CN102277606A - Preparation method of thermal barrier coating on surface of aluminum-magnesium alloy and composite material of alloy - Google Patents
Preparation method of thermal barrier coating on surface of aluminum-magnesium alloy and composite material of alloy Download PDFInfo
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- CN102277606A CN102277606A CN2010101962335A CN201010196233A CN102277606A CN 102277606 A CN102277606 A CN 102277606A CN 2010101962335 A CN2010101962335 A CN 2010101962335A CN 201010196233 A CN201010196233 A CN 201010196233A CN 102277606 A CN102277606 A CN 102277606A
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Abstract
The invention provides a preparation method of a thermal barrier coating on the surface of an aluminum-magnesium alloy and a composite material of the alloy. The preparation method is characterized in that the thermal barrier coating on the surface of the aluminum-magnesium alloy and the composite material of the alloy is prepared by carrying out electrolytic oxidation on the surface of the aluminum-magnesium alloy and the composite material of the alloy with a silicatic and phosphatic system plasma electrolyte to form a film medium, and carrying out electrophoretic deposition on the plasma electrolytic oxidation film (the film medium) with an electrophoretic deposition electrolyte. A plasma electrolytic oxidation-electrophoresis composite ceramic layer obtained with the preparation method of the invention, which has the advantages of smooth surface, firm combination, controllable thickness, densification and less aperture, good thermal insulation and thermal shock resistance, is suitable for workpieces with various dimensions and surfaces of complicated shapes.
Description
Technical field
The invention belongs to material surface coating coating technology field, relate to the preparation method of a kind of aluminium, magnesium alloy and composite material surface thermal barrier coating thereof.
Background technology
The non-ferrous metal of, light weight little as density, aluminium, magnesium alloy and matrix material thereof are extensively adopted by all multiple components such as automobile, aviation gas engine, ordnance engine equipments in recent years, for the lightweight development of product provides direction.But because the hot strength and the creep property of aluminium, magnesium alloy self are all lower, limited the application of aluminium, magnesium alloy and matrix material thereof, caused it to be difficult to satisfy the complex working condition of high temperature, high pressure, high corrosive medium etc. in high temperature (150～350 ℃) occasion.For this reason, this area is normally adopted and is carried out thermal barrier coating at material surface and handle and reduce the material surface thermal load, and then improves the high thermal resistance of member integral body and anti-ablative.Thermal barrier coating plays an important role to the use temperature of further raising alloy material, can improve 100～150 ℃ of use temperatures.
In the prior art, the thermal barrier coating Technology mainly contains thermospray, electro beam physics vapour deposition technology such as (EB-PVD).Hot-spraying techniques is not subjected to the restriction of body material, and operating procedure is flexible, and coat-thickness is controlled, but the bonding force of the ceramic layer of spraying and aluminum substrate is poor, and the high temperature ceramic easily be full of cracks in running back is down peeled off.The thermal barrier coating weave construction of EB-PVD method preparation has good strain ability to bear, thereby improved the performance of the thermal fatigue resistance of coating greatly, but, the sedimentation rate of EB-PVD is lower, and the equipment manufacturing cost costliness is influenced by the element vapour pressure, the Composition Control of coating is difficulty, the matrix part needs heating, and specimen size can not be too big, and these have all limited the industrialization promotion of this method to a great extent.Can improve its surface property to a certain extent though use hard anodizing, ion plating, chemistry or physical vapor deposition TiN (or CrN) coating technology, but in the face of the service condition under high speed and the high contact stress time, still be apparent not enough, also can bring certain environmental problem simultaneously.In addition, utilize the effect of the heat insulation of ceramic layer and reduction stress concentration, at the firm thermal insulation ceramics of engine component surface spraying one deck also is the common a kind of selection in this area, but the spraying ceramic layer because and aluminum substrate between have the tangible separation surface of one deck, difference of thermal expansion coefficients is bigger, thermo-labile impact easily comes off in thermal cycling.
Summary of the invention
The objective of the invention is to the problem that prior art exists is solved, so provide a kind of simple to operate, coated component to be easy to control, product is high temperature resistant and anti-ablation property is good, the preparation method of the aluminium, magnesium alloy and the composite material surface thermal barrier coating thereof that are suitable for industrial applications.
The preparation method who is used to finish the foregoing invention purpose a kind ofly can improve that aluminium, magnesium alloy and composite material surface thereof are heat insulation, the plasma electrolysis oxidation of resistance toheat-electrophoresis composite treatment process, the realization of its technical scheme is: make aluminium, magnesium alloy and composite material surface electrolytic oxidation filming medium thereof by silicate and phosphate system plasma electrolysis liquid earlier, again on plasma electrolysis oxidation film basis with the electrophoretic deposition of electrophoretic deposition electrolytic solution, make aluminium, magnesium alloy and composite material surface thermal barrier coating thereof.
In the technical solution of the present invention, plasma electrolysis liquid by the prescription of substance weight and cumulative volume ratio is: silicate 1～50g/L, phosphoric acid salt 1～40g/L, all the other are deionized water, wherein silicate, the phosphoric acid salt in the plasma electrolysis liquid is its sodium salt or sylvite; Electrophoretic deposition electrolytic solution is Zr (OH)
2Colloidal electrolyte, every liter of Zr (OH)
2Colloidal electrolyte is formed by zirconate 1～50g/L and alkali lye 1～20g/L and deionized water reaction, wherein is used for reaction generation Zr (OH)
2The zirconate of colloidal electrolyte is its sodium salt or sylvite, and alkali lye is sodium hydroxide solution or potassium hydroxide solution.
Realization of the present invention is that also the preparation method of described aluminium, magnesium alloy or its composite material surface thermal barrier coating comprises following step of preparation process:
1) adding pH regulator agent adjusting pH value earlier in deionized water is 8～12, presses configuration proportion then and adds silicate and phosphoric acid salt, makes plasma electrolysis liquid;
2) adding pH regulator agent adjusting pH value earlier in other part deionized water is 3～7, presses configuration proportion then and adds zirconate and alkali lye, makes electrophoretic deposition electrolytic solution;
3) be anode with aluminium, magnesium alloy and matrix material thereof, stainless steel is a negative electrode, in the plasma electrolysis liquid for preparing, adopts the pulse power, at constant current density 2～30A/dm
2, frequency is 50～2000HZ, dutycycle is 5～50%, distance is to carry out plasma electrolytic oxidation under the condition of 5～30cm between cathode-anode plate, keep 10～50 ℃ of electrolyte temperatures, the treatment time is 2～90min, makes aluminium, magnesium alloy and composite material surface electrolytic oxidation filming medium thereof;
4) to be anode through aluminium, magnesium alloy and matrix material thereof behind the plasma electrolytic oxidation, stainless steel is a negative electrode, in the electrophoretic deposition electrolytic solution for preparing, adopts the pulse power, at constant current density 5～20A/dm
2, frequency is 50～500HZ, and dutycycle is 5～30%, and distance is to carry out electrophoretic deposition under the condition of 5～30cm between cathode-anode plate, keeps 50～90 ℃ of electrolyte temperatures, and the treatment time is 2～90min, makes aluminium, magnesium alloy and composite material surface thermal barrier coating thereof.
In the embodiment of the present invention, adopt plasma electrolysis oxidation (Plasma Electrolytic Oxidation, english abbreviation PEO) technology can overcome between aluminium, magnesium alloy component surface spraying thermal insulation ceramics layer and the aluminum substrate bigger, the thermo-labile impact of difference of thermal expansion coefficients and caducous shortcoming in thermal cycling, can prepare in conjunction with good ceramic coating, thereby reach excellent effect of heat insulation at aluminium, Mg alloy surface.The ceramic layer that this method forms since high rigidity, high anti-corrosion, strong, high temperature oxidation resisting, good insulating with basal body binding force be specially adapted to high-speed motion and need high abrasion, the ballistic light metal alloy component of high temperature resistance.In addition, another advantage of this method is its cleanliness without any pollution, belongs to the environment-friendly type process of surface treatment.
Traditional PEO technology can only obtain the single ceramic coating identical with the matrix composition at matrix surface, the Al that forms behind plasma electrolysis oxidation as aluminium, magnesium alloy
2O
3With the MgO ceramic membrane, but single ceramic film also can not effectively reach effect of heat insulation.In order to obtain the good thermal barrier coating of heat insulation temperature, the present invention adopts plasma electrolysis oxidation-electrophoresis composite treatment technology, prepares to contain ZrO
2The complex phase ceramic film.ZrO
2Higher because of its fusing point that has, electric conductivity is low, anti-oxidant, corrosion-resistant, thermal structure stability is good, the more high plurality of advantages of physical strength becomes stupalith the best in the thermal barrier coating, and ZrO
2Thermal expansivity is also approaching with the thermal expansivity of metal, so ZrO
2It is the preferred material of thermal barrier coating.
Compared with prior art, the present invention has the following advantages:
1, plasma electrolysis oxidation, the electrophoretic deposition electrolytic solution of the present invention's employing do not contain human body and the deleterious toxic positively charged ion (Cr of environment
6+Deng), solution composition is simple, is easy to control, does not contain easy decomposition composition, process stabilizing;
2, smooth, the controllable thickness of the film surface that adopts the present invention to make and fine and close few hole, in conjunction with firmly, high, the heat insulation heat resisting temperature height of hardness, thermal shock resistance be good, detect through experiment, thicknesses of layers is 10～150 μ m, bonding strength is 10～40MPa, surface hardness is 400～1000HV, 30～80 ℃ of heat insulation temperature are at 500 flawlesses of 300 ℃ of warm shakes;
3, raw material of the present invention be easy to get, cheap, constant current oxidation, simple to operate, be suitable for suitability for industrialized production.
Embodiment
The present invention will be further described below with reference to embodiment.
Embodiment one
Plasma electrolysis liquid is silicate and phosphate system, and adding pH regulator agent adjusting pH value in deionized water earlier is 9～10, adds water glass and sodium phosphate then, by weight with the cumulative volume ratio, get water glass 10g/L, sodium phosphate 15g/L makes plasma electrolysis liquid.Alloy sample is placed electrolytic solution, connect positive source, stainless steel connects power cathode, adopts galvanostatic method control differential arc oxidation process, and current density is 3A/dm
2, oxidization time 10min.From experimental phenomena, reacting balance.Striking voltage is 183V, and final voltage is 270V.Prolong with oxidization time, spark transfers safran to from brilliant white, sends atomic weak explosion in the experimentation.Specimen surface evenly generates the plasma electrolysis oxidation ceramic layer of the smooth densification of one deck light gray-white after the oxidation, can find out that from its microcosmic SEM surface topography map the surface has than macroscopic void, and is better with matrix bond.Electrophoretic deposition electrolytic solution is Zr (OH)
2Colloidal electrolyte, adding pH regulator agent adjusting pH value in deionized water earlier is 5～6, adds sodium zirconate and sodium hydroxide then, with the cumulative volume ratio, gets sodium zirconate 15g/L by weight, sodium hydroxide 15g/L makes electrophoretic deposition electrolytic solution.To place electrophoretic deposition electrolytic solution through the alloy sample behind the plasma electrolytic oxidation, and connect positive source, stainless steel connects power cathode, at constant current density 10A/dm
2Frequency is 200HZ, dutycycle is 20%, distance is kept 70 ℃ of electrolyte temperatures for carrying out electrophoretic deposition under the condition of 20cm between cathode-anode plate, and the treatment time is 10min, make aluminium, magnesium alloy and composite material surface thermal barrier coating thereof, by plasma electrolysis oxidation-electrophoretic deposition composite film surface and cross section scanning electron microscope shape appearance figure as can be seen, the fine and close hole less of film surface, and intact with matrix bond.
Embodiment two
Plasma electrolysis liquid is silicate and phosphate system, with the cumulative volume ratio, gets potassium silicate 20g/L by weight, potassiumphosphate 15g/L, and current density is 5A/dm
2, oxidization time 20min.Striking voltage is 145V, and final voltage is 295V, and all the other operate same precedent.Because electrolyte concentration is big, oxidization time is longer, and from being coated with the SEM shape appearance figure of layer cross section, thick but roughness increases the rete of generation than precedent.Electrophoretic deposition electrolytic solution is Zr (OH)
2Colloidal electrolyte with the cumulative volume ratio, is got potassium zirconium 15g/L, potassium hydroxide 15g/L, current density 8A/dm by weight
2,, the treatment time is 15min, all the other operate same precedent.By plasma electrolysis oxidation-electrophoretic deposition composite film surface and cross section scanning electron microscope shape appearance figure as can be seen, the fine and close hole less of film surface, and intact with matrix bond.
Embodiment three
Plasma electrolysis oxidation electrolytic solution is silicate and phosphate system, with the cumulative volume ratio, gets water glass 20g/L by weight, sodium phosphate 15g/L, and current density is 3A/dm
2, oxidization time 2min, the pH value is controlled at 8～12, and striking voltage is 175V, and final voltage is 192V, and all the other are operated with embodiment one.Electrophoretic deposition electrolytic solution forms depositing current density 8A/dm by sodium zirconate 20g/L and sodium hydroxide 20g/L reaction
2, electrophoresis time 30min.The pH value is controlled at 3～7, and all the other are operated with embodiment one.
Embodiment four
Plasma electrolysis oxidation electrolytic solution is silicate and phosphoric acid salt compound system, with the cumulative volume ratio, gets silicate 20g/L by weight, phosphoric acid salt 15g/L, and current density is 5A/dm
2, oxidization time 5min, the pH value is controlled at 8～12, and striking voltage is 175V, and final voltage is 203V.Electrophoretic deposition electrolytic solution forms depositing current density 10A/dm by zirconate 30g/L and alkali lye 30g/L reaction
2, electrophoresis time 30min.The pH value is controlled at 3～7.All the other operations except above-mentioned points are all with embodiment one.
Embodiment five
Plasma electrolysis oxidation electrolytic solution is silicate and phosphoric acid salt compound system, with the cumulative volume ratio, gets silicate 20g/L by weight, phosphoric acid salt 25g/L, and current density is 5A/dm
2, oxidization time 3min, the pH value is controlled at 8～12, and striking voltage is 135V, and final voltage is 172V.Electrophoretic deposition electrolytic solution is formed by zirconate 15g/L and alkali lye 15g/L reaction.Depositing current density 10A/dm
2, electrophoresis time 30min, the pH value is controlled at 3～7.All the other operations except above-mentioned points are all with embodiment one.
Claims (6)
1. the preparation method of an aluminium, magnesium alloy and composite material surface thermal barrier coating thereof, it is characterized in that making aluminium, magnesium alloy and composite material surface electrolytic oxidation filming medium thereof by silicate and phosphate system plasma electrolysis liquid earlier, again on plasma electrolysis oxidation film basis with the electrophoretic deposition of electrophoretic deposition electrolytic solution, make aluminium, magnesium alloy and composite material surface thermal barrier coating thereof.
2. the preparation method of aluminium according to claim 1, magnesium alloy or its composite material surface thermal barrier coating, it is characterized in that plasma electrolysis liquid by the prescription of substance weight and cumulative volume ratio is: silicate 1～50g/L, phosphoric acid salt 1～40g/L, all the other are deionized water.
3. the preparation method of aluminium according to claim 2, magnesium alloy or its composite material surface thermal barrier coating is characterized in that silicate, the phosphoric acid salt in the plasma electrolysis liquid is its sodium salt or sylvite.
4. the preparation method of aluminium according to claim 1, magnesium alloy or its composite material surface thermal barrier coating is characterized in that electrophoretic deposition electrolytic solution is Zr (OH)
2Colloidal electrolyte, every liter of Zr (OH)
2Colloidal electrolyte is formed by zirconate 1～50g/L and alkali lye 1～20g/L and deionized water reaction.
5. the preparation method of aluminium according to claim 4, magnesium alloy or its composite material surface thermal barrier coating is characterized in that being used for reaction and generates Zr (OH)
2The zirconate of colloidal electrolyte is its sodium salt or sylvite, and alkali lye is sodium hydroxide solution or potassium hydroxide solution.
6. according to the preparation method of claim 1,2 or 4 described aluminium, magnesium alloy or its composite material surface thermal barrier coating, it is characterized in that comprising following step of preparation process:
1) adding pH regulator agent adjusting pH value earlier in deionized water is 8～12, presses configuration proportion then and adds silicate and phosphoric acid salt, makes plasma electrolysis liquid;
2) adding pH regulator agent adjusting pH value earlier in other part deionized water is 3～7, presses configuration proportion then and adds zirconate and alkali lye, makes electrophoretic deposition electrolytic solution;
3) be anode with aluminium, magnesium alloy and matrix material thereof, stainless steel is a negative electrode, in the plasma electrolysis liquid for preparing, adopts the pulse power, at constant current density 2～30A/dm
2, frequency is 50～2000HZ, dutycycle is 5～50%, distance is to carry out plasma electrolytic oxidation under the condition of 5～30cm between cathode-anode plate, keep 10～50 ℃ of electrolyte temperatures, the treatment time is 2～90min, makes aluminium, magnesium alloy and composite material surface electrolytic oxidation filming medium thereof;
4) to be anode through aluminium, magnesium alloy and matrix material thereof behind the plasma electrolytic oxidation, stainless steel is a negative electrode, in the electrophoretic deposition electrolytic solution for preparing, adopts the pulse power, at constant current density 5～20A/dm
2, frequency is 50～500HZ, and dutycycle is 5～30%, and distance is to carry out electrophoretic deposition under the condition of 5～30cm between cathode-anode plate, keeps 50～90 ℃ of electrolyte temperatures, and the treatment time is 2～90min, makes aluminium, magnesium alloy and composite material surface thermal barrier coating thereof.
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| CN104562154A (en) * | 2015-01-06 | 2015-04-29 | 中国科学院金属研究所 | Zr-based ceramic coating protection method for surface of refractory metal material |
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| CN114540842A (en) * | 2022-02-25 | 2022-05-27 | 山东第一医科大学附属省立医院(山东省立医院) | Device for preparing sodium hypochlorite disinfection colloid by electrolyzing salt |
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| CN104911663A (en) * | 2012-05-10 | 2015-09-16 | 中国兵器工业第五九研究所 | Durable surface coating layer preparation method and system |
| CN102634832A (en) * | 2012-05-10 | 2012-08-15 | 中国兵器工业第五九研究所 | Method for preparing aluminum alloy element surface coating and system thereof |
| CN102634832B (en) * | 2012-05-10 | 2015-04-22 | 中国兵器工业第五九研究所 | Method for preparing aluminum alloy element surface coating and system thereof |
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| CN104911662A (en) * | 2012-05-10 | 2015-09-16 | 中国兵器工业第五九研究所 | Preparation method of composite ceramic coating layer |
| CN104911662B (en) * | 2012-05-10 | 2017-05-10 | 中国兵器工业第五九研究所 | Preparation method of composite ceramic coating layer |
| CN102677127B (en) * | 2012-06-11 | 2014-08-06 | 西北有色金属研究院 | Magnesium alloy microarc oxidation-electrophoresis composite coating and preparation method thereof |
| CN102677127A (en) * | 2012-06-11 | 2012-09-19 | 西北有色金属研究院 | Magnesium alloy microarc oxidation-electrophoresis composite coating and preparation method thereof |
| CN104562154A (en) * | 2015-01-06 | 2015-04-29 | 中国科学院金属研究所 | Zr-based ceramic coating protection method for surface of refractory metal material |
| CN108504983A (en) * | 2018-07-10 | 2018-09-07 | 中国科学院长春应用化学研究所 | A kind of Mg alloy surface new construction thermal barrier coating and preparation method thereof |
| CN108504983B (en) * | 2018-07-10 | 2019-06-18 | 中国科学院长春应用化学研究所 | A kind of Mg alloy surface new construction thermal barrier coating and preparation method thereof |
| CN113431696A (en) * | 2021-06-29 | 2021-09-24 | 潍柴动力股份有限公司 | Cylinder cover and preparation device and preparation method of composite coating |
| CN113431696B (en) * | 2021-06-29 | 2023-04-18 | 潍柴动力股份有限公司 | Cylinder cover and preparation device and preparation method of composite coating |
| CN114540842A (en) * | 2022-02-25 | 2022-05-27 | 山东第一医科大学附属省立医院(山东省立医院) | Device for preparing sodium hypochlorite disinfection colloid by electrolyzing salt |
| CN114540842B (en) * | 2022-02-25 | 2024-01-19 | 山东第一医科大学附属省立医院(山东省立医院) | Device for preparing sodium hypochlorite disinfection colloid by electrolyzing salt |
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