CN107190298A - A kind of method that micro-arc oxidation of aluminum alloy surface black film layer - Google Patents
A kind of method that micro-arc oxidation of aluminum alloy surface black film layer Download PDFInfo
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- CN107190298A CN107190298A CN201710370367.6A CN201710370367A CN107190298A CN 107190298 A CN107190298 A CN 107190298A CN 201710370367 A CN201710370367 A CN 201710370367A CN 107190298 A CN107190298 A CN 107190298A
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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
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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
- C25D11/14—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 method that micro-arc oxidation of aluminum alloy surface black film layer, by surface treatment, electrolyte and the coloring of differential arc oxidation ionic reaction are prepared in Al alloy parts surface formation black ceramic oxide film layer；This method technique is easy, and film forming speed is fast, and bath composition is easy to get, and ionic adsorption is delivered into differential arc oxidation reactive tank cathode and anode using ionic adsorption chance, to supplement ionic availability, setting level is reached so that the film layer reaction time is reduced, and reduces energy consumption；Obtained ceramic film meets market to ceramic film color diversification requirement well, solve many applications limitation that Micro-Arc Oxidized Ceramic Coating needs secondary coloring to obtain skin color, good technical background is provided for the expanded application of aluminium alloy, and the electrolyte of black ceramic film layer, containing numerous to environment, human body poisonous metal, liquid waste processing is simple and convenient.
Description
Technical field
The invention belongs to the metal coloring in process for treating surface and colour developing field, specifically a kind of aluminum alloy surface differential of the arc
The method for aoxidizing black film layer.
Background technology
In recent years in order to meet the requirement to materials'use and outward appearance, so as to investigated integral colouring method, anodic oxidation
Electrolytic coloring and chemical dyeing method after processing, although integral colouring method can obtain the strong oxide-film of good corrosion resistance, durability
Layer, the power consumption of the technology is big, coloring effect is poor, although and film layer that chemical dyeing method staining technique is simply obtained have it is good
Corrosion resistance, but the durability of its color is poor, is only applicable to the finishing of interior.And closed by differential arc oxidation dye technology in aluminium
Gold surface colorful ceramic film layer is better than in terms of wearability, corrosion resistance, presentation quality, thickness, film layer color stability
Process above, receives and is widely applied.
In terms of aluminum alloy differential arc oxidation coloring, seldom, recent year has fractional unit to do to external pertinent literature
A series of research, has obtained a series of aluminium alloy black ceramic film layers with premium properties, has obtained in the industrial production
Extensive use.But still suffer from problems with film layer preparation at present：(1) Zhang Wenfan is by adding the potassium ferricyanide (K3[Fe
(CN)6]), six cyanogen close the sour potassium (K of iron (II)4[Fe(CN)6]·3H2O) coloured in micro-arc oxidation of aluminum alloy surface, but its electrolyte
In contain many heavy metals, harmful to human, pollute environment.(2) patent No. CN 201310439874.2 discloses a kind of to magnesium conjunction
The technique of gold surface black ceramicization processing, but its pretreatment not only needs alkaline etching drying etc., post processing also needs to cleaning envelope
The techniques such as hole, processing is complicated, increases cost and film layer fugitive color.(3) patent No. CN 201010267526.8 discloses one kind
The differential arc oxidation dark-colored ceramic membranes layer preparation method of magnesium alloy chemical conversion one, system is combined together by chemical conversion and differential arc oxidation
It is standby go out dark-colored ceramic membranes layer, but it is needed after two-step film forming, first chemical membrane in long, the complex procedures that carry out differential arc oxidation film formation time
And film forming speed is slow.
The content of the invention
It is an object of the invention to overcome existing technological deficiency there is provided a kind of micro-arc oxidation of aluminum alloy surface black film
Layer method, be using silicate and phosphate as the electrolyte of main salt in, aluminium alloy is entered using the AC bi-polar pulse power
The processing of row differential arc oxidation；This method technological operation is simple, specific energy consumption is low, environmental pollution is small, prepared ceramic film compared with
Thick, uniform color and color durability is good.
Realizing the technical scheme of the object of the invention is：
A kind of method that micro-arc oxidation of aluminum alloy surface black film layer, specifically includes following steps：
1) pre-process：Al alloy parts are pre-processed, the oxide and greasy dirt of aluminum alloy surface is removed；
2) electrolyte is prepared：It is according to weight：Sodium metasilicate：Sodium phosphate：Ammonium metavanadate：Sodium tungstate：Detergent alkylate sulphur
Sour sodium：Sodium acid carbonate=2.2 ~ 6.2：4.2~6.2 ：1.8~3.4 ：4.2~6.2 ：1~2.2 ：1 ~ 1.8, silicic acid is weighed respectively
Sodium, sodium phosphate, ammonium metavanadate, sodium tungstate, neopelex, sodium acid carbonate, add in deionized water, are stirred continuously,
Each composition is fully dissolved, micro-arc oxidation electrolyte is made；
3) differential arc oxidation ionic reaction is coloured：By step 1) pretreated Al alloy parts are fixed on step 2）Prepare
Micro-arc oxidation electrolyte reactive tank in, using Al alloy parts as anode, stainless steel plate is negative electrode, using AC bi-polar arteries and veins
Rush power supply and differential arc oxidation reaction is carried out to Al alloy parts, 15-35 μm of black ceramic oxide film is formed on Al alloy parts surface
Layer；
4）Clean, dry：After the completion of the coloring of differential arc oxidation ionic reaction, Al alloy parts are taken out, it is natural with deionized water rinsing
Dry, you can obtain aluminum alloy micro-arc oxidation black layer；
By above-mentioned steps, black ceramic oxide film layer is formed on Al alloy parts surface.
Step 1）In, described pretreatment is to Al alloy parts seamed edge deburring, respectively with 240#、320#、400#Metallographic
Sand paper roughly grinds fine grinding Al alloy parts matrix, removes Al alloy parts surface film oxide then completely, then using 1500#Sand paper enters
Row polishing, in the ultrasonic washing instrument equipped with acetone, shakes cleaning aluminum alloy workpiece, goes to degrease, then use deionization
Water cleaning aluminum alloy workpiece, the Al alloy parts after cleaning are put into dryer and dried, standby.
Step 2）In, the concentration of described sodium metasilicate is 5.5 ~ 15.5g/L, and the concentration of sodium phosphate is 10.5 ~ 15 .5g/L,
The concentration of ammonium metavanadate is 4.5 ~ 8.5 g/L, and the concentration of sodium tungstate is 10.5 ~ 15.5 g/L, neopelex it is dense
Spend for 2.5 ~ 5 .5g/L, the concentration of sodium acid carbonate is 2.5 ~ 4.5 g/L.
Step 3）In, described differential arc oxidation reaction whole process uses current constant control, micro-arc oxidation electrolyte reactive tank
In, also external ionic adsorption machine is furnished with step 2 in ionic adsorption machine）Configuration electrolyte, using ionic adsorption machine by ion
Differential arc oxidation reactive tank cathode and anode is delivered in absorption, to supplement ionic availability, while ON cycle cooling will pass through step 1) it is pre-
Al alloy parts after processing are put into progress differential arc oxidation processing in the electrolyte.
Step 3）In, described technological parameter is：4.5 ~ 8.5A/dm of current density2, 30 ~ 450Hz of frequency, dutycycle
10.5% ~ 30.5%, positive negative pulse stuffing ratio (2.5 ~ 4.5)：1.
The aluminium alloy that there is differential arc oxidation black film layer on obtained surface is tested：
A, appearance color test：By the surface color of tested sample and GSB05-1426--2001 (instead of GSBG51001-
94) paint film color standard sample card is analyzed, to determine the specific color of differential arc oxidation film layer；It is digital using TT260
Cladding thickness measurer detects the thickness of film layer；
B, color durability test：Using the experiment that drenches with rain, film forming sample is placed on the homemade imitative device 48h that drenches with rain, simulation four
Season rain when temperature, air humidity situations such as, spring, summer, autumn, the four seasons in winter, per season simulated time be 12h, film is observed with this
Layer surface whether have color change or whether existing defects.
C, ceramic layer presentation quality checked using ocular examination, appropriate viewing distance is selected, for ornamental micro-
Arc oxide-film, its viewing distance is generally 0.5m, by natural scattered light or in the sunlight under range estimation test condition with perpendicular to
Test surfaces are observed with 45 ° of oblique angles.
Test result is：The thicknesses of layers that differential arc oxidation the aluminium alloy of black film layer is uniform, black film layer not damaged, nothing
The defect such as bubble-free, pin hole, spot, decortication and colour fading on change, film layer face.
Beneficial effect：
The invention provides a kind of method that micro-arc oxidation of aluminum alloy surface black film layer, film forming speed is fast, in matrix material
Aspect is applied widely, beneficial to batch production and industrial applications are realized, by the way that the aluminium alloy after cleaning is put into dryer,
Because temperature rise can make alloy interior molecules occur electron transition, energy is inspired, increases surface-active, so that the film layer starting the arc
Time is reduced, and reduces energy consumption.Ion utilization rate is set using homemade ionic adsorption machine, to exclude the extraneous ring such as temperature, humidity
Influence of the border to film layer so that the film layer reaction time is reduced, reduces energy consumption, is found, adopted by making rain device analog detection by oneself
The surface ceramic film layer prepared with the present invention has good color durability, meets actual operation requirements and meets actual use want
Ask, and black ceramic film layer electrolyte containing numerous to environment, human body poisonous metal, liquid waste processing is simple and convenient.
Embodiment
With reference to embodiment, the invention will be further elaborated, but is not limitation of the invention.
A kind of method that micro-arc oxidation of aluminum alloy surface black film layer, specifically includes following steps：
1) pre-process：Al alloy parts are pre-processed, the oxide and greasy dirt of aluminum alloy surface is removed；
2) electrolyte is prepared：It is according to weight：Sodium metasilicate：Sodium phosphate：Ammonium metavanadate：Sodium tungstate：Detergent alkylate sulphur
Sour sodium：Sodium acid carbonate=2.2 ~ 6.2：4.2~6.2 ：1.8~3.4 ：4.2~6.2 ：1~2.2 ：1 ~ 1.8, silicic acid is weighed respectively
Sodium, sodium phosphate, ammonium metavanadate, sodium tungstate, neopelex, sodium acid carbonate, add in deionized water, are stirred continuously,
Each composition is fully dissolved, micro-arc oxidation electrolyte is made；
3) differential arc oxidation ionic reaction is coloured：By step 1) pretreated Al alloy parts are fixed on step 2）Prepare
Micro-arc oxidation electrolyte reactive tank in, using Al alloy parts as anode, stainless steel plate is negative electrode, using AC bi-polar arteries and veins
Rush power supply and differential arc oxidation reaction is carried out to Al alloy parts, 15-35 μm of black ceramic oxide film is formed on Al alloy parts surface
Layer；
4）Clean, dry：After the completion of the coloring of differential arc oxidation ionic reaction, Al alloy parts are taken out, it is natural with deionized water rinsing
Dry, you can obtain aluminum alloy micro-arc oxidation black layer；
By above-mentioned steps, black ceramic oxide film layer is formed on Al alloy parts surface.
Step 1）In, described pretreatment is to Al alloy parts seamed edge deburring, respectively with 240#、320#、400#Metallographic
Sand paper roughly grinds fine grinding Al alloy parts matrix, removes Al alloy parts surface film oxide then completely, then using 1500#Sand paper enters
Row polishing, in the ultrasonic washing instrument equipped with acetone, shakes cleaning aluminum alloy workpiece, goes to degrease, then use deionization
Water cleaning aluminum alloy workpiece, the Al alloy parts after cleaning are put into dryer and dried, standby.
Step 2）In, the concentration of described sodium metasilicate is 5.5 ~ 15.5g/L, and the concentration of sodium phosphate is 10.5 ~ 15 .5g/L,
The concentration of ammonium metavanadate is 4.5 ~ 8.5 g/L, and the concentration of sodium tungstate is 10.5 ~ 15.5 g/L, neopelex it is dense
Spend for 2.5 ~ 5 .5g/L, the concentration of sodium acid carbonate is 2.5 ~ 4.5 g/L.
Step 3）In, differential arc oxidation reaction whole process is used in current constant control, micro-arc oxidation electrolyte reactive tank, also outer
Ionic adsorption machine is connect, is furnished with step 2 in ionic adsorption machine）Configuration electrolyte, ionic adsorption is sent using ionic adsorption machine
To differential arc oxidation reactive tank cathode and anode, to supplement ionic availability, while ON cycle cooling will be by step 1) pre-process after
Al alloy parts be put into the electrolyte progress differential arc oxidation processing.
Step 3）In, described technological parameter is：4.5 ~ 8.5A/dm of current density2, 30 ~ 450Hz of frequency, dutycycle
10.5% ~ 30.5%, positive negative pulse stuffing ratio (2.5 ~ 4.5)：1.
Embodiment 1：
1）From the aluminium alloy of model 1050（Size Control is 30cm × 20cm × 2cm）Successively with 240#、320#、400#Metallographic
Sand paper roughly grinds fine grinding alloy matrix aluminum, surface film oxide is removed completely, then using 1500#Sand paper is processed by shot blasting, will be beaten
Matrix after mill carries out surface degreasing processing, is cleaned with deionized water, the aluminium alloy after cleaning is put into dryer；To aluminium alloy
The purpose for carrying out pre-treatment is the oxide and greasy dirt for removing aluminum alloy surface.
2）Configure electrolyte：Contained with differential arc oxidation reactive tank and take 3L deionized waters, the silicon that 20g concentration is 8g/L is weighed respectively
Sour sodium, 32g concentration are 12 g/ L sodium phosphate, the wolframic acid that 14g concentration is 5 g/L ammonium metavanadate, 32g concentration is 12 g/L
The sodium acid carbonate that neopelex that sodium, 8g concentration are 3g/L, 8g concentration are 3g/L, is sequentially added into deionized water
In, and being stirred continuously during addition makes it fully dissolve.
3）Differential arc oxidation ionic reaction is coloured：By step 1）Matrix after processing is fixed in differential arc oxidation reactive tank, micro-
The external ionic adsorption machine of arc oxidation reaction groove, is furnished with step 2 in ionic adsorption machine）Configuration electrolyte, and ensure surface at
Alloy matrix aluminum after reason wants the part of growth in situ ceramic film to be totally immersed in electrolyte, using aluminium alloy as anode,
Stainless steel substrates are as negative electrode, and the distance between negative electrode and anode are 6cm, magnesium alloy carried out using the ac polar pulse power micro-
Arc oxidation processes, whole process uses current constant control, sets electrical parameter as current density 4A/dm2, frequency 300HZ, dutycycle
10%, positive negative pulse stuffing compares 4：1, all participation reactive ions reach used when setting ionic adsorption machine intermediate ion utilization rate as 100%
Oxidization time is 20min.
4）Clean, dry：After the completion of the coloring of differential arc oxidation ionic reaction, Al alloy parts are taken out, with deionized water rinsing,
Naturally dry, you can obtain aluminum alloy micro-arc oxidation black layer；Its smooth in appearance is uniform after tested, average thicknesses of layers
25 μm or so.
5）Measure the persistence of film layer appearance color：The experiment that drenches with rain is that film forming sample is placed on into homemade imitative device of drenching with rain
In 48h, according to this area weather forecast, it is 15 DEG C in spring that the temperature on average when simulation four seasons rain, which is, summer is 20 DEG C, autumn
Be 9 DEG C for 10 DEG C, winter, the average relative air humidity when four seasons rain be spring be 70%, summer be 65% in 85%, autumn,
Winter is 60%, the mean precipitation total amount when four seasons rain be spring be 150 mm, summer be 300mm, autumn be 100mm, winter
It is 12h per season test period for 60mm, film surface is observed after experiment and changes or exist bubble, pin hole without color fading
Etc. defect.
Embodiment 2：
A kind of method that micro-arc oxidation of aluminum alloy surface black film layer, specifically includes following steps：
1）Pretreatment：From the aluminium alloy of model 1050（Size Control is 30cm × 20cm × 2cm）Successively with 240#、320#、
400#Abrasive paper for metallograph roughly grinds fine grinding alloy matrix aluminum, surface film oxide is removed completely, then using 1500#Sand paper is polished place
Reason, carries out surface degreasing processing by the matrix after polishing, is cleaned with deionized water, the aluminium alloy after cleaning is put into dryer；
It is the oxide and greasy dirt for removing aluminum alloy surface to the purpose that aluminium alloy carries out pre-treatment.
2）Configure electrolyte：Contained with differential arc oxidation reactive tank and take 3L deionized waters, it is 10g/L's that 30g concentration is weighed respectively
Sodium metasilicate, 40g concentration be 12 g/ L sodium phosphate, 16g concentration be 6g/L ammonium metavanadate, 40g concentration be 14g/L wolframic acid
The sodium acid carbonate that neopelex that sodium, 10g concentration are 4g/L, 10g concentration are 3g/L, is sequentially added into deionized water
In, and being stirred continuously during addition makes it fully dissolve.
3）Differential arc oxidation ionic reaction is coloured：By step 1）Matrix after processing is fixed in differential arc oxidation reactive tank, micro-
The external ionic adsorption machine of arc oxidation reaction groove, is furnished with step 2 in ionic adsorption machine）Configuration electrolyte, and ensure surface at
Alloy matrix aluminum after reason wants the part of growth in situ ceramic film to be totally immersed in electrolyte, using aluminium alloy as anode,
Stainless steel substrates are as negative electrode, and the distance between negative electrode and anode are 6cm, magnesium alloy carried out using the ac polar pulse power micro-
Arc oxidation processes, whole process uses current constant control, sets electrical parameter as current density 6A/dm2, frequency 500HZ, dutycycle
20%, positive negative pulse stuffing compares 3：1, all participation reactive ions reach used when setting ionic adsorption machine intermediate ion utilization rate as 100%
Oxidization time is 30min.
4）Clean, dry：After the completion of the coloring of differential arc oxidation ionic reaction, Al alloy parts are taken out, with deionized water rinsing,
Naturally dry, you can obtain aluminum alloy micro-arc oxidation black layer；Its smooth in appearance is uniform after tested, average thicknesses of layers
40 μm or so.
5）Measure the persistence of film layer appearance color：The experiment that drenches with rain is that film forming sample is placed on into homemade imitative device of drenching with rain
In 48h, according to this area weather forecast, it is 15 DEG C in spring that the temperature on average when simulation four seasons rain, which is, summer is 20 DEG C, autumn
Be 9 DEG C for 10 DEG C, winter, the average relative air humidity when four seasons rain be spring be 70%, summer be 65% in 85%, autumn,
Winter is 60%, the mean precipitation total amount when four seasons rain be spring be 150 mm, summer be 300mm, autumn be 100mm, winter
It is 12h per season test period for 60mm, film surface is observed after experiment and changes or exist bubble, pin hole without color fading
Etc. defect.
Embodiment 3：
1）Pretreatment：From the aluminium alloy of model 6061 (size Control is 30cm × 20cm × 3cm), successively with 240#、
320#、400#Abrasive paper for metallograph roughly grinds fine grinding alloy matrix aluminum, surface film oxide is removed completely, then using 1500#Sand paper is thrown
Light processing, carries out surface degreasing processing by the matrix after polishing, is cleaned with deionized water, the aluminium alloy after cleaning is put into dryer
In；It is the oxide and greasy dirt for removing aluminum alloy surface to the purpose that aluminium alloy carries out pre-treatment.
2）Configure electrolyte：Contained with differential arc oxidation reactive tank and take 3L deionized waters, it is 15g/L's that 40g concentration is weighed respectively
Sodium metasilicate, 45g concentration be 15 g/ L sodium phosphate, 20g concentration be 8g/L ammonium metavanadate, 45g concentration be 14g/L wolframic acid
The sodium acid carbonate that neopelex that sodium, 15g concentration are 5g/L, 10g concentration are 4g/L, is sequentially added into deionized water
In, and being stirred continuously during addition makes it fully dissolve.
3）Differential arc oxidation ionic reaction is coloured：By step 1）Matrix after middle processing is fixed in differential arc oxidation reactive tank,
The external ionic adsorption machine of differential arc oxidation reactive tank, configures (2) electrolyte, and ensure after surface treatment in ionic adsorption machine
Alloy matrix aluminum wants the part of growth in situ ceramic film to be totally immersed in electrolyte, regard aluminium alloy as anode, stainless steel
Piece is as negative electrode, and the distance between negative electrode and anode are 6cm, and differential arc oxidation is carried out to magnesium alloy using the ac polar pulse power
Processing, whole process uses current constant control, sets electrical parameter as current density 8A/dm2, frequency 400HZ, dutycycle 30% is positive and negative
Pulse ratio 2：1, all participation reactive ions reach oxidization time used when setting ionic adsorption machine intermediate ion utilization rate as 100%
For 40min.
4）Clean, dry：After the completion of the coloring of differential arc oxidation ionic reaction, Al alloy parts are taken out, with deionized water rinsing,
Naturally dry, you can obtain aluminum alloy micro-arc oxidation black layer；Its smooth in appearance is uniform after tested, average thicknesses of layers
40 μm or so.
5）Measure the persistence of film layer appearance color：The experiment that drenches with rain is that film forming sample is placed on into homemade imitative device of drenching with rain
In 48h, according to this area weather forecast, it is 15 DEG C in spring that the temperature on average when simulation four seasons rain, which is, summer is 20 DEG C, autumn
Be 9 DEG C for 10 DEG C, winter, the average relative air humidity when four seasons rain be spring be 70%, summer be 65% in 85%, autumn,
Winter is 60%, the mean precipitation total amount when four seasons rain be spring be 150 mm, summer be 300mm, autumn be 100mm, winter
It is 12h per season test period for 60mm, film surface is observed after experiment and changes or exist bubble, pin hole without color fading
Etc. defect.
Embodiment 4：
1）Pretreatment：From model LY12 aluminium alloys (size Control is 30cm × 20cm × 3cm), successively with 240#、
320#、400#Abrasive paper for metallograph roughly grinds fine grinding alloy matrix aluminum, surface film oxide is removed completely, then using 1500#Sand paper is thrown
Light processing, carries out surface degreasing processing by the matrix after polishing, is cleaned with deionized water, the aluminium alloy after cleaning is put into dryer
In；It is the oxide and greasy dirt for removing aluminum alloy surface to the purpose that aluminium alloy carries out pre-treatment.
2）Configure electrolyte：Contained with differential arc oxidation reactive tank and take 3L deionized waters, the silicon that 20g concentration is 8g/L is weighed respectively
Sour sodium, 32g concentration are 12 g/ L sodium phosphate, the wolframic acid that 14g concentration is 5 g/L ammonium metavanadate, 32g concentration is 12 g/L
The sodium acid carbonate that neopelex that sodium, 8g concentration are 3g/L, 8g concentration are 3g/L, is sequentially added into deionized water
In, and being stirred continuously during addition makes it fully dissolve.
3）Differential arc oxidation ionic reaction is coloured：By step 1）Matrix after processing is fixed in differential arc oxidation reactive tank, micro-
The external ionic adsorption machine of arc oxidation reaction groove, is furnished with step 2 in ionic adsorption machine）Configuration electrolyte, and ensure surface at
Alloy matrix aluminum after reason wants the part of growth in situ ceramic film to be totally immersed in electrolyte, using aluminium alloy as anode,
Stainless steel substrates are as negative electrode, and the distance between negative electrode and anode are 6cm, magnesium alloy carried out using the ac polar pulse power micro-
Arc oxidation processes, whole process uses current constant control, sets electrical parameter as current density 4A/dm2, frequency 300HZ, dutycycle
10%, positive negative pulse stuffing compares 4：1, all participation reactive ions reach used when setting ionic adsorption machine intermediate ion utilization rate as 100%
Oxidization time is 20min.
4）Clean, dry：After the completion of the coloring of differential arc oxidation ionic reaction, Al alloy parts are taken out, with deionized water rinsing,
Naturally dry, you can obtain aluminum alloy micro-arc oxidation black layer；Its smooth in appearance is uniform after tested, average thicknesses of layers
25 μm or so.
5）Measure the persistence of film layer appearance color：The experiment that drenches with rain is that film forming sample is placed on into homemade imitative device of drenching with rain
In 48h, according to this area weather forecast, it is 15 DEG C in spring that the temperature on average when simulation four seasons rain, which is, summer is 20 DEG C, autumn
Be 9 DEG C for 10 DEG C, winter, the average relative air humidity when four seasons rain be spring be 70%, summer be 65% in 85%, autumn,
Winter is 60%, the mean precipitation total amount when four seasons rain be spring be 150 mm, summer be 300mm, autumn be 100mm, winter
It is 12h per season test period for 60mm, film surface is observed after experiment and changes or exist bubble, pin hole without color fading
Etc. defect.
Embodiment 5：
1）Pretreatment：6063 aluminium alloys (size Control is 30cm × 20cm × 3cm), successively with 240#、320#、400#Metallographic sand
Paper roughly grinds fine grinding alloy matrix aluminum, surface film oxide is removed completely, then using 1500#Sand paper is processed by shot blasting, will be polished
Matrix afterwards carries out surface degreasing processing, is cleaned with deionized water, the aluminium alloy after cleaning is put into dryer；Aluminium alloy is entered
The purpose of row pre-treatment is the oxide and greasy dirt for removing aluminum alloy surface.
2）Configure electrolyte：Contained with differential arc oxidation reactive tank and take 3L deionized waters, the silicon that 20g concentration is 8g/L is weighed respectively
Sour sodium, 32g concentration are 12 g/ L sodium phosphate, the wolframic acid that 14g concentration is 5 g/L ammonium metavanadate, 32g concentration is 12 g/L
The sodium acid carbonate that neopelex that sodium, 8g concentration are 3g/L, 8g concentration are 3g/L, is sequentially added into deionized water
In, and being stirred continuously during addition makes it fully dissolve.
3）Differential arc oxidation ionic reaction is coloured：By step 1）Matrix after processing is fixed in differential arc oxidation reactive tank, micro-
The external ionic adsorption machine of arc oxidation reaction groove, is furnished with step 2 in ionic adsorption machine）Configuration electrolyte, and ensure surface at
Alloy matrix aluminum after reason wants the part of growth in situ ceramic film to be totally immersed in electrolyte, using aluminium alloy as anode,
Stainless steel substrates are as negative electrode, and the distance between negative electrode and anode are 6cm, magnesium alloy carried out using the ac polar pulse power micro-
Arc oxidation processes, whole process uses current constant control, sets electrical parameter as current density 6A/dm2, frequency 500HZ, dutycycle
20%, positive negative pulse stuffing compares 3：1, all participation reactive ions reach used when setting ionic adsorption machine intermediate ion utilization rate as 100%
Oxidization time is 30min.
4）Clean, dry：After the completion of the coloring of differential arc oxidation ionic reaction, Al alloy parts are taken out, with deionized water rinsing,
Naturally dry, you can obtain aluminum alloy micro-arc oxidation black layer；Its smooth in appearance is uniform after tested, average thicknesses of layers
40 μm or so.
5）Measure the persistence of film layer appearance color：The experiment that drenches with rain is that film forming sample is placed on into homemade imitative device of drenching with rain
In 48h, according to this area weather forecast, it is 15 DEG C in spring that the temperature on average when simulation four seasons rain, which is, summer is 20 DEG C, autumn
Be 9 DEG C for 10 DEG C, winter, the average relative air humidity when four seasons rain be spring be 70%, summer be 65% in 85%, autumn,
Winter is 60%, the mean precipitation total amount when four seasons rain be spring be 150 mm, summer be 300mm, autumn be 100mm, winter
It is 12h per season test period for 60mm, film surface is observed after experiment and changes or exist bubble, pin hole without color fading
Etc. defect.
Claims (5)
1. a kind of method that micro-arc oxidation of aluminum alloy surface black film layer, it is characterised in that specifically include following steps：
1) pre-process：Al alloy parts are pre-processed, the oxide and greasy dirt of aluminum alloy surface is removed；
2) electrolyte is prepared：It is according to weight：Sodium metasilicate：Sodium phosphate：Ammonium metavanadate：Sodium tungstate：Detergent alkylate sulphur
Sour sodium：Sodium acid carbonate=2.2 ~ 6.2：4.2~6.2 ：1.8~3.4 ：4.2~6.2 ：1~2.2 ：1 ~ 1.8, silicic acid is weighed respectively
Sodium, sodium phosphate, ammonium metavanadate, sodium tungstate, neopelex, sodium acid carbonate, add in deionized water, are stirred continuously,
Each composition is fully dissolved, micro-arc oxidation electrolyte is made；
3) differential arc oxidation ionic reaction is coloured：By step 1) pretreated Al alloy parts are fixed on step 2）Prepare
Micro-arc oxidation electrolyte reactive tank in, using Al alloy parts as anode, stainless steel plate is negative electrode, using AC bi-polar arteries and veins
Rush power supply and differential arc oxidation reaction is carried out to Al alloy parts, 15-35 μm of black ceramic oxide film is formed on Al alloy parts surface
Layer；
4）Clean, dry：After the completion of the coloring of differential arc oxidation ionic reaction, Al alloy parts are taken out, it is natural with deionized water rinsing
Dry, you can obtain aluminum alloy micro-arc oxidation black layer；
By above-mentioned steps, black ceramic oxide film layer is formed on Al alloy parts surface.
2. according to the method described in claim 1, it is characterised in that step 1）In, described pretreatment is to Al alloy parts
Seamed edge deburring, respectively with 240#、320#、400#Abrasive paper for metallograph roughly grinds fine grinding Al alloy parts matrix, and aluminium alloy work is removed completely
Part surface film oxide then, then using 1500#Sand paper is processed by shot blasting, in the ultrasonic washing instrument equipped with acetone, vibrations
Cleaning aluminum alloy workpiece, goes to degrease, then with deionized water cleaning aluminum alloy workpiece, the Al alloy parts after cleaning are put into drying
Dried in machine, it is standby.
3. according to the method described in claim 1, it is characterised in that step 2）In, the concentration of described sodium metasilicate for 5.5 ~
15.5g/L, the concentration of sodium phosphate is 10.5 ~ 15 .5g/L, and the concentration of ammonium metavanadate is 4.5 ~ 8.5 g/L, the concentration of sodium tungstate
For 10.5 ~ 15.5 g/L, the concentration of neopelex is 2.5 ~ 5 .5g/L, and the concentration of sodium acid carbonate is 2.5 ~ 4.5
g/L。
4. according to the method described in claim 1, it is characterised in that step 3）In, described differential arc oxidation reaction whole process
Using current constant control, in micro-arc oxidation electrolyte reactive tank, also external ionic adsorption machine is furnished with step 2 in ionic adsorption machine）
Configuration electrolyte, ionic adsorption is delivered into differential arc oxidation reactive tank cathode and anode using ionic adsorption machine, with supplement ion utilization
Rate, at the same ON cycle cooling will pass through step 1) pretreated Al alloy parts be put into the electrolyte carry out differential of the arc oxygen
Change is handled.
5. according to the method described in claim 1, it is characterised in that step 3）In, described technological parameter is：Current density
4.5~8.5A/dm2, 30 ~ 450Hz of frequency, dutycycle 10.5% ~ 30.5%, positive negative pulse stuffing ratio (2.5 ~ 4.5)：1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541763A (en) * | 2017-10-11 | 2018-01-05 | 四川恒诚信电子科技有限公司 | A kind of oxidation treatment method of high thermal conductivity aluminum matrix plate |
| CN108203781A (en) * | 2018-03-28 | 2018-06-26 | 安徽华中天力铝业有限公司 | A kind of 2024 aluminium alloys and its electroplating technology |
| CN109402699A (en) * | 2018-11-01 | 2019-03-01 | 中国科学院兰州化学物理研究所 | A kind of aluminum alloy surface acid resistance corrosion function ceramic membrane preparation process |
| CN114420347A (en) * | 2022-02-24 | 2022-04-29 | 远东电缆有限公司 | Cable for new energy automobile, preparation method and application |
| CN114540914A (en) * | 2022-03-11 | 2022-05-27 | 西安理工大学 | Method for preparing megaohm-level high-impedance ceramic layer on surface of aluminum alloy in situ |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101270495A (en) * | 2008-04-21 | 2008-09-24 | 华南理工大学 | Method for preparing corrosion protection abrasion resistant ceramic coating with alloy surface differential arc oxidization |
| CN101775633A (en) * | 2010-01-18 | 2010-07-14 | 哈尔滨工业大学 | Method for preparing black titanium oxide coating on titanium surface |
| CN102154673A (en) * | 2011-04-12 | 2011-08-17 | 中国船舶重工集团公司第十二研究所 | Method for preparing environment-friendly micro-arc oxidation black ceramic film on aluminum alloy surface |
| CN102230205A (en) * | 2011-06-20 | 2011-11-02 | 华南理工大学 | Aluminum alloy micro-arc oxidation black ceramic membrane and preparation method thereof |
| RU2570869C1 (en) * | 2014-09-10 | 2015-12-10 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" | Method of producing of black wear-resistant anti-corrosion coating on aluminium and aluminium based alloys by method of microarc oxydation |
| CN106637341A (en) * | 2016-12-18 | 2017-05-10 | 中国工程物理研究院材料研究所 | Preparation method for black micro arc oxidation film layers of surfaces of pure aluminum and aluminum alloys |
-
2017
- 2017-05-23 CN CN201710370367.6A patent/CN107190298A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101270495A (en) * | 2008-04-21 | 2008-09-24 | 华南理工大学 | Method for preparing corrosion protection abrasion resistant ceramic coating with alloy surface differential arc oxidization |
| CN101775633A (en) * | 2010-01-18 | 2010-07-14 | 哈尔滨工业大学 | Method for preparing black titanium oxide coating on titanium surface |
| CN102154673A (en) * | 2011-04-12 | 2011-08-17 | 中国船舶重工集团公司第十二研究所 | Method for preparing environment-friendly micro-arc oxidation black ceramic film on aluminum alloy surface |
| CN102230205A (en) * | 2011-06-20 | 2011-11-02 | 华南理工大学 | Aluminum alloy micro-arc oxidation black ceramic membrane and preparation method thereof |
| RU2570869C1 (en) * | 2014-09-10 | 2015-12-10 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" | Method of producing of black wear-resistant anti-corrosion coating on aluminium and aluminium based alloys by method of microarc oxydation |
| CN106637341A (en) * | 2016-12-18 | 2017-05-10 | 中国工程物理研究院材料研究所 | Preparation method for black micro arc oxidation film layers of surfaces of pure aluminum and aluminum alloys |
Non-Patent Citations (3)
| Title |
|---|
| 梁戈 等: ""电解液参数对铝合金微弧氧化黑色陶瓷膜性能的影响"", 《材料热处理学报》 * |
| 王瑞金: "《特种加工技术》", 28 February 2011 * |
| 石小超 等: ""铝合金微弧氧化技术研究概况"", 《兵器材料科学与工程》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541763A (en) * | 2017-10-11 | 2018-01-05 | 四川恒诚信电子科技有限公司 | A kind of oxidation treatment method of high thermal conductivity aluminum matrix plate |
| CN108203781A (en) * | 2018-03-28 | 2018-06-26 | 安徽华中天力铝业有限公司 | A kind of 2024 aluminium alloys and its electroplating technology |
| CN109402699A (en) * | 2018-11-01 | 2019-03-01 | 中国科学院兰州化学物理研究所 | A kind of aluminum alloy surface acid resistance corrosion function ceramic membrane preparation process |
| CN114420347A (en) * | 2022-02-24 | 2022-04-29 | 远东电缆有限公司 | Cable for new energy automobile, preparation method and application |
| CN114540914A (en) * | 2022-03-11 | 2022-05-27 | 西安理工大学 | Method for preparing megaohm-level high-impedance ceramic layer on surface of aluminum alloy in situ |
| CN114540914B (en) * | 2022-03-11 | 2024-03-22 | 西安理工大学 | Method for preparing megaohm-level high-impedance ceramic layer on aluminum alloy surface in situ |
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