CN112981487A - Low-energy-consumption quick black aluminum alloy micro-arc oxidation method - Google Patents
Low-energy-consumption quick black aluminum alloy micro-arc oxidation method Download PDFInfo
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- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 title claims abstract description 36
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000005265 energy consumption Methods 0.000 title claims abstract description 13
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 16
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000003792 electrolyte Substances 0.000 claims abstract description 13
- 239000003086 colorant Substances 0.000 claims abstract description 12
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims abstract description 10
- XVNRSQASUCMHGX-UHFFFAOYSA-N O[Si](O)(O)O.OP(O)(O)=O Chemical compound O[Si](O)(O)O.OP(O)(O)=O XVNRSQASUCMHGX-UHFFFAOYSA-N 0.000 claims abstract description 9
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000654 additive Substances 0.000 claims abstract description 8
- 239000011698 potassium fluoride Substances 0.000 claims abstract description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 8
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 8
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 6
- 235000003270 potassium fluoride Nutrition 0.000 claims abstract description 5
- 229960001484 edetic acid Drugs 0.000 claims abstract description 4
- 229910003206 NH4VO3 Inorganic materials 0.000 claims abstract 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical group [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 8
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 8
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- PHIQPXBZDGYJOG-UHFFFAOYSA-N sodium silicate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-][Si]([O-])=O PHIQPXBZDGYJOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910003243 Na2SiO3·9H2O Inorganic materials 0.000 claims 1
- 241001460678 Napo <wasp> Species 0.000 claims 1
- 239000004115 Sodium Silicate Substances 0.000 claims 1
- 150000004690 nonahydrates Chemical class 0.000 claims 1
- 229910052911 sodium silicate Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000035484 reaction time Effects 0.000 abstract description 5
- 239000012528 membrane Substances 0.000 abstract description 4
- 239000011224 oxide ceramic Substances 0.000 abstract description 4
- 229910052574 oxide ceramic Inorganic materials 0.000 abstract description 4
- 238000004381 surface treatment Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 238000005498 polishing Methods 0.000 description 8
- 229910001250 2024 aluminium alloy Inorganic materials 0.000 description 5
- CYPRMUMKDSHJER-UHFFFAOYSA-N O.O.O.O.O.O.O.O.O.[Na] Chemical compound O.O.O.O.O.O.O.O.O.[Na] CYPRMUMKDSHJER-UHFFFAOYSA-N 0.000 description 4
- 244000137852 Petrea volubilis Species 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 235000017550 sodium carbonate Nutrition 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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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
-
- 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
- C25D11/024—Anodisation under pulsed or modulated current or potential
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention relates to a surface treatment method, in particular to a low-energy-consumption rapid aluminum alloy black micro-arc oxidation method which is suitable for preparing a black oxide ceramic membrane on the surface of aluminum alloy rapidly and with low energy consumption. The electrolyte adopts a phosphate-silicate system, and is added with an additive and a colorant to carry out micro-arc oxidation treatment on the aluminum alloy. The colorant comprises ammonium metavanadate NH4VO3The additives comprise ethylene diamine tetraacetic acid EDTA, sodium fluoride NaF, potassium fluoride KF and sodium carbonate Na2CO3. And carrying out micro-arc oxidation treatment on the aluminum alloy. By adopting a micro-arc oxidation pulse power supply, the current is continuously adjustable at 1-500A, the voltage is continuously adjustable at 0-700V, the frequency is continuously adjustable at 50-1000Hz, and the duty ratio is continuously adjustable at 10% -30%. Compared with the traditional domestic micro-arc oxidation arc striking voltage and reaction time, the method has the advantages that the electrolyte can be recycled through scientific proportioning, the production efficiency can be improved, the energy is saved, and the green effect is realizedLow energy consumption and sustainable development.
Description
Technical Field
The invention relates to a surface treatment method, which is suitable for preparing a black oxide ceramic film on the surface of an aluminum alloy quickly with low energy consumption.
Background
The aluminum element is the metal element with the largest content in the earth crust and accounts for 7.45 percent of the total amount. The aluminum material is the second most used metal material in the world, is second only to the steel material, and is the most used non-ferrous metal material. The aluminum material has the advantages of high specific strength, good machinability, good heat conductivity and electrical conductivity, good corrosion resistance and the like, and is widely applied to the fields of automobiles, aviation, building materials, electronic products and the like. The surface of aluminum alloy is necessary to be treated because an oxide film is naturally formed on the surface of aluminum material in the atmosphere, but the performance of the oxide film cannot meet the industrial requirement.
The micro-arc oxidation technology is a novel surface treatment technology, and a layer of oxide ceramic film grows in situ on the surface of the aluminum alloy under the action of high-temperature and high-voltage electric arcs. The ceramic oxide membrane prepared by micro-arc oxidation has excellent comprehensive performance, and the corrosion resistance, the friction resistance, the hardness and the like are obviously improved. The oxide ceramic membrane prepared by micro-arc oxidation grows in situ, and the bonding force is high. Compared with anodic oxidation, the electrolyte used in micro-arc oxidation has no pollution to the environment, and the green production is really realized.
However, the prior micro-arc oxidation technology has a plurality of technical difficulties, namely, the arcing voltage is overhigh. At present, the arcing voltage of domestic micro-arc oxidation production is basically over 270V, the termination voltage is about 500V, the high voltage greatly increases the energy consumption of micro-arc oxidation, and the control of the production cost is not facilitated. Secondly, the reaction time of the prior micro-arc oxidation is too long, usually 30min-120min, which is also not beneficial to the control of the production cost.
Disclosure of Invention
The invention aims to provide a low-energy-consumption quick black micro-arc oxidation method for aluminum alloy, which reduces micro-arc oxidation voltage and reaction time, realizes low-energy-consumption quick production and reduces production cost.
The technical scheme of the invention is as follows:
a low-energy-consumption quick aluminum alloy micro-arc oxidation method adopts a micro-arc oxidation pulse power supply, adopts a phosphate-silicate system as electrolyte, and adds an additive and a coloring agent to carry out micro-arc oxidation treatment on aluminum alloy. The colorant comprises ammonium metavanadate, and the additive comprises one or a mixture of ethylenediamine tetraacetic acid, sodium fluoride, potassium fluoride and sodium carbonate. 2024 aluminum alloy sample as anode connects to positive electrode of power supply, stainless steel plate as cathode connects to negative electrode of power supply. The electrode is completely immersed in the electrolyte, the temperature is controlled at 30 ℃ by using a low-temperature constant-temperature bath, and the temperature of the electrolyte is controlled to be uniform by using magnetic stirring.
The micro-arc oxidation pulse power supply has the advantages that the current is continuously adjustable within 1-500A, the voltage is continuously adjustable within 0-700V, the frequency is continuously adjustable within 50-1000Hz, and the duty ratio is continuously adjustable within 10% -30%.
The phosphate-silicate system electrolyte is prepared from sodium hexametaphosphate, sodium silicate nonahydrate, sodium hydroxide and deionized water, and the proportion is as follows:
sodium hexametaphosphate 10-20 g.L-1
Sodium silicate nonahydrate 5-15 g.L-1
Sodium hydroxide 1-2 g.L-1
The additive is one or a mixture of ethylene diamine tetraacetic acid, sodium fluoride, potassium fluoride and sodium carbonate;
the colorant is 5-10 g.L of ammonium metavanadate-1。
The method comprises the following specific steps:
1. the sample is made of 2024 aluminum alloy plates, is cut into a rectangle with the size of 25mm multiplied by 20mm multiplied by 2mm, and is punched at the edge of the sample for connecting a lead;
2. polishing the surface of the sample by using sand paper, polishing to 1200#, putting the sample into an ultrasonic cleaning instrument, cleaning by using absolute ethyl alcohol, and drying for later use;
3. the electrolyte adopts a phosphate-silicate system, and 10-20 g.L of sodium hexametaphosphate is added-15-15 g.L of sodium nonahydrate-1Sodium hydroxide 1-2 g.L-1(ii) a 5-10 g.L of colorant ammonium metavanadate-1(ii) a Adding 2-10 g.L of additive-1;
4. And (3) using a pulse power supply for micro-arc oxidation, adopting a constant voltage mode, increasing the voltage step by step, finally increasing the voltage to 190V, oxidizing for 8min, respectively cleaning with deionized water and absolute ethyl alcohol after the reaction is finished, drying, and performing performance test.
The invention has the advantages that:
1. the voltage adopted by the invention is below 200V, and compared with the traditional domestic micro-arc oxidation arcing voltage of above 270V, the termination voltage is about 500V, so that the cost can be effectively reduced, and the energy can be saved;
2. the reaction time of the method is 7-10min, and compared with the reaction time of 30-120 min in the traditional micro-arc oxidation, the production efficiency can be effectively improved, and the energy is saved;
3. the black micro-arc oxidation ceramic membrane prepared by the invention has good binding force with a substrate and has good performance in practical application.
Drawings
FIG. 1 is a scanning electron microscope image of the micro-arc oxidation ceramic film in example 1.
Detailed Description
The present invention is described in detail below with reference to examples.
Example 1
1. The sample is made of 2024 aluminum alloy plates, is cut into a rectangle with the size of 25mm multiplied by 20mm multiplied by 2mm, and is punched at the edge of the sample for connecting a lead;
2. polishing the surface of the sample by using sand paper, polishing to 1200#, putting the sample into an ultrasonic cleaning instrument, cleaning by using absolute ethyl alcohol, and drying for later use;
3. the electrolyte adopts a phosphate-silicate system, and 10 g.L of sodium hexametaphosphate is added-1Sodium nonahydrate 5 g.L-1Sodium hydroxide 1 g.L-1(ii) a Colorant ammonium metavanadate 5 g.L-1(ii) a Sodium fluoride 5 g.L is added into the additive-1;
4. And (3) using a pulse power supply for micro-arc oxidation, adopting a constant voltage mode, gradually increasing the voltage, finally increasing the voltage to 190V, oxidizing for 10min, respectively cleaning with deionized water and absolute ethyl alcohol after the reaction is finished, and drying.
Example 2
1. The sample is made of 2024 aluminum alloy plates, is cut into a rectangle with the size of 25mm multiplied by 20mm multiplied by 2mm, and is punched at the edge of the sample for connecting a lead;
2. polishing the surface of the sample by using sand paper, polishing to 1200#, putting the sample into an ultrasonic cleaning instrument, cleaning by using absolute ethyl alcohol, and drying for later use;
3. the electrolyte adopts a phosphate-silicate system, and 15 g.L of sodium hexametaphosphate is added-110 g.L of sodium nonahydrate-1Sodium hydroxide 1.5 g.L-1(ii) a Colorant ammonium metavanadate 8 g.L-1(ii) a Adding potassium fluoride 10 g.L into the additive-1Ethylenediaminetetraacetic acid 2 g.L-1;
4. And (3) using a pulse power supply for micro-arc oxidation, adopting a constant voltage mode, increasing the voltage step by step, finally increasing the voltage to 190V, oxidizing for 5min, respectively cleaning with deionized water and absolute ethyl alcohol after the reaction is finished, and drying.
Example 3
1. The sample is made of 2024 aluminum alloy plates, is cut into a rectangle with the size of 25mm multiplied by 20mm multiplied by 2mm, and is punched at the edge of the sample for connecting a lead;
2. polishing the surface of the sample by using sand paper, polishing to 1200#, putting the sample into an ultrasonic cleaning instrument, cleaning by using absolute ethyl alcohol, and drying for later use;
3. the electrolyte adopts a phosphate-silicate system, and 20 g.L of sodium hexametaphosphate is added-18 g.L sodium nonahydrate-1Sodium hydroxide 2 g.L-1(ii) a Colorant ammonium metavanadate 6 g.L-1(ii) a Adding 10 g.L of sodium carbonate into the additive-1;
4. And (3) using a pulse power supply for micro-arc oxidation, adopting a constant voltage mode, increasing the voltage step by step, finally increasing the voltage to 190V, oxidizing for 8min, respectively cleaning with deionized water and absolute ethyl alcohol after the reaction is finished, and drying.
Claims (5)
1. A low-energy-consumption quick aluminum alloy micro-arc oxidation method is characterized in that a micro-arc oxidation pulse power supply is adopted, a phosphate-silicate system is adopted as an electrolyte, an additive and a coloring agent are added, and micro-arc oxidation treatment is carried out on the aluminum alloy; the additives are ethylene diamine tetraacetic acid EDTA, sodium fluoride NaF, potassium fluoride KF and sodium carbonate Na2CO3Colorant ammonium metavanadate NH4VO3。
2. The low-energy-consumption rapid aluminum alloy micro-arc oxidation method as claimed in claim 1, wherein the micro-arc oxidation pulse power supply has a continuously adjustable current of 1-500A, a continuously adjustable voltage of 0-700V, a continuously adjustable frequency of 50-1000Hz, and a continuously adjustable duty cycle of 10% -30%.
3. The method of claim 1, wherein the phosphate-silicate system electrolyte is sodium hexametaphosphate (NaPO)3)6Sodium metasilicate nonahydrate Na2SiO3·9H2O, NaOH and deionized water, and the mixture ratio is as follows:
sodium hexametaphosphate 10-20 g.L-1
Sodium silicate nonahydrate 5-15 g.L-1
Sodium hydroxide 1-2 g.L-1。
4. The method for micro-arc oxidation of a low energy consumption aluminum alloy according to claim 1, wherein the additive is EDTA, NaF, KF, Na2CO3One or a mixture of (1) at a concentration of 2-10 g.L-1。
5. The method of micro-arc oxidation of a low energy consuming aluminum alloy according to claim 1, wherein the colorant is ammonium metavanadate NH4VO3The mixture ratio is as follows: 5-10 g.L-1。
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Cited By (1)
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CN113981504A (en) * | 2021-06-23 | 2022-01-28 | 中南机诚精密制品(深圳)有限公司 | Micro-arc oxidation patterning process method for ceramic alloy film layer and micro-arc oxidation cargo |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
CN102877104A (en) * | 2012-10-09 | 2013-01-16 | 西南石油大学 | Low-voltage rapid micro-arc oxidation technique |
CN107964673A (en) * | 2016-10-19 | 2018-04-27 | 宁波瑞隆表面技术有限公司 | A kind of method that aluminum alloy differential arc oxidation prepares black ceramic film layer |
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Publication number | Priority date | Publication date | Assignee | Title |
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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 |
CN102877104A (en) * | 2012-10-09 | 2013-01-16 | 西南石油大学 | Low-voltage rapid micro-arc oxidation technique |
CN107964673A (en) * | 2016-10-19 | 2018-04-27 | 宁波瑞隆表面技术有限公司 | A kind of method that aluminum alloy differential arc oxidation prepares black ceramic film layer |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113981504A (en) * | 2021-06-23 | 2022-01-28 | 中南机诚精密制品(深圳)有限公司 | Micro-arc oxidation patterning process method for ceramic alloy film layer and micro-arc oxidation cargo |
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