrolysis coloring processes as described in claim 1, it is characterised in that：Add in the re-electrolysis coloring liquid
Add the boric acid of 5-6g/L.
8. pink salt aluminium alloy electrolysis coloring processes as described in claim 1, it is characterised in that：Add in the re-electrolysis coloring liquid
Add the silver nitrate of 0.2-0.3g/L.
9. pink salt aluminium alloy electrolysis coloring processes as described in claim 1, it is characterised in that：Once electrolytic coloring and secondary
The electrode shape used during electrolytic coloring is stick electrode.
10. pink salt aluminium alloy electrolysis coloring processes as described in claim 1, it is characterised in that：The once electrolytic coloring and two
The electrode shape used during secondary electrolytic coloring is hollow edged electrode.
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| CN201711270207.0A CN108149298A (en) | 2017-12-05 | 2017-12-05 | A kind of pink salt aluminium alloy electrolysis coloring processes |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108505096A (en) * | 2018-04-19 | 2018-09-07 | 佛山市小沙江科技有限公司 | A kind of workpiece color method |
| CN113638025A (en) * | 2021-07-15 | 2021-11-12 | 惠州市安泰普表面处理科技有限公司 | Method suitable for coloring surface of aluminum alloy |
| CN115449878A (en) * | 2022-08-24 | 2022-12-09 | 四会市建鑫装饰材料有限公司 | Black coloring process for aluminum profile |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108505096A (en) * | 2018-04-19 | 2018-09-07 | 佛山市小沙江科技有限公司 | A kind of workpiece color method |
| CN113638025A (en) * | 2021-07-15 | 2021-11-12 | 惠州市安泰普表面处理科技有限公司 | Method suitable for coloring surface of aluminum alloy |
| CN115449878A (en) * | 2022-08-24 | 2022-12-09 | 四会市建鑫装饰材料有限公司 | Black coloring process for aluminum profile |
| CN115449878B (en) * | 2022-08-24 | 2023-08-11 | 四会市建鑫装饰材料有限公司 | Black coloring process for aluminum profile |
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