CN102367584A - Metal microarc oxidation electrolyte and method for forming black ceramic coating on metal surface by microarc oxidation - Google Patents
Metal microarc oxidation electrolyte and method for forming black ceramic coating on metal surface by microarc oxidation Download PDFInfo
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Abstract
The invention discloses a metal microarc oxidation electrolyte and a method for forming a black ceramic coating on a metal surface by microarc oxidation, belonging to the technical field of metal surface treatment. The electrolyte comprises sodium silicate, sodium fluoride, potassium hydroxide, sodium citrate, sodium tungstate and pigment, carbon black. The method for forming the black ceramic coating on the metal surface by microarc oxidation comprises the following steps: carrying out pretreatment on a sample, preparing a electrolyte electrolyte, setting electrical parameters, turning of a circulating cooling water device, connecting the sample with a conducting rod, immersing the sample in the electrolyte to be as the anode, using a stainless steel electrolytic tank doubling as the cathode, switching on a bidirectional pulse power supply to carry out microarc oxidation treatment, then washing the treated sample with deionized water to obtain a black ceramic membrane layer, and then carrying out air drying naturally. The prepared metal surface black ceramic membrane layer has high black degree, uniform color, large thickness value, high density and hardness of the membrane layer, and good bonding strength with the metal matrix. The preparation process of the electrolyte is easy to operate, and is beneficial to realize batch production and industrial applications.
Description
Technical field
The invention belongs to field of metal surface treatment technology, be specifically related to a kind of metal differential arc oxidation electrolytic solution and surface black potteryization method.。
Background technology
Differential arc oxidation (claiming micro-plasma oxidation again) is a kind of through electrolytic solution and respective electrical combinations of parameters; In the TRANSIENT HIGH TEMPERATURE high pressure effect that aluminium, magnesium, titanium, zirconium, tantalum, niobium and alloy surface thereof rely on arc discharge to produce, growth in situ goes out with the substrate metal oxide novel surface treatment technology of the ceramic film that is the master.Prepared ceramic film and matrix bond are firm, compact structure, and toughness is high, has characteristics such as good wear-resisting, anti-corrosion, high temperature resistant impact and electrical isolation.Differential arc oxidization technique is implemented easily, and the rete function is easy to adjust, and technology is simple, and environmentally safe is a brand-new environment-friendly type metal process for treating surface, and is of many uses in industries such as Aeronautics and Astronautics, automobile, building, electronics, machinery, decorations.When being purpose with the protection usually, the metallic surface is as long as realize arc differential oxide ceramicization; But for used metalworks such as aircraft engine, part opticinstrument and some military devices, also requiring its surface ceramic rete is black, is beneficial to reduce reflecting rate or increases thermal radiation.In addition, because the decorate properties of black is excellent, the surface has the metal of black ceramic rete in field extensive application such as building, household electrical appliances and automobile makings.
At present, people have begun to carry out to obtain in the metallic surface correlative study of required color Micro-Arc Oxidized Ceramic Coating: application number be 200810051692.7 Chinese invention patent to adopt cupric sulfate pentahydrate be color additive, with ammoniacal liquor to Cu
2+Carry out adding electrolytic solution after the complexing, magnesiumalloy is carried out differential arc oxidation make the black ceramic rete on its surface; Application number is that 02111521.4 Chinese invention patent is a color additive with potassium permanganate or nickelous nitrate, makes colored retes such as light orange and coffee color at Mg alloy surface; Application number is that 200710056085.5 Chinese invention patent is color additive with the SRM 935a, and magnesium-rare earth is carried out differential arc oxidation, makes light green, medium green and dark green a series of green ceramic rete; Application number is that 200710125721.5 Chinese invention patent is a color additive with cupric pyrophosphate/copper sulfate, has made peach ceramic film at duraluminum and Mg alloy surface.But prior art exists tangible deficiency: utilize inorganic salt as color additive, it is higher to have a cost, problems such as contaminate environment; Resulting product surface ceramic rete is thin, and degree of blackness is lower, and micropore and crackle are on the high side, and the ceramic film density is not high enough; Formed pottery is mainly oxide ceramics, and quality is more crisp.
Colour carbon black is that gaseous state or liquid hydrocarbon polymer carry out incomplete combustion under the condition of lack of air or the decolorizing carbon that is generated is decomposed in hot tearing, and it is elementary composition to be main with carbon.When colour carbon black was heated to 2700 ℃ under not having the situation of oxygen, colour carbon black then was transformed into graphite.The chemically reactive of the colour carbon black after the greying and all will descend with the binding ability of matrix etc.
Colour carbon black is to use the most sophisticated a kind of blackout material in the modern industry, and light, heat and chemical reagent etc. are all had very high stability, has good weatherability, nontoxic, blackness and tinting strength advantages of higher.But, colour carbon black is used as the color additive that differential arc oxidation does not prepare metallic surface black ceramic rete as yet at present.Therefore, exploitation is the differential arc oxidation electrolytic solution and the metallic surface black ceramic rete preparation method of color additive with the colour carbon black, has great importance for the green preparation that promotes metallic surface high quality black ceramic rete.
Summary of the invention
The objective of the invention is to overcome the deficiency that exists in the existing differential of arc on metal surface oxidation black ceramic technology; Adopt promptly that inorganic salt are higher as the cost that color additive exists, environmental pollution is heavier; Ceramic film is thin, degree of blackness is lower, the rete density is not high; Problems such as the oxide ceramics quality is more crisp; Proposition with the mineral dye colour carbon black as color additive; Prepare the high quality Micro-Arc Oxidized Ceramic Coating that degree of blackness is high, one-tenth-value thickness 1/10 is big that constitutes jointly by carbon black fine particle, oxide compound and carbide in the metallic surface, a kind of eco-friendly low-cost metal differential arc oxidation electrolytic solution is provided, a kind of method that realizes differential of arc on metal surface oxidation black ceramicization also is provided.
A kind of metal differential arc oxidation electrolytic solution provided by the invention contains water glass, Sodium Fluoride, Pottasium Hydroxide, Trisodium Citrate, sodium wolframate and colour carbon black.The concentration of said water glass is 1.0 ~ 10.0g/L; The concentration of said Pottasium Hydroxide is 1.0 ~ 5.0g/L; The concentration of said Sodium Fluoride is 1.0 ~ 5.0g/L; The concentration of said sodium wolframate is 0.5 ~ 2.5g/L, and the concentration of said Trisodium Citrate is 0.3 ~ 0.9g/L, and said colour carbon black derives from the burnt black ink that concentration is 10.0 ~ 50.0mL/L.
A kind of metal differential arc oxidization surface black ceramic method provided by the invention is:
1, sample pre-treatment: the test button surface finish is smooth, carry out oil removal treatment then, use deionized water rinsing again, dry subsequent use;
2, electrolyte quota: water glass, Sodium Fluoride, Pottasium Hydroxide, Trisodium Citrate, sodium wolframate and colour carbon black are mixed, prepare required electrolytic solution;
3, electrical parameter setting: take constant current mode, current density 1 ~ 15A/dm
2, frequency 50 ~ 600Hz, dutycycle 10 ~ 90%, anode and cathode current density ratio 0.8 ~ 1.4, reaction times 15 ~ 60min;
4, differential arc oxidation: the ON cycle chilled water unit, sample is connected on the conducting rod immerses in the electrolytic solution as anode, the double negative electrode of doing of stainless steel electrolytic groove is opened the bidirectional pulse power supply, carries out differential arc oxidation and handles.
5, aftertreatment: the sample after the differential arc oxidation processing is taken out,, dry naturally then with deionized water rinsing gained black ceramic rete.
Adopt as in the accompanying drawing shown in Figure 2 0.1～1.0 totally ten grade degree of blackness coefficients increase progressively model, characterize in conjunction with the degree of blackness of the visual detection method of stipulating among the GB GB/T 14952.3-1994 ceramic film; Adopt TT230 type thickness measurement of eddy current appearance to measure the thickness of ceramic film.
Take water logging test and photostabilization testing method that the persistence of gained sample rete degree of blackness is detected.Wherein water logging test is that sample is immersed in temperature fully is that in whole test process, keeping the aqueous solution is constant temperature, and utilizes the sonic oscillation appearance that the aqueous solution is carried out the continuous ultrasound vibration in 60 ℃ the aqueous solution, and the test duration is 48 hours.The photostabilization test then is that sample is placed under the physical environment, stands natural light irradiation after for some time, observes its surperficial colourity changing conditions, and the time of this test is 30 days.After test is accomplished, detect according to the method for GB GB/T 14952.3-1994 defined changing conditions to rete aberration before and after the test.
Major advantage of the present invention is:
1, adopt the mineral dye colour carbon black to prepare the color additive of the required electrolytic solution of metallic surface black ceramic rete as differential arc oxidation, it is to use the most sophisticated blackout material in the industrial production, and is cheap and easy to get, environmental protection, and preparation cost is cheap; The electrolytic solution layoutprocedure is simple, and operation easily is beneficial to and realizes producing in batches and industrial applications.
2, adopt the metallic surface black ceramic rete degree of blackness of the inventive method preparation high, colourity is even, one-tenth-value thickness 1/10 is big, rete density and hardness are high, good with the metallic matrix bonding strength, and can obtain the ceramic film of different degree of blackness through adjusting concentration of electrolyte and related electrical parameters.
3, find through detecting, adopt the metallic surface black ceramic rete of the present invention's preparation to have good colourity persistence and photostabilization, satisfy actual request for utilization.
Description of drawings
The magnesium alloy sample that Fig. 1 prepares for the present invention with different degree of blackness Micro-Arc Oxidized Ceramic Coating.
Fig. 2 increases progressively model for the degree of blackness coefficient of the black ceramic rete that detection the present invention prepares.
Embodiment
Embodiment 1
Choosing sample is the AZ91D magnesiumalloy, and it is shaped as the sheet of 30mm * 30mm * 5mm, and concrete preparation process condition and operation steps are following:
1, sample pre-treatment: use 400#, 600#, 800# and 1000# sand papering smooth successively on the magnesium alloy sample surface, deionized water rinsing is used in oil removing in acetone then again, dries subsequent use;
2, electrolyte quota: preparing electrolyte solution 2L, each concentration of component is water glass 6.0g/L, Pottasium Hydroxide 2.0g/L, Sodium Fluoride 2.0g/L, sodium wolframate 2.0g/L, Trisodium Citrate 0.5g/L, burnt black ink 25.0mL/L in the electrolytic solution;
3, electrical parameter setting: take current constant mode, current density 2A/dm
2, frequency 600Hz, dutycycle 20%, anode and cathode current density ratio 1.0, reaction times 20min;
4, differential arc oxidation: the ON cycle chilled water unit, magnesium alloy sample is connected on the conducting rod immerses in the electrolytic solution as anode, the double negative electrode of doing of stainless steel electrolytic groove is opened the bidirectional pulse power supply, carries out differential arc oxidation and handles;
5, aftertreatment: the sample after the differential arc oxidation processing is taken out,, dry naturally then with deionized water rinsing gained black ceramic rete.
The magnesium alloy sample that Fig. 1 prepares for the present invention with different degree of blackness Micro-Arc Oxidized Ceramic Coating.Fig. 2 increases progressively model for the degree of blackness coefficient of the black ceramic rete that detection the present invention prepares.Adopt as in the accompanying drawing shown in Figure 2 0.1～1.0 totally ten grade degree of blackness coefficients increase progressively model, characterize in conjunction with the degree of blackness of the visual detection method of stipulating among the GB GB/T 14952.3-1994 ceramic film; Adopt TT230 type thickness measurement of eddy current appearance to measure the thickness of ceramic film.
Take water logging test and photostabilization testing method that the persistence of gained sample rete degree of blackness is detected.Wherein water logging test is that sample is immersed in temperature fully is that in whole test process, keeping the aqueous solution is constant temperature, and utilizes the sonic oscillation appearance that the aqueous solution is carried out the continuous ultrasound vibration in 60 ℃ the aqueous solution, and the test duration is 48 hours.The photostabilization test then is that sample is placed under the physical environment, stands natural light irradiation after for some time, observes its surperficial colourity changing conditions, and the time of this test is 30 days.After test is accomplished, detect according to the method for GB GB/T 14952.3-1994 defined changing conditions to rete aberration before and after the test.
Sample to preparing is estimated sign, finds that sample ceramic film surface is comparatively smooth and entire body is pitch-black, and degree of blackness reaches 1.0; The ceramic film average thickness value is 38.6 μ m; The black ceramic rete has good colourity persistence.
Embodiment 2
Choosing sample is the AZ91D magnesiumalloy, and it is shaped as the sheet of 30mm * 30mm * 5mm, and concrete preparation process condition and operation steps are following:
1, sample pre-treatment: with embodiment 1;
2, electrolyte quota: preparing electrolyte solution 2L, each concentration of component is water glass 8.0g/L, Pottasium Hydroxide 2.0g/L, Sodium Fluoride 2.0g/L, sodium wolframate 1.0g/L, Trisodium Citrate 0.3g/L, burnt black ink 20.0mL/L in the electrolytic solution;
3, electrical parameter setting: take current constant mode, current density 1A/dm
2, frequency 600Hz, dutycycle 20%, anode and cathode current density ratio 1.0, reaction times 15min;
4, differential arc oxidation: with embodiment 1;
5, aftertreatment: with embodiment 1.
Sample to preparing is estimated sign, finds that sample ceramic film surface is comparatively smooth and entire body is pitch-black, and degree of blackness reaches 0.9; The ceramic film average thickness value is 32.4 μ m; The black ceramic rete has good colourity persistence.
Embodiment 3
Choosing sample is the AZ91D magnesiumalloy, and it is shaped as the sheet of 30mm * 15mm * 5mm, and concrete preparation process condition and operation steps are following:
1, sample pre-treatment: with embodiment 1;
2, electrolyte quota: preparing electrolyte solution 2L, each concentration of component is water glass 10.0g/L, Pottasium Hydroxide 2.0g/L, Sodium Fluoride 3.0g/L, sodium wolframate 1.5g/L, Trisodium Citrate 0.9g/L, burnt black ink 15.0mL/L in the electrolytic solution;
3, electrical parameter setting: take current constant mode, current density 3A/dm
2, frequency 600Hz, dutycycle 20%, anode and cathode current density ratio 1.0, reaction times 15min;
4, differential arc oxidation: with embodiment 1;
5, aftertreatment: with embodiment 1.
Sample to preparing is estimated sign, finds that sample ceramic film surface is comparatively smooth and entire body is pitch-black, and degree of blackness reaches 0.9; The ceramic film average thickness value is 33.3 μ m; The black ceramic rete has good photostabilization.
Embodiment 4
Choosing sample is the LY12 duraluminum, and it is shaped as the disk shape of radius 25mm, thickness 5mm, and concrete preparation process condition and operation steps are following:
1, sample pre-treatment: use 400#, 600#, 800# and 1000# sand papering smooth successively on the aluminum alloy specimen surface, deionized water rinsing is used in oil removing in acetone then again, dries subsequent use;
2, electrolyte quota: preparing electrolyte solution 10L, each concentration of component is water glass 6.0g/L, Pottasium Hydroxide 2.0g/L, Sodium Fluoride 2.0g/L, sodium wolframate 2.5g/L, Trisodium Citrate 0.6g/L, burnt black ink 30.0mL/L in the electrolytic solution;
3, electrical parameter setting: take current constant mode, current density 10A/dm
2, frequency 50Hz, dutycycle 40%, anode and cathode current density ratio 1.0, reaction times 45min;
4, differential arc oxidation: the ON cycle chilled water unit, aluminum alloy specimen is connected on the conducting rod immerses in the electrolytic solution as anode, the double negative electrode of doing of stainless steel electrolytic groove is opened the bidirectional pulse power supply, carries out differential arc oxidation and handles;
5, aftertreatment: the sample after the differential arc oxidation processing is taken out,, dry naturally then with deionized water rinsing gained black ceramic rete.
Sample to preparing is estimated sign, finds that sample ceramic film surface is comparatively smooth and entire body is pitch-black, and degree of blackness reaches 1.0; The ceramic film average thickness value is 55.7 μ m; The black ceramic rete has good light fastness.
Embodiment 5
Choosing sample is the LY12 duraluminum, and it is shaped as the disk shape of radius 25mm, thickness 5mm, and concrete preparation process condition and operation steps are following:
1, sample pre-treatment: with embodiment 4;
2, electrolyte quota: preparing electrolyte solution 10L, each concentration of component is water glass 10.0g/L, Pottasium Hydroxide 4.0g/L, Sodium Fluoride 2.0g/L, sodium wolframate 2.0g/L, Trisodium Citrate 0.3g/L, burnt black ink 40.0mL/L in the electrolytic solution;
3, electrical parameter setting: take current constant mode, current density 15A/dm
2, frequency 100Hz, dutycycle 50%, anode and cathode current density ratio 0.8, reaction times 60min;
4, differential arc oxidation: with embodiment 4;
5, aftertreatment: with embodiment 4.
Sample to preparing is estimated sign, finds that sample ceramic film surface is comparatively smooth and entire body is pitch-black, and degree of blackness reaches 1.0; The ceramic film average thickness value is 65.8 μ m; The black ceramic rete has good colourity persistence.
Claims (2)
1. metal differential arc oxidation electrolytic solution, it is characterized in that: the composition of said metal differential arc oxidation electrolytic solution comprises: water glass, Sodium Fluoride, Pottasium Hydroxide, Trisodium Citrate, sodium wolframate and colour carbon black; Wherein, The concentration of said water glass is 1.0 ~ 10.0g/L; The concentration of said Pottasium Hydroxide is 1.0 ~ 5.0g/L, and the concentration of said Sodium Fluoride is 1.0 ~ 5.0g/L, and the concentration of said sodium wolframate is 0.5 ~ 2.5g/L; The concentration of said Trisodium Citrate is 0.3 ~ 0.9g/L, and said colour carbon black derives from the burnt black ink that concentration is 10.0 ~ 50.0mL/L.
2. metal differential arc oxidization surface black ceramic method is characterized in that: may further comprise the steps:
(1) sample pre-treatment: the test button surface finish is smooth, carry out oil removal treatment then, use deionized water rinsing again, dry subsequent use;
(2) electrolyte quota: water glass, Sodium Fluoride, Pottasium Hydroxide, Trisodium Citrate, sodium wolframate and colour carbon black are mixed, prepare required electrolytic solution;
(3) electrical parameter setting: take constant current mode, current density 1 ~ 15A/dm
2, frequency 50 ~ 600Hz, dutycycle 10 ~ 90%, anode and cathode current density ratio 0.8 ~ 1.4, reaction times 15 ~ 60min;
(4) differential arc oxidation: the ON cycle chilled water unit, sample is connected on the conducting rod immerses in the electrolytic solution as anode, the double negative electrode of doing of stainless steel electrolytic groove is opened the bidirectional pulse power supply, carries out differential arc oxidation and handles;
Aftertreatment: the sample after the differential arc oxidation processing is taken out,, dry naturally then with deionized water rinsing gained black ceramic rete.
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Cited By (9)
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| CN102797024A (en) * | 2012-09-11 | 2012-11-28 | 山东大学 | Method for carrying out micro-arc oxidation on blue-colored film layer by aluminum alloy |
| CN103014812A (en) * | 2012-11-23 | 2013-04-03 | 北京星航机电设备厂 | Process for coloring titanium alloy through micro-arc oxidation |
| CN104831332A (en) * | 2015-04-17 | 2015-08-12 | 江苏大学 | Method for directly generating black corrosion-resistant micro-arc oxidation film layer on steel surface |
| CN105525325A (en) * | 2016-01-12 | 2016-04-27 | 北京石油化工学院 | Surface treatment method for metal alloy |
| 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 |
| CN108531955A (en) * | 2018-05-31 | 2018-09-14 | 杭州泛亚卫浴股份有限公司 | One kind being used for bathroom metal works micro-arc oxidization surface processing method |
| CN109881234A (en) * | 2019-04-16 | 2019-06-14 | 北京石油化工学院 | A method of aluminium alloy is coloured by differential arc oxidation |
| CN110004476A (en) * | 2019-04-16 | 2019-07-12 | 北京石油化工学院 | A method of black ceramic layer is prepared in aluminum alloy surface |
| CN111172537A (en) * | 2017-11-23 | 2020-05-19 | 中国兵器工业第五九研究所 | Preparation method of stainless steel surface coating with excellent wear resistance and corrosion resistance |
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| CN102797024A (en) * | 2012-09-11 | 2012-11-28 | 山东大学 | Method for carrying out micro-arc oxidation on blue-colored film layer by aluminum alloy |
| CN102797024B (en) * | 2012-09-11 | 2015-01-21 | 山东大学 | Method for carrying out micro-arc oxidation on blue-colored film layer by aluminum alloy |
| CN103014812A (en) * | 2012-11-23 | 2013-04-03 | 北京星航机电设备厂 | Process for coloring titanium alloy through micro-arc oxidation |
| CN104831332A (en) * | 2015-04-17 | 2015-08-12 | 江苏大学 | Method for directly generating black corrosion-resistant micro-arc oxidation film layer on steel surface |
| CN104831332B (en) * | 2015-04-17 | 2017-09-29 | 江苏大学 | A kind of method that steel surface directly generates the anti-corrosion differential arc oxidation film layer of black |
| CN105525325A (en) * | 2016-01-12 | 2016-04-27 | 北京石油化工学院 | Surface treatment method for metal alloy |
| 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 |
| CN111172537A (en) * | 2017-11-23 | 2020-05-19 | 中国兵器工业第五九研究所 | Preparation method of stainless steel surface coating with excellent wear resistance and corrosion resistance |
| CN111172537B (en) * | 2017-11-23 | 2021-11-02 | 中国兵器工业第五九研究所 | Preparation method of stainless steel surface coating with excellent wear resistance and corrosion resistance |
| CN108531955A (en) * | 2018-05-31 | 2018-09-14 | 杭州泛亚卫浴股份有限公司 | One kind being used for bathroom metal works micro-arc oxidization surface processing method |
| CN109881234A (en) * | 2019-04-16 | 2019-06-14 | 北京石油化工学院 | A method of aluminium alloy is coloured by differential arc oxidation |
| CN110004476A (en) * | 2019-04-16 | 2019-07-12 | 北京石油化工学院 | A method of black ceramic layer is prepared in aluminum alloy surface |
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