CN105175025A - Silicon carbide fiber surface alumina-titanium oxide composite coating preparation method - Google Patents
Silicon carbide fiber surface alumina-titanium oxide composite coating preparation method Download PDFInfo
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- CN105175025A CN105175025A CN201510555077.XA CN201510555077A CN105175025A CN 105175025 A CN105175025 A CN 105175025A CN 201510555077 A CN201510555077 A CN 201510555077A CN 105175025 A CN105175025 A CN 105175025A
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Abstract
The present invention provides a silicon carbide fiber surface alumina-titanium oxide composite coating preparation method, wherein the components of the oxide coating comprise alumina and titanium oxide. The specific preparation method comprises: carrying out a mixing heating reflux reaction on an organic alcohol compound of aluminum, an organic alcohol compound of titanium and deionized water according to a certain ratio, adding hot lactic acid or acetic acid to the solution, carrying out a constant temperature reaction to obtain a transparent sol, placing the sol in a sealed container, carrying out thermal insulation for a certain time, placing cleaned silicon carbide fibers in the gel to complete immersing coating, and carrying out thermal insulation on the obtained sample for a certain time at a high temperature so as to prepare the oxide coating on the silicon carbide fiber surface. According to the present invention, the prepared oxide coating is compact and uniform, combines the performance advantages of alumina and titanium oxide, and can be widely used in the technical fields of anti-oxidation, corrosion resistance, heat resistance, gas permeation resistance, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of oxide coating, particularly relate to a kind of preparation method at silicon carbide fiber surface alumina oxide-titanium oxide composite coating.
Background technology
Silicon carbide fiber is that a kind of intensity is large, modulus is high, high temperature resistant, radioprotective, creep resisting high-performance ceramic fiber, is widely used in the high-tech sectors such as aerospace, weaponry and nuclear industry.Silicon carbide fiber has certain oxidation-resistance, but also oxidative phenomena can occur after life-time service in high temperature environments, and the mode preparing oxide ceramics on its surface usually can be adopted to improve its oxidation-resistance.At present, the mode preparing oxide ceramic coating has a lot, is directed to different body materials and can selects different preparation methods.
Application publication number is that the Chinese invention patent of CN102491639A discloses a kind of nanometer aluminum oxide composite ceramic coating layer and preparation method thereof, coating is prepared by heat spraying method, and spray finishing material is mixed by aluminum oxide, zirconium white and rare earth oxide to melt through cooling the glass particle formed rapidly.Preparation method is: preparation mixing fine powders material, is directly injected in normal-temperature water purification by fine powder material after waiting thermic lance melting, then dries to sieve and obtain alumina base glass particle, and ceramic coating is prepared in last thermospray.The coating of this invention is the nanostructure be evenly distributed, and has excellent mechanical property.But this invention is compared and is applicable to metallic matrix, is not too applicable to silicon carbide fiber matrix.
Application publication number is the preparation method that the Chinese invention patent of CN104213099A discloses a kind of silicon carbide fiber oxide on surface ceramic coating, comprises the following steps: silicon carbide fiber removes photoresist, cleans by (1); (2) put into ALD reaction chamber, repeatedly vacuumize, displacement nitrogen three times; (3) according to the type of deposition oxide coating, selective reaction presoma, parameters; (4) carry at nitrogen or argon gas and lower precursor vapor is incorporated in ALD reaction chamber; (5) with nitrogen or argon purge reaction chamber; (6) carry at nitrogen or argon gas and lower oxygen source steam is incorporated in ALD reaction chamber; (7) with nitrogen or argon purge reaction chamber; (8) repeating step (4)-step (7), until the required coat-thickness of deposition; (9) high temperature process furnances is put into, heat-treat under nitrogen protection.Oxide ceramic coating prepared by this invention evenly, fine and close, impurity is few and thickness can accurately control.But the operation steps of this invention is very loaded down with trivial details, the requirement for equipment is very high, and manufacturing cost is very large, is unfavorable for promoting the use of on a large scale.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, provides a kind of preparation method at silicon carbide fiber surface alumina oxide-titanium oxide composite coating.
The technical scheme adopted for realizing object of the present invention is: provide a kind of silicon carbide fiber oxide on surface coating, it is characterized in that the thickness of described oxide coating is 1 ~ 10 μm, the component of described oxide coating comprises aluminum oxide and titanium oxide.
Present invention also offers a kind of preparation method of silicon carbide fiber oxide on surface coating, it is characterized in that realizing according to the following step:
(1) the proportionally organic alcohol compound of aluminum mixture and the organic alcohol compound of titanium, then pour in appropriate deionized water, obtain mixing solutions, then by mixing solutions churned mechanically while in the thermostat water bath of 75 ~ 100 DEG C reflux 10 ~ 20 hours;
(2) in the mixing solutions after above-mentioned heating, add appropriate lactic acid or acetum, after stirring, isothermal reaction 2 ~ 5 hours between 50 ~ 100 DEG C, obtains vitreosol;
(3) colloidal sol prepared above is placed in sealed vessel, reserves the space of at least 30%, reheat to 150 ~ 250 DEG C of insulations 5 ~ 15 hours;
(4) colloidal sol after insulation is taken out, silicon carbide fiber bundle through removing photoresist, after ultrasonic cleaning or fibrage body to be immersed in colloidal sol 5 minutes, then from colloidal sol, silicon carbide fiber cloth or fibrage body is taken out, put and dry in atmosphere, complete single-steeping, repeat above-mentioned steeping process 20 ~ 30 times, complete sol impregnation coating;
(5) sample that said process obtains is put in an oven, with ramp to 700 ~ 1000 DEG C of 5 ~ 15 DEG C/min, be incubated after 2 ~ 5 hours and take out, the oxide coating on final obtained silicon carbide fiber surface.
Wherein, the organic alcohol compound of aluminium, the organic alcohol compound of titanium, the proportioning of deionized water are (1 ~ 5g) in step (1): (0.1 ~ 1g): (10 ~ 50ml).
Wherein, the concentration of lactic acid or acetum is 0.5 ~ 2mol/L in step (2), and the volume of lactic acid or acetum accounts for 5% ~ 20% of ionized water.
Effect: the present invention compared with prior art, has the following advantages: (1) preparation technology is simple, lower to the requirement of equipment, cost is lower, is applicable to large-scale promotion and uses; (2) the oxide coating dense uniform prepared of the present invention, combines the feature performance benefit of aluminum oxide and titanium oxide, can be widely used in the technical fields such as anti-oxidant, protection against corrosion, solar heat protection, gas barrier; (3) titanium dioxide has bibulous feature, can improve the infiltration of oxide slurry in fibrous bundle, increases the densification rate of silicon carbide fiber cloth; (4) titanium dioxide is material the whitest in the world, can change the color that silicon carbide fiber strengthens ceramic matric composite.
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) add after 40g aluminum isopropylate, the mixing of 8g titanium isopropylate in 400ml deionized water, obtain mixing solutions, then by mixing solutions churned mechanically while in the thermostat water bath of 80 DEG C reflux 15 hours; (2) in the mixing solutions after above-mentioned heating, add the lactic acid solution that 40ml concentration is 1mol/L, after stirring, isothermal reaction 3 hours between 70 DEG C, obtains vitreosol; (3) colloidal sol prepared above is placed in sealed vessel, reserves the space of at least 30%, reheat to 200 DEG C of insulations 8 hours; (4) take out the colloidal sol after insulation, the silicon carbide fiber bundle through removing photoresist, after ultrasonic cleaning to be immersed in colloidal sol 5 minutes, then from colloidal sol, to take out silicon carbide fiber cloth, put and dry in atmosphere, complete single-steeping, repeat above-mentioned steeping process 20 times, complete sol impregnation coating; (5) sample that said process obtains is put in an oven, with the ramp to 800 DEG C of 10 DEG C/min, be incubated after 3 hours and take out, the oxide coating on final obtained silicon carbide fiber surface.
embodiment 2
(1) add after 80g isobutanol aluminum, the mixing of 16g titanium isobutoxide in 800ml deionized water, obtain mixing solutions, then by mixing solutions churned mechanically while in the thermostat water bath of 90 DEG C reflux 18 hours; (2) in the mixing solutions after above-mentioned heating, add the lactic acid solution that 80ml concentration is 1mol/L, after stirring, isothermal reaction 3 hours between 90 DEG C, obtains vitreosol; (3) colloidal sol prepared above is placed in sealed vessel, reserves the space of at least 30%, reheat to 200 DEG C of insulations 12 hours; (4) colloidal sol after insulation is taken out, silicon carbide fiber knitted body through removing photoresist, after ultrasonic cleaning to be immersed in colloidal sol 5 minutes, then from colloidal sol, silicon carbide fiber knitted body is taken out, put and dry in atmosphere, complete single-steeping, repeat above-mentioned steeping process 25 times, complete sol impregnation coating; (5) sample that said process obtains is put in an oven, with the ramp to 900 DEG C of 10 DEG C/min, be incubated after 4 hours and take out, the oxide coating on final obtained silicon carbide fiber surface.
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., in a preparation method for silicon carbide fiber surface alumina oxide-titanium oxide composite coating, the thickness of this oxide coating is 1 ~ 10 μm, and component comprises aluminum oxide and titanium oxide, it is characterized in that comprising following operation steps:
(1) the proportionally organic alcohol compound of aluminum mixture and the organic alcohol compound of titanium, then pour in appropriate deionized water, obtain mixing solutions, again by mixing solutions churned mechanically while in the thermostat water bath of 75 ~ 100 DEG C reflux 10 ~ 20 hours, the proportioning of the organic alcohol compound of aluminium, the organic alcohol compound of titanium, deionized water is (1 ~ 5g): (0.1 ~ 1g): (10 ~ 50ml);
(2) in the mixing solutions after above-mentioned heating, appropriate lactic acid or acetum is added, isothermal reaction 2 ~ 5 hours between 50 ~ 100 DEG C after stirring, obtain vitreosol, the concentration of lactic acid or acetum is 0.5 ~ 2mol/L, and the volume of lactic acid or acetum accounts for 5% ~ 20% of ionized water;
(3) colloidal sol prepared above is placed in sealed vessel, reserves the space of at least 30%, reheat to 150 ~ 250 DEG C of insulations 5 ~ 15 hours;
(4) colloidal sol after insulation is taken out, silicon carbide fiber bundle through removing photoresist, after ultrasonic cleaning or fibrage body to be immersed in colloidal sol 5 minutes, then from colloidal sol, silicon carbide fiber cloth or fibrage body is taken out, put and dry in atmosphere, complete single-steeping, repeat above-mentioned steeping process 20 ~ 30 times, complete sol impregnation coating;
(5) sample that said process obtains is put in an oven, with ramp to 700 ~ 1000 DEG C of 5 ~ 15 DEG C/min, be incubated after 2 ~ 5 hours and take out, the oxide coating on final obtained silicon carbide fiber surface.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109077620A (en) * | 2017-06-14 | 2018-12-25 | 佛山市顺德区美的电热电器制造有限公司 | Non-sticking lining and preparation method thereof and cookware or baking tray panel and equipment of cooking |
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| CN100999624A (en) * | 2007-01-05 | 2007-07-18 | 福州大学 | Compounding of inorganic anti-pollution coating for high pressure insulator surface and preparation process thereof |
| CN101550030A (en) * | 2009-05-12 | 2009-10-07 | 东北大学 | Method for preparing Al2O3 ceramic film on surface of 3D-SiC |
| CN101791524A (en) * | 2010-03-26 | 2010-08-04 | 南京工业大学 | Asymmetrically-structural ceramic ultrafiltration membrane and preparation method thereof |
| CN102557670A (en) * | 2010-12-24 | 2012-07-11 | 中国科学院兰州化学物理研究所 | Preparation method of aluminum oxide and titanium oxide compound nanometer powder body |
| CN103757618A (en) * | 2014-01-08 | 2014-04-30 | 同济大学 | Preparation method of antireflection film applicable to different bases |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999624A (en) * | 2007-01-05 | 2007-07-18 | 福州大学 | Compounding of inorganic anti-pollution coating for high pressure insulator surface and preparation process thereof |
| CN101550030A (en) * | 2009-05-12 | 2009-10-07 | 东北大学 | Method for preparing Al2O3 ceramic film on surface of 3D-SiC |
| CN101791524A (en) * | 2010-03-26 | 2010-08-04 | 南京工业大学 | Asymmetrically-structural ceramic ultrafiltration membrane and preparation method thereof |
| CN102557670A (en) * | 2010-12-24 | 2012-07-11 | 中国科学院兰州化学物理研究所 | Preparation method of aluminum oxide and titanium oxide compound nanometer powder body |
| CN103757618A (en) * | 2014-01-08 | 2014-04-30 | 同济大学 | Preparation method of antireflection film applicable to different bases |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109077620A (en) * | 2017-06-14 | 2018-12-25 | 佛山市顺德区美的电热电器制造有限公司 | Non-sticking lining and preparation method thereof and cookware or baking tray panel and equipment of cooking |
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