CN105174986A - Silicon carbide fiber-based magnesium oxide-alumina double-layer coating preparation method - Google Patents
Silicon carbide fiber-based magnesium oxide-alumina double-layer coating preparation method Download PDFInfo
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- CN105174986A CN105174986A CN201510555074.6A CN201510555074A CN105174986A CN 105174986 A CN105174986 A CN 105174986A CN 201510555074 A CN201510555074 A CN 201510555074A CN 105174986 A CN105174986 A CN 105174986A
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Abstract
The invention provides a silicon carbide fiber-based magnesium oxide-alumina double-layer coating preparation method, wherein the oxide coating comprises two layers, the inner layer component is magnesium oxide, and the outer layer component is alumina. The specific preparation method comprises: adding magnesium oxide particles to alcohol, carrying out wet ball milling to obtain fine powder, spraying the fine powder of the magnesium oxide onto pre-treated silicon carbide fiber bundle or fiber braiding body by using a plasma spraying technology to obtain silicon carbide fibers with the magnesium oxide coating, mixing aluminum isopropoxide, deionized water and a nitric acid solution to prepare an alumina sol, and carrying out immersing coating of the alumina sol onto the silicon carbide fibers so as to finally prepare the oxide coating adopting the silicon carbide fibers as the matrix. According to the present invention, the different processes are respectively used to prepare the alumina coating and the magnesium oxide coating, the operation steps are simple and easy to perform, and the high temperature resistance and the anti-oxidation property of the silicon carbide fibers are substantially improved.
Description
Technical field
The present invention relates to a kind of preparation method of oxide coating, particularly relate to a kind of preparation method of silicon carbide fiber base magnesia-alumina duplex coating.
Background technology
The application of known aluminum oxide coating layer is very extensive, comprises electric and optics industry etc.Aluminum oxide coating layer can be deposited on various matrix, and these matrixes comprise metal, semiconductor material and glass.The method preparing coating has a lot, such as chemical vapour deposition, spray pyrolysis and magnetron sputtering etc.Silicon carbide fiber to refer in fibrous texture the main fiber containing Si, C two kinds of elements, is one of important ceramic fiber.Silicon carbide fiber can be used as high-temperature heat-resistance material, is made into high-temperature resistant belt conveyer, high-temperature smoke strainer, metal melt filtering material etc.Because aluminum oxide has extremely strong oxidation-resistance, therefore in order to improve silicon carbide fiber oxidation-resistance at high temperature, can consider to prepare the ceramic coating that one deck take aluminum oxide as main component on its surface.
Application publication number is that the Chinese invention patent of CN103643276A discloses a kind of method at lead alloy surface growth alumina coating, first lead alloy is heat-treated, lead alloy surface is made to generate oxide film, then lead alloy is placed in the electrolytic solution based on alcohol and aluminum nitrate, with pulse direct current or the input of pulse ac voltage, under the effect of liquid phase plasma, prepare alumina coating at lead alloy surface.Coating prepared by this invention and lead alloy have good bonding strength and corrosion-resistant intensity, enhance the corrosion resistance of lead alloy in wet environment, can also delay the work-ing life of lead-acid cell and delay the corrosion of lead alloy nuke rubbish tank, protection of the environment.
Application publication number is that the Chinese invention patent of CN104141122A discloses a kind of metal base surface aluminum oxide coating layer and preparation method thereof, aluminum oxide coating layer is formed primarily of γ phase alumina, thickness is between 1 micron to 10 microns, and matrix is the alloy material such as carbon steel, structure iron.By the organic alcohol compound of water, aluminium and mineral acid proportionally heated and stirred acquisition alumina sol, afterwards colloidal sol is carried out hydrothermal treatment consists, again colloidal sol is repeatedly applied drying at metal base surface, carry out calcination processing in last hot environment below 500 DEG C, obtain and there is certain thickness, fine and close γ phase alumina coating.The aluminum oxide coating layer that this invention provides not only anticorrosive, anti-permeability well, and has certain thickness and good compactness.
Foregoing invention is all aimed at aluminum oxide coating layer prepared by metallic matrix, and is directed to silicon carbide fiber, preferably by aluminum oxide and the mixing of other oxide compound, can prepare the oxide compound composite ceramic coat with excellent properties.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, and providing a kind of take silicon carbide fiber as the preparation method of the magnesia-alumina duplex coating of matrix.
The technical scheme adopted for realizing object of the present invention is: providing a kind of take silicon carbide fiber as the magnesia-alumina duplex coating of matrix, it is characterized in that described oxide coating thickness is 5 ~ 25 μm, altogether comprise two-layer, nexine composition is magnesium oxide, thickness is 1 ~ 10 μm, outer composition of layer is aluminum oxide, and thickness is 4 ~ 15 μm.
Present invention also offers a kind of take silicon carbide fiber as the preparation method of the magnesia-alumina duplex coating of matrix, it is characterized in that comprising following operative step:
(1) silicon carbide fiber bundle or fibrage body are placed in tube furnace are warming up to 300 ~ 500 DEG C of insulations 20 ~ 50 minutes, then put into acetone ultrasonic cleaning 10 ~ 40 minutes, then at room temperature dry, to remove surface contaminants;
(2) take appropriate magnesium oxide particle, added in alcohol and carry out wet ball grinding 5 ~ 10 hours, then oven dry is sieved, obtain the fine powder material that granularity is 1 ~ 10 μm;
(3) utilize plasma spraying technology to be sprayed on silicon carbide fiber bundle or fibrage body by magnesian fine powder material, obtain the silicon carbide fiber with magnesium oxide coating, coat-thickness is 1 ~ 10 μm;
(4) after aluminum isopropylate, deionized water and salpeter solution being mixed according to a certain percentage, 80 ~ 95 DEG C of stirring reactions 5 ~ 15 hours, then 75 ~ 90 DEG C of heating reflux reactions 5 ~ 10 hours, alumina sol is obtained;
(5) the silicon carbide fiber bundle or fibrage body with magnesium oxide coating to be immersed in alumina sol 3 ~ 8 minutes, then to take out and dry, complete single-steeping, repeat said process 10 ~ 30 times;
(6) sample obtained by said process is incubated 1 ~ 3 hour at 500 ~ 800 DEG C, and silicon carbide fiber bundle or fibrage body obtain 4 ~ 15 μm of thick aluminum oxide coating layers, and finally preparing with silicon carbide fiber is the oxide coating of matrix.
Wherein, in step (2), the ratio of magnesium oxide particle and alcohol is (0.5 ~ 2g): 10ml.
Wherein, in step (4), the ratio of aluminum isopropylate, deionized water and salpeter solution is (1 ~ 5g): (40 ~ 60ml): (1 ~ 5ml), the concentration of salpeter solution is 0.01 ~ 0.2mol/L.
Effect: the present invention compared with prior art, has the following advantages: (1) adopts different process to prepare aluminum oxide and magnesium oxide coating respectively, and operation steps is simple; (2) combine aluminum oxide and magnesium oxide feature performance benefit separately, increase substantially high thermal resistance and the oxidation-resistance of silicon carbide fiber.
Embodiment
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims and limited.
embodiment 1
(1) silicon carbide fiber bundle is placed in tube furnace is heated to 400 DEG C of insulations 40 minutes, then put into acetone ultrasonic cleaning 20 minutes, then at room temperature dry, to remove surface contaminants; (2) magnesium oxide particle and alcohol are mixed according to the ratio of 1g:10ml, wet ball grinding 6 hours, then oven dry is sieved, obtain the fine powder material that granularity is 1 ~ 10 μm; (3) utilize plasma spraying technology to be sprayed on silicon carbide fiber bundle by magnesian fine powder material, obtain the silicon carbide fiber with magnesium oxide coating; (4) by the salpeter solution of aluminum isopropylate, deionized water and 0.05mol/L according to after the ratio mixing of 1g:25ml:1ml, 85 DEG C of stirring reactions 8 hours, then 80 DEG C of heating reflux reactions 6 hours, obtain alumina sol; (5) the silicon carbide fiber bundle with magnesium oxide coating to be immersed in alumina sol 5 minutes, then to take out and dry, complete single-steeping, repeat said process 15 times; (6) sample obtained by said process is incubated 1.5 hours at 600 DEG C, and silicon carbide fiber bundle obtains aluminum oxide coating layer, and finally preparing with silicon carbide fiber is the oxide coating of matrix.
embodiment 2
(1) silicon carbide fiber bundle is placed in tube furnace is heated to 450 DEG C of insulations 30 minutes, then put into acetone ultrasonic cleaning 25 minutes, then at room temperature dry, to remove surface contaminants; (2) magnesium oxide particle and alcohol are mixed according to the ratio of 1.5g:10ml, wet ball grinding 7 hours, then oven dry is sieved, obtain the fine powder material that granularity is 1 ~ 10 μm; (3) utilize plasma spraying technology to be sprayed on silicon carbide fiber bundle by magnesian fine powder material, obtain the silicon carbide fiber with magnesium oxide coating; (4) by the salpeter solution of aluminum isopropylate, deionized water and 0.1mol/L according to after the ratio mixing of 3g:50ml:3ml, 90 DEG C of stirring reactions 10 hours, then 85 DEG C of heating reflux reactions 7 hours, obtain alumina sol; (5) the silicon carbide fiber bundle with magnesium oxide coating to be immersed in alumina sol 6 minutes, then to take out and dry, complete single-steeping, repeat said process 20 times; (6) sample obtained by said process is incubated 2 hours at 700 DEG C, and silicon carbide fiber bundle obtains aluminum oxide coating layer, and finally preparing with silicon carbide fiber is the oxide coating of matrix.
Above are only two embodiments of the present invention, but design concept of the present invention is not limited thereto, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content not departing from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (1)
1. a preparation method for silicon carbide fiber base magnesia-alumina duplex coating, is characterized in that described oxide coating thickness is 5 ~ 25 μm, altogether comprises two-layer, nexine composition is magnesium oxide, thickness is 1 ~ 10 μm, and outer composition of layer is aluminum oxide, and thickness is 4 ~ 15 μm; The method preparing this coating comprises the step of following order:
(1) silicon carbide fiber bundle or fibrage body are placed in tube furnace are warming up to 300 ~ 500 DEG C of insulations 20 ~ 50 minutes, then put into acetone ultrasonic cleaning 10 ~ 40 minutes, then at room temperature dry, to remove surface contaminants;
(2) take appropriate magnesium oxide particle, added in alcohol and carry out wet ball grinding 5 ~ 10 hours, then oven dry is sieved, obtain the fine powder material that granularity is 1 ~ 10 μm, the ratio of magnesium oxide particle and alcohol is (0.5 ~ 2g): 10ml;
(3) utilize plasma spraying technology to be sprayed on silicon carbide fiber bundle or fibrage body by magnesian fine powder material, obtain the silicon carbide fiber with magnesium oxide coating, coat-thickness is 1 ~ 10 μm;
(4) after aluminum isopropylate, deionized water and salpeter solution being mixed according to a certain percentage, 80 ~ 95 DEG C of stirring reactions 5 ~ 15 hours, then 75 ~ 90 DEG C of heating reflux reactions 5 ~ 10 hours, obtain alumina sol, the ratio of aluminum isopropylate, deionized water and salpeter solution is (1 ~ 5g): (40 ~ 60ml): (1 ~ 5ml), and the concentration of salpeter solution is 0.01 ~ 0.2mol/L;
(5) the silicon carbide fiber bundle or fibrage body with magnesium oxide coating to be immersed in alumina sol 3 ~ 8 minutes, then to take out and dry, complete single-steeping, repeat said process 10 ~ 30 times;
(6) sample obtained by said process is incubated 1 ~ 3 hour at 500 ~ 800 DEG C, and silicon carbide fiber bundle or fibrage body obtain 4 ~ 15 μm of thick aluminum oxide coating layers, and finally preparing with silicon carbide fiber is the oxide coating of matrix.
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Cited By (6)
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| CN107417270A (en) * | 2016-05-24 | 2017-12-01 | 江苏美佳马达有限公司 | A kind of preparation method of slug type calcium lanthanum ferrite permanent-magnet materials |
| CN108176249A (en) * | 2017-12-28 | 2018-06-19 | 南京工业大学 | A kind of preparation method of SiC nano fiber film |
| CN109608176A (en) * | 2018-12-18 | 2019-04-12 | 辽宁省轻工科学研究院有限公司 | A kind of novel ablation dimension shape fiber coat and preparation, construction method |
| CN112142498A (en) * | 2020-09-15 | 2020-12-29 | 上海富乐华半导体科技有限公司 | Backing plate for simultaneous sintering of copper foils on two sides of DBC substrate and preparation method thereof |
| CN113121206A (en) * | 2019-12-30 | 2021-07-16 | 辽宁省轻工科学研究院有限公司 | Preparation method of inner wall ceramic coating for pseudo spark switch |
| CN115093209A (en) * | 2022-07-05 | 2022-09-23 | 江苏锡沂高新材料产业技术研究院有限公司 | Preparation method of high-strength high-stability multilayer composite structure fused quartz material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107417270A (en) * | 2016-05-24 | 2017-12-01 | 江苏美佳马达有限公司 | A kind of preparation method of slug type calcium lanthanum ferrite permanent-magnet materials |
| CN108176249A (en) * | 2017-12-28 | 2018-06-19 | 南京工业大学 | A kind of preparation method of SiC nano fiber film |
| CN108176249B (en) * | 2017-12-28 | 2021-03-30 | 南京工业大学 | Preparation method of silicon carbide nanofiber membrane |
| CN109608176A (en) * | 2018-12-18 | 2019-04-12 | 辽宁省轻工科学研究院有限公司 | A kind of novel ablation dimension shape fiber coat and preparation, construction method |
| CN109608176B (en) * | 2018-12-18 | 2021-11-05 | 辽宁省轻工科学研究院有限公司 | Ablation fiber-shaped coating and preparation and construction methods thereof |
| CN113121206A (en) * | 2019-12-30 | 2021-07-16 | 辽宁省轻工科学研究院有限公司 | Preparation method of inner wall ceramic coating for pseudo spark switch |
| CN113121206B (en) * | 2019-12-30 | 2023-08-22 | 辽宁省轻工科学研究院有限公司 | Preparation method of inner wall ceramic coating for pseudo spark switch |
| CN112142498A (en) * | 2020-09-15 | 2020-12-29 | 上海富乐华半导体科技有限公司 | Backing plate for simultaneous sintering of copper foils on two sides of DBC substrate and preparation method thereof |
| CN115093209A (en) * | 2022-07-05 | 2022-09-23 | 江苏锡沂高新材料产业技术研究院有限公司 | Preparation method of high-strength high-stability multilayer composite structure fused quartz material |
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Application publication date: 20151223 |