CN112159234A - High-entropy ceramic powder and preparation method and application thereof - Google Patents
High-entropy ceramic powder and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of ceramic materials, and discloses high-entropy ceramic powder and a preparation method and application thereof. The method is to add Hf (NO)3)4、Zr(NO3)4、Ti(NO3)4、TaO(NO3)3、NbO(NO3)3Mixing with amorphous boron, adding absolute ethyl alcohol and a dispersing agent, adjusting the pH value to 9-10, stirring and heating at 70-90 ℃, then drying, grinding, carrying out heat treatment at 600-800 ℃ in a protective atmosphere, grinding, sieving, pressing into a blank, calcining at 1400-1600 ℃ in the protective atmosphere, grinding and sieving to obtain high-entropy ceramic powder; the molecular formula is (Hf)xZryTizTanNbm)B2X is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, m is more than or equal to 0 and less than or equal to 1, and x + y + z + n + m is equal to 1. The method is simpleThe method is mild in reaction, green and environment-friendly, and the powder is uniform and fine in particle size, so that the sintering of the high-entropy ceramic is facilitated.
Description
Technical Field
The invention belongs to the technical field of high-entropy ceramics, and particularly relates to high-entropy ceramic powder and a preparation method and application thereof.
Background
Ultrahigh-temperature ceramic boride ZrB2、TiB2、HfB2The material has good thermal stability and chemical stability, and attracts great attention of researchers, and becomes a candidate material in an extreme environment such as supersonic flight (at a temperature of 1400 ℃ or higher in the air), atmosphere reentry (at a temperature of 2000 ℃ or higher in an oxygen atom and nitrogen atom environment), rocket engine (at a temperature of 3000 ℃ or higher in a chemical reaction atmosphere), and the like. Because the melting points are above 3000 ℃, the alloy still has good strength and good thermal shock resistance at above 1200 ℃. Therefore, the composite material is hopeful to be applied to wing leading edges and other parts needing to be used in extreme environments. Researchers are now working on how to further improve their performance to accommodate applications in extreme environments. The prepared solid solution can effectively improve the performance of the material, and in recent years, due to the large entropy value of the high-entropy ceramic material, a plurality of dislocations exist in the system, thereby arousing the interest of researchers. The material has greatly improved performance, excellent properties of high hardness, high toughness, corrosion resistance and the like, and is a very promising material applied to the fields of aerospace, ultrahigh-speed reentry vehicles, nuclear reactors and the like.
At present, most of the powder materials are ball-milled and mixed by adopting a mechanical ball milling method to obtain high-entropy powder, the method has long time effect and high energy consumption, impurities are easily brought in the ball milling process, the quality of the powder is influenced, the subsequent preparation of high-entropy ceramics is also influenced, and the powder prepared by a related chemical method is not reported in the field of ultrahigh-temperature high-entropy ceramics.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the invention provides the preparation method of the high-entropy ceramic powder, which is simple and convenient in process, green and environment-friendly, short in aging, free of impurities and safe, reliable and optimized.
The invention also aims to provide the high-entropy ceramic powder prepared by the method.
The invention further aims to provide application of the high-entropy ceramic powder.
The purpose of the invention is realized by the following technical scheme:
a preparation method of high-entropy ceramic powder comprises the following specific steps:
s1, adding Hf (NO)3)4、Zr(NO3)4、Ti(NO3)4、TaO(NO3)3、NbO(NO3)3Mixing with amorphous boron, adding absolute ethyl alcohol and a dispersing agent, dropwise adding an alkali solution to adjust the pH value to 9-10, and heating at 70-90 ℃ under the stirring condition to obtain dry gel;
s2, drying, grinding, sieving, carrying out heat treatment at 600-800 ℃ in a protective atmosphere, sampling, grinding, sieving, and carrying out dry pressing to obtain a blank;
s3, calcining the green body at 1400-1600 ℃ in a protective atmosphere, and grinding and sieving to obtain high-entropy ceramic powder; the molecular formula of the high-entropy ceramic powder is (Hf)xZryTizTanNbm)B2X is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, m is more than or equal to 0 and less than or equal to 1, and x + y + z + n + m is equal to 1.
Preferably, the dispersant in step S1 is ammonium citrate or polyethylene glycol.
Preferably, the alkali solution in step S1 is ammonia water or sodium hydroxide.
Preferably, the Hf (NO) in step S13)4、Zr(NO3)4、Ti(NO3)4、TaO(NO3)3、NbO(NO3)3And the molar ratio of the total amount of amorphous boron, anhydrous ethanol and the dispersant is 1: (1.5-3): (0.5-2).
Preferably, the stirring speed in the step S1 is 800-1000 r/min, and the stirring time is 1-3 h.
Preferably, the heat treatment time in the step S2 is 1-3 h; the calcining time in the step S3 is 0.5-2 h.
Preferably, the protective atmosphere in steps S2 and S3 is vacuum, argon or nitrogen.
The high-entropy ceramic powder is prepared by the method.
Preferably, the particle size of the high-entropy ceramic powder is 50 nm-1 μm.
The high-entropy ceramic powder is applied to the field of ultra-high temperature limit.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts the mixed preparation of various metal salts (Hf)xZryTizTanNbm)B2The high-entropy powder has simple and convenient process, environmental protection and short time effect, and can not introduce impurities; the anhydrous ethanol treatment mode promotes the rapid crystallization of the product and reduces the particle size of the product.
2. The anhydrous ethanol treated powder is dried and calcined, so that the safety is high, the requirement on equipment is not high, the specific surface area of the high-entropy powder can be increased by adopting the anhydrous ethanol treatment and introducing the additive, and the preparation method is safe, reliable and optimized.
3. The high-entropy ceramic powder prepared by the method is uniform and fine in particle size, and is beneficial to subsequent sintering of high-entropy ceramic.
Drawings
FIG. 1 shows (Hf) obtained in example 10.2Zr0.2Ti0.2Ta0.2Nb0.2)B2XRD pattern of high entropy ceramic powder;
FIG. 2 shows (Hf) obtained in example 10.2Zr0.2Ti0.2Ta0.2Nb0.2)B2SEM photograph of high entropy ceramic powder.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
1. 9.86g Hf (NO)3)4、8.59g Zr(NO3)4、8.42g Ti(NO3)4、8.86g TaO(NO3)3、6.82gNbO(NO3)3Mixing with 5g of amorphous boron powder, adding into 8.6205g of absolute ethyl alcohol, then adding 0.19g of polyethylene glycol, dropwise adding ammonia water to adjust the pH value to 10, and magnetically stirring for 2 hours at 80 ℃ at 1000r/min to obtain xerogel;
2. filtering and washing the dried gel by absolute ethyl alcohol, grinding and sieving after vacuum drying, carrying out heat treatment for 2 hours at 650 ℃ under the vacuum condition, cooling along with a furnace, taking out a sample, grinding and sieving, pressing into a blank body by a tablet press with 2t of vertical drying,
3. calcining the green body at 1600 ℃ for 1h under vacuum condition, cooling along with the furnace, taking out, grinding and sieving to obtain (Hf)0.2Zr0.2Ti0.2Ta0.2Nb0.2)B2High entropy ceramic powder.
FIG. 1 shows (Hf) obtained in example 10.2Zr0.2Ti0.2Ta0.2Nb0.2)B2XRD pattern of high entropy ceramic powder. As is clear from FIG. 1, the powder obtained exhibited a diffraction peak of Hf-Zr-Ti-Ta-Nb-B solid solution. FIG. 2 shows (Hf) obtained in example 10.2Zr0.2Ti0.2Ta0.2Nb0.2)B2SEM photograph of high entropy ceramic powder. Calculated according to FIG. 2, (Hf)0.2Zr0.2Ti0.2Ta0.2Nb0.2)B2The average grain diameter of the high-entropy ceramic powder is 346 nm.
Example 2
1. 9.86g Hf (NO)3)4、8.59g Zr(NO3)4、8.42g Ti(NO3)4、8.86g TaO(NO3)3、6.82gNbO(NO3)3And 5g of amorphous boron powder are added into 8.6205g of absolute ethyl alcohol, 0.48g of ammonium citrate is added, ammonia water is added dropwise to adjust the pH value to 10, and magnetic stirring is carried out at 80 ℃ for 2h at 800r/min to obtain dry gel.
2. Filtering and washing the dried gel by absolute ethyl alcohol, grinding and sieving after vacuum drying, calcining for 2 hours at 650 ℃ under the vacuum condition, cooling along with a furnace, taking out a sample, grinding and sieving, pressing into a blank body by a tablet press with 2t of vertical drying,
3. the blank is put under vacuum conditionCalcining at 1500 ℃ for 1h, cooling with the furnace, taking out, grinding and sieving to obtain (Hf)0.2Zr0.2Ti0.2Ta0.2Nb0.2)B2The high-entropy ceramic powder has an average particle size of 286 nm.
Example 3
1. 9.86g Hf (NO)3)4、8.59g Zr(NO3)4、8.42g Ti(NO3)4、8.86g TaO(NO3)3、6.82gNbO(NO3)3And 5g of amorphous boron powder are added into 8.6205g of absolute ethyl alcohol, 0.28g of polyethylene glycol is added, ammonia water is added dropwise to adjust the pH value to 10, and the mixture is magnetically stirred for 2 hours at the temperature of 80 ℃ at the speed of 900r/min to obtain xerogel.
2. Adding absolute ethyl alcohol, filtering, washing, vacuum drying, grinding, sieving, performing heat treatment at 650 ℃ for 2h under vacuum condition, cooling with a furnace, taking out a sample, grinding, sieving, and pressing into a blank by a tablet press machine for 2 t;
3. calcining the green body at 1600 ℃ for 1h under vacuum condition, cooling along with the furnace, taking out, grinding and sieving to obtain (Hf)0.2Zr0.2Ti0.2Ta0.2Nb0.2)B2High entropy ceramic powder. The grain diameter of the high-entropy ceramic powder is 462 nm.
Example 4
1. 9.86g Hf (NO)3)4、8.59gZr(NO3)4、8.42gTi(NO3)4、8.86gTaO(NO3)3、6.82gNbO(NO3)3And 5g of amorphous boron powder are added into 8.6205g of absolute ethyl alcohol, 0.28g of polyethylene glycol is added, ammonia water is added dropwise to adjust the pH value to 10, and magnetic stirring is carried out at 80 ℃ for 2h at 1000r/min, so as to obtain xerogel.
2. Filtering and washing the dried gel by using absolute ethyl alcohol, grinding and sieving the dried gel after vacuum drying, carrying out heat treatment for 2 hours at 650 ℃ under the vacuum condition, cooling along with a furnace, taking out a sample, grinding and sieving the sample, and pressing the sample into a blank body by using a tabletting machine for 2t vertical drying;
3. calcining the green body at 1600 ℃ for 1h under the argon atmosphere, then cooling along with the furnace, taking out, grinding and sieving to obtain (Hf)0.2Zr0.2Ti0.2Ta0.2Nb0.2)B2The particle size of the high-entropy ceramic powder is 438 nm.
The invention adopts the mixed preparation of various metal salts (Hf)xZryTizTanNbm)B2The high-entropy powder has simple and convenient process, environmental protection and short time effect, and can not introduce impurities; the absolute ethyl alcohol treatment mode promotes the rapid crystallization of the product, reduces the particle size of the product, and is the high-entropy ceramic powder. The high-entropy ceramic powder is uniform and fine in particle size, and the particle size of the high-entropy ceramic powder is 50 nm-1 mu m, so that the high-entropy ceramic powder is beneficial to subsequent sintering of high-entropy ceramic.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The preparation method of the high-entropy ceramic powder is characterized by comprising the following specific steps of:
s1, adding Hf (NO)3)4、Zr(NO3)4、Ti(NO3)4、TaO(NO3)3、NbO(NO3)3Mixing with amorphous boron, adding absolute ethyl alcohol and a dispersing agent, dropwise adding an alkali solution to adjust the pH value to 9-10, stirring and heating at 70-90 ℃ to obtain dry gel;
s2, filtering and washing the dried gel by using absolute ethyl alcohol, drying, grinding and sieving, carrying out heat treatment at 600-800 ℃ in a protective atmosphere, sampling, grinding and sieving, and carrying out dry pressing to obtain a blank;
s3, calcining the green body at 1400-1600 ℃ in a protective atmosphere, and grinding and sieving to obtain high-entropy ceramic powder; the molecular formula of the high-entropy ceramic powder is (Hf)xZryTizTanNbm)B2X is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, m is more than or equal to 0 and less than or equal to 1, and x + y + z + n + m is equal to 1.
2. A method for preparing high-entropy ceramic powder according to claim 1, wherein the dispersant in step S1 is ammonium citrate or polyethylene glycol.
3. The method for preparing high-entropy ceramic powder of claim 1, wherein the alkali solution in step S1 is ammonia water or sodium hydroxide.
4. The method according to claim 1, wherein the Hf (NO) in step S1 is used for preparing the high-entropy ceramic powder3)4、Zr(NO3)4、Ti(NO3)4、TaO(NO3)3、NbO(NO3)3And the molar ratio of the total amount of amorphous boron, anhydrous ethanol and the dispersant is 1: (1.5-3): (0.5-2).
5. The preparation method of the high-entropy ceramic powder of claim 1, wherein the stirring speed in step S1 is 800-1000 r/min, and the stirring time is 1-3 h.
6. The preparation method of the high-entropy ceramic powder of claim 1, wherein the heat treatment time in step S2 is 1-3 hours; the calcining time in the step S3 is 0.5-2 h.
7. A method for preparing high-entropy ceramic powder according to claim 1, wherein the protective atmosphere in steps S2 and S3 is vacuum, argon, or nitrogen.
8. A high-entropy ceramic powder, characterized in that the high-entropy ceramic powder is prepared by the method of any one of claims 1 to 7.
9. A high-entropy ceramic powder according to claim 8, wherein the particle size of the high-entropy ceramic powder is 50nm to 1 μm.
10. The use of the high-entropy ceramic powder of claim 8 or 9 in the ultra-high temperature limit field.
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Cited By (3)
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| CN114988881A (en) * | 2021-03-02 | 2022-09-02 | 中国科学院化学研究所 | Boride high-entropy ceramic precursor, high-entropy ceramic and preparation method |
| CN115073183A (en) * | 2022-06-27 | 2022-09-20 | 山东大学 | High-entropy boride nano powder and sol-gel preparation method thereof |
| CN115772034A (en) * | 2023-02-13 | 2023-03-10 | 中国人民解放军国防科技大学 | High-entropy carbide ceramic precursor, high-entropy carbide ceramic and preparation method |
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| CN114988881A (en) * | 2021-03-02 | 2022-09-02 | 中国科学院化学研究所 | Boride high-entropy ceramic precursor, high-entropy ceramic and preparation method |
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| CN115073183B (en) * | 2022-06-27 | 2023-06-13 | 山东大学 | High-entropy boride nano powder and sol-gel preparation method thereof |
| CN115772034A (en) * | 2023-02-13 | 2023-03-10 | 中国人民解放军国防科技大学 | High-entropy carbide ceramic precursor, high-entropy carbide ceramic and preparation method |
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