CN115611642B - SiC whisker with BN coating on surface and molten salt method preparation method thereof - Google Patents
SiC whisker with BN coating on surface and molten salt method preparation method thereof Download PDFInfo
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Abstract
The invention discloses a SiC whisker with a BN coating on the surface and a molten salt method preparation method thereof, which comprise the following steps: fully mixing molten salt, a BN generating reactant and SiC whiskers according to a certain proportion to obtain uniformly mixed powder; heating and sintering the uniformly mixed powder to fully react to obtain SiC whiskers coated with the BN coating of the mixed molten salt, washing the SiC whiskers coated with the BN coating of the mixed molten salt with water, and washing off the molten salt attached to the surface to obtain the SiC whiskers coated with the BN coating; and finally, drying the powder obtained by suction filtration to obtain the SiC whisker with the BN coating on the surface. The method is suitable for preparing the surface BN coatings such as SiC whiskers, chopped fibers and the like, and the obtained SiC whiskers coated with the flaky BN can be used for reinforcing and toughening the SiC-based composite material.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a SiC whisker with a BN coating on the surface and a molten salt method preparation method thereof.
Background
With the development of science and technology, researchers have developed a lot of researches on composite materials.
The ceramic matrix composite is widely applied to the aerospace field due to excellent high temperature resistance, corrosion resistance, wear resistance and other properties. Among them, the SiC whisker has high strength, high modulus, high temperature resistance and other properties and is widely used as a reinforcing material for ceramic matrix composites. However, during the high-temperature sintering process, the chopped fibers or whiskers easily form interface bonding with the ceramic matrix, so that the composite material may exhibit poor mechanical properties. The interfacial layer is necessary to adjust the interfacial bond strength between the reinforcement and the matrix, to deflect matrix cracks at the interface, which can transfer loads from the matrix to the reinforcement.
The BN coating has the following advantages as a coating capable of improving the performance of the SiC whisker:
1. the oxidation resistance is good. Compared with PyC, the BN interface coating has better oxidation resistance, chemical stability is kept in a medium temperature area (800 ℃), and the BN interface coating has self-lubricating performance at high temperature.
2. The toughening effect is better. BN is used as a reinforcement and can be oxidized to generate B under the high-temperature condition 2 O 3 From BN to B 2 O 3 The volume is slightly expanded, so that on one hand, the crack can be filled; on the other hand, B 2 O 3 The cracks are sealed and prevented from further propagation, and the fracture toughness of the composite material can be enhanced.
3. The chemical resistance is strong.
Currently, there are two main methods for preparing BN coatings, namely CVD method and impregnation cracking method. However, the deposition process of the BN coating in the prior art still has the following defects: the CVD method for preparing the coating is mainly used for deposition on SiC fibers and is less applied to SiC whiskers. The CVD method for preparing the coating has high requirements on conditions such as the proportion of mixed gas, deposition time, pressure and the like, and the deposition speed can influence the uniform formation of the coating. Although the preparation process of the precursor impregnation cracking method is simple, the generated coating has more defects, and the preparation process of the impregnation cracking method has certain damage to the original reinforcement. Compared with the former two methods, the method for preparing the BN coating on the SiC whisker by using the molten salt method has the advantages of low cost, high efficiency and the like, the difficulty is in controlling the coating degree of the coating due to the sheet structure of the BN coating, but the coating condition of the coating can be controlled by controlling the mass ratio of the molten salt, the reactant and the SiC whisker and the heat preservation time, and simultaneously, the change of the temperature can influence the crystallinity of the BN, the temperature is increased, the crystallinity of the BN is increased, and the generated BN can be better attached to the SiC whisker.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the SiC whisker with the BN coating on the surface and the molten salt method for preparing the same.
The technical scheme includes that the SiC whisker with the BN coating on the surface is provided, the BN coating is formed on the surface of the SiC whisker through a molten salt method, the BN coating is uniformly distributed on the surface of the SiC whisker in a scaly shape, the BN of the BN coating is a hexagonal boron nitride structure (h-BN), and the thickness of the BN coating is within the range of 10 to 50nm.
The invention also provides a molten salt method for preparing the SiC whisker with the BN coating on the surface, which comprises the following steps:
1. powder mixing: ball-milling and mixing molten salt, a BN-generating reactant and SiC whiskers according to a certain proportion to obtain uniformly mixed powder;
2. sintering treatment: heating and sintering the uniformly mixed powder obtained in the step one to fully react to obtain SiC whiskers coated with the BN coating of the mixed molten salt;
3. and (3) suction filtration treatment: washing the SiC whiskers coated with the BN coating of the mixed molten salt obtained in the second step with water, and washing off the molten salt attached to the surface to obtain the SiC whiskers coated with the BN coating;
4. drying treatment: and D, drying the SiC whisker with the BN coating on the surface obtained in the step three to obtain the SiC whisker with the BN coating on the surface.
Further, in the first step, the molten salt is sodium chloride and potassium chloride, and the reactants for generating BN are melamine and borax.
Further, in the first step: the molar ratio of nitrogen elements in the melamine to boron elements in the borax is (1) - (4; the mass ratio of the sodium chloride to the potassium chloride is 11; the mass ratio of the BN-forming reactant to the molten salt is (1); the mass ratio of the total mass of the reactants and the molten salt to the SiC whiskers is (5) - (1) (10.
Further, the operation method of the temperature-raising sintering treatment in the second step comprises: heating the uniformly mixed powder to 900-1200 ℃ under nitrogen atmosphere at a heating rate of 3-5 ℃/min, preserving heat for 1-4 hours, and then cooling to room temperature under nitrogen atmosphere, wherein the equipment adopted for heating and sintering treatment is a vacuum cracking furnace.
Further, the operation method of the suction filtration treatment in the third step is as follows: and (3) putting the product obtained in the second step into deionized water, uniformly mixing, then filtering out liquid by using a suction filtration device, and repeating for 4-5 times.
Further, the drying temperature in the fourth step is 80-90 ℃.
Compared with the prior art, the invention has the advantages that:
1. the invention provides the silicon carbide whisker with the surface interface layer BN, and the uniformly distributed BN layer can improve the physical and chemical properties of the silicon carbide whisker and expand the application field of the silicon carbide whisker.
2. The BN coating on the surface of the silicon carbide whisker is scaly microscopically, and is different from a uniformly paved BN coating prepared on SiC fibers in the prior art, hexagonal BN is scaly, whiskers which are not treated by the BN coating can be combined with powder in the sintering process to lose the original reinforcing and toughening effect, and after the BN coating is prepared on the surfaces of the whiskers, cracks can deflect when encountering the coating when the composite material is subjected to an external force, so that the reinforcement is enhanced, and the SiC whiskers attached with the scaly BN coating can enrich the application of the SiC whiskers in the field of reinforcing and toughening of ceramic matrix composite materials.
3. In the preparation method, the crystallinity and the grain size of the generated h-BN are controlled by regulating the rate and the temperature range of temperature-rising sintering, the temperature range of the method can ensure that the crystal grains of the BN grow to a certain extent, and simultaneously the crystallinity is optimally controlled, so that the more the scale-shaped BN is generated, the sintering at the temperature lower than 900 ℃ is not beneficial to the crystallization of the BN coating, and the sintering at the temperature higher than 1200 ℃ can cause the crystal grains of the generated BN coating to grow too large, so that the BN layer loses the burr sense of scales.
4. The BN coating is prepared by a molten salt method, salt in a product can be cleaned by deionized water, and the conversion rate of the product is higher.
Drawings
These and/or other aspects and advantages of the present invention will become more apparent and more readily appreciated from the following detailed description of the embodiments of the invention, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic flow chart of the preparation method of the present invention;
FIG. 2 is an SEM picture of a BN coated SiC whisker prepared in example 1 of the invention;
FIG. 3 is an SEM picture of a BN coating coated SiC whisker prepared in example 2 of the invention;
FIG. 4 is a comparative XRD pattern of BN coated SiC whiskers produced in examples 1 and 2 of the invention;
FIG. 5 is an SEM picture of a SiC whisker coated with a BN coating prepared in example 3 of the invention;
FIG. 6 is an SEM picture of a BN coated SiC whisker prepared in example 4 of the invention;
figure 7 is a comparative XRD pattern of BN coated SiC whiskers prepared in examples 4 and 5 of the invention.
Detailed Description
In order that those skilled in the art will better understand the present invention, the following detailed description of the invention is provided in conjunction with the accompanying drawings and the detailed description of the invention.
Example 1:
in this embodiment, the flow of the method for preparing a BN coating on the surface of a SiC whisker is shown in fig. 1, and the method is performed according to the following steps:
1. powder mixing: taking 4g of beta-SiC whiskers with the length of about 20-40 mu m and the diameter of 50-200nm; 10g of fused salt (4.4 g of sodium chloride and 5.6g of potassium chloride); a total of 10g of BN-forming reactants (the mass ratio of B to N was 1).
2. Sintering treatment: sintering the powder uniformly mixed in the first step, wherein the sintering equipment is a vacuum cracking furnace, and the sintering process conditions are as follows: and under the condition of nitrogen atmosphere, heating to 900 ℃ at the speed of 5 ℃/min, preserving heat for 3 hours, and keeping the nitrogen atmosphere to cool along with the furnace to obtain the molten salt coated SiC whisker with the BN coating on the surface.
3. And (3) suction filtration treatment: washing the SiC whiskers coated with the BN coating mixed with the molten salt and obtained in the second step with deionized water, and performing suction filtration for 4 times to wash off the salt attached to the surface, so as to obtain the SiC whiskers coated with the BN coating;
4. drying treatment: and (4) drying the powder obtained in the step three in an oven at the temperature of 85 ℃ to obtain the final SiC whisker with the BN coating attached to the surface.
Example 2:
in this example, the method for preparing a BN coating on the surface of a SiC whisker is performed according to the following steps:
1. powder mixing:
taking 4g of beta-SiC whiskers with the length of about 20-40 mu m and the diameter of 50-200nm; 10g of fused salt (4.4 g of sodium chloride and 5.6g of potassium chloride); the total amount of BN-forming reactants was 10g (the mass ratio of B to N was 1.
2. Sintering treatment:
sintering the powder uniformly mixed in the step one, wherein the sintering equipment is a vacuum cracking furnace, and the sintering process conditions are as follows: and under the condition of nitrogen atmosphere, heating to 1200 ℃ at the speed of 5 ℃/min, preserving heat for 3 hours, and keeping the nitrogen atmosphere to cool along with the furnace to obtain the SiC whisker coated with the molten salt and provided with the BN coating on the surface.
3. And (3) suction filtration treatment: washing the SiC whiskers mixed with the molten salt and coated with the BN coating for 4 times by using deionized water, and leaching to remove the salt attached to the surface to obtain the SiC whiskers with the BN coating attached to the surface;
4. drying treatment: and (4) drying the powder obtained in the step three in an oven at the temperature of 85 ℃ to obtain the final SiC whisker with the BN coating attached to the surface.
SEM images of example 1 and example 2 are shown in fig. 1 and 2, and it can be seen that BN coating was generated on the surface of SiC whisker under 900 ℃ and 1200 ℃. Compared with the BN coating produced at 900 ℃ and 1200 ℃, the flaky BN coating is more uniform, the burr feeling is heavier, and the BN coating is favorably generated by raising the temperature. From the XRD images of both of FIG. 3, it can be seen that the BN produced is h-BN, and the higher the temperature is, the better the crystallinity of BN, and the more prominent the diffraction peak of BN.
Example 3:
in this example, the method for preparing a BN coating on the surface of a SiC whisker comprises the following steps:
1. powder mixing: taking 3.33g of beta-SiC whiskers with the length of about 20-40 mu m and the diameter of 50-200nm and 10g of fused salt (4.4 g of sodium chloride and 5.6g of potassium chloride); the total amount of BN-forming reactants was 10g (the mass ratio of B to N was 1.
2. Sintering treatment: sintering the powder uniformly mixed in the step one, wherein the sintering equipment is a vacuum cracking furnace, and the sintering process conditions are as follows: and under the condition of nitrogen atmosphere, heating to 1200 ℃ at the speed of 5 ℃/min, preserving heat for 1 hour, and keeping the nitrogen atmosphere to cool along with the furnace to obtain the SiC whisker coated with molten salt and having a BN coating on the surface.
3. And (3) suction filtration treatment: washing the SiC whiskers coated with the BN coating mixed with the molten salt and obtained in the second step with deionized water, and performing suction filtration for 4 times to wash off the salt attached to the surface, so as to obtain the SiC whiskers coated with the BN coating;
4. drying treatment: and (4) drying the powder obtained in the step three in an oven at the temperature of 85 ℃ to obtain the final SiC whisker with the BN coating attached to the surface.
Example 4:
in this example, the method for preparing a BN coating on the surface of a SiC whisker comprises the following steps:
powder mixing: taking 3.33g of beta-SiC whiskers with the length of about 20-40 mu m and the diameter of 50-200nm and 10g of fused salt (4.4 g of sodium chloride and 5.6g of potassium chloride); the total amount of reactants was 10g (the mass ratio of B to N was 1).
Sintering treatment: sintering the powder uniformly mixed in the first step, wherein the sintering equipment is a vacuum cracking furnace, and the sintering process conditions are as follows: and under the condition of nitrogen atmosphere, heating to 1200 ℃ at the speed of 5 ℃/min, preserving heat for 4 hours, and keeping the nitrogen atmosphere to cool along with the furnace to obtain the SiC whisker coated with molten salt and having a BN coating on the surface.
3. And (3) suction filtration treatment: washing the SiC whiskers mixed with the molten salt and coated with the BN coating for 4 times by using deionized water, and leaching to remove the salt attached to the surface to obtain the SiC whiskers with the BN coating attached to the surface;
4. drying treatment: and (4) drying the powder obtained in the step three in an oven at 85 ℃ to obtain the final SiC whisker with the BN coating attached to the surface.
The SEM images of examples 3 and 4 are shown in fig. 5 and 6, and it can be seen that the holding time mainly affects the growth of the crystal grains, and when the holding time is 1 hour, the crystal grains of the BN coating attached to the surface are small, and appear as small pieces, and the burr feeling on the whole surface of the SiC whisker is obvious; when the temperature is kept for 4 hours, BN crystal grains grow up remarkably, and the crystal grains grow up to cover the whole SiC crystal whisker, so that no burr feeling is displayed on the whole surface of the SiC crystal whisker. According to XRD patterns of the two materials in figure 7, h-BN is generated in the two materials, and a BN diffraction peak is more obvious after the two materials are kept for 4 hours.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (2)
1. A preparation method of SiC whiskers with BN coatings on the surfaces is characterized in that the BN coatings are formed on the surfaces of the SiC whiskers through a molten salt method, the BN coatings are uniformly distributed on the surfaces of the SiC whiskers in a scaly shape, the BN of the BN coatings is in a hexagonal boron nitride structure, and the thickness of the BN coatings is within the range of 10 to 50nm;
the method comprises the following steps:
1. powder mixing: ball-milling and mixing molten salt, a BN-generating reactant and SiC whiskers according to a certain proportion to obtain uniformly mixed powder;
2. sintering treatment: heating and sintering the uniformly mixed powder obtained in the step one to fully react to obtain SiC whiskers coated with the BN coating of the mixed molten salt;
3. and (3) suction filtration treatment: washing the SiC whiskers coated with the BN coating in the mixed molten salt obtained in the step two, and washing off the molten salt attached to the surface to obtain SiC whiskers coated with the BN coating;
4. drying treatment: drying the SiC crystal whisker with the BN coating on the surface obtained in the step three to obtain the SiC crystal whisker with the BN coating on the surface;
in the first step, the molten salt is sodium chloride and potassium chloride, and reactants for generating BN are melamine and borax;
the length of the SiC whisker is 20-40 μm, and the diameter is 50-200nm;
the molar ratio of nitrogen elements in the melamine to boron elements in the borax is (1) - (4;
the mass ratio of sodium chloride to potassium chloride is 11:14;
the mass ratio of the BN-forming reactant to the molten salt is (1);
the mass ratio of the total mass of the reactants and the molten salt to the SiC whiskers is (5) - (1) (10;
the operation method of the temperature-rising sintering treatment in the second step comprises the following steps: heating the uniformly mixed powder to 900-1200 ℃ at a heating rate of 3-5 ℃/min in a nitrogen atmosphere, preserving the heat for 1-4 hours, and then cooling to room temperature in the nitrogen atmosphere, wherein the equipment adopted for heating and sintering treatment is a vacuum cracking furnace.
2. A molten salt method of producing SiC whiskers having a BN coating layer on the surface thereof according to claim 1,
the operation method of the suction filtration treatment in the third step comprises the following steps: and (5) placing the product obtained in the second step into deionized water, uniformly mixing, then filtering out liquid by using a suction filtration device, and repeating for 4-5 times.
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| EP0356267A1 (en) * | 1988-06-27 | 1990-02-28 | Rhone-Poulenc Chimie | Material based on boron nitride, process of producing the same and use as reinforcing agent |
| JPH02252660A (en) * | 1989-03-24 | 1990-10-11 | Takeo Oki | Calcined compact of hardly calcinable powder, its abrasive grain and grindstone and production thereof |
| JPH04268079A (en) * | 1991-02-19 | 1992-09-24 | Nachi Fujikoshi Corp | Coated parts and production thereof |
| JP2000264741A (en) * | 1999-03-16 | 2000-09-26 | Japan Science & Technology Corp | Silicon carbide-base ceramic composite material and its product |
| CN112062567A (en) * | 2020-09-17 | 2020-12-11 | 中国科学院上海应用物理研究所 | Method for preparing zirconium-yttrium-doped barium cerate powder by using molten salt and powder obtained by method |
| FR3115785A1 (en) * | 2020-11-03 | 2022-05-06 | Safran Ceramics | Formation of metallic carbide on fibers by the molten salt method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR3115784B1 (en) * | 2020-11-03 | 2023-03-31 | Safran Ceram | Formation of boron nitride on fibers by the molten salt method |
| CN112521156B (en) * | 2021-02-18 | 2021-04-27 | 中国人民解放军国防科技大学 | Hybrid matrix SiCf/SiC composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5153000A (en) * | 1974-11-05 | 1976-05-11 | Sumitomo Chemical Co | Chitsukahososeni seikeibutsu oyobi fuirumuno seizoho |
| US4794044A (en) * | 1986-12-10 | 1988-12-27 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Method for surface treatment |
| EP0356267A1 (en) * | 1988-06-27 | 1990-02-28 | Rhone-Poulenc Chimie | Material based on boron nitride, process of producing the same and use as reinforcing agent |
| JPH02252660A (en) * | 1989-03-24 | 1990-10-11 | Takeo Oki | Calcined compact of hardly calcinable powder, its abrasive grain and grindstone and production thereof |
| JPH04268079A (en) * | 1991-02-19 | 1992-09-24 | Nachi Fujikoshi Corp | Coated parts and production thereof |
| JP2000264741A (en) * | 1999-03-16 | 2000-09-26 | Japan Science & Technology Corp | Silicon carbide-base ceramic composite material and its product |
| CN112062567A (en) * | 2020-09-17 | 2020-12-11 | 中国科学院上海应用物理研究所 | Method for preparing zirconium-yttrium-doped barium cerate powder by using molten salt and powder obtained by method |
| FR3115785A1 (en) * | 2020-11-03 | 2022-05-06 | Safran Ceramics | Formation of metallic carbide on fibers by the molten salt method |
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