CN112028635A - Ultrahigh-temperature ceramic composite material and preparation method thereof - Google Patents
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Abstract
The invention relates to an ultrahigh-temperature ceramic composite material and a preparation method thereof, in particular to (Hf)0.25Ta0.25Zr0.25Ti0.25)B2The preparation method of the-SiC-Si composite material comprises the steps of firstly preparing (Hf) by taking transition metal oxide and boron powder as raw materials through a boron thermal reaction0.25Ta0.25Zr0.25Ti0.25)B2Ceramic powder, the powder is smaller than boride sold in the market, the purity is high and the components are uniform; SiC is introduced as an additive, so that the sintering of the high-entropy ceramic is promoted, the sintering temperature is reduced, and the growth of crystal grains is inhibited; the gas phase siliconizing process can effectively fill the defects of pores and the like in the ceramic through the infiltration of Si vapor, and finally, the high-density (Hf) can be quickly formed0.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si composite material.
Description
Technical Field
The invention belongs to an ultrahigh-temperature ceramic composite material and a preparation method thereof, and relates to a gas-phase siliconizing method for preparing (Hf)0.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si composite material.
Background
Ultra-high temperature ceramics (UHTCs) generally refer to a special class of ceramic materials that have melting points in excess of 3000 ℃ and maintain stable physical and chemical properties in extreme environments. In the large family of ultra-high temperature ceramics, transition metal borides, especially ZrB2、HfB2、TiB2、TaB2Has relatively excellent comprehensive performance, such as high melting point, high strength, high hardness, high heat conductivity and electric conductivity, excellent chemical stability, thermal shock resistance and the like. However, the above transition metal boride is bonded by a strong covalent bond, and the corresponding ceramic is difficult to be sintered and densified, and further, the fracture toughness is low and the oxidation resistance is poor. Therefore, how to improve the compactness, fracture toughness and oxidation resistance of the transition metal boride ceramic becomes a hot research in recent years.
Currently, there are two main ways to solve the above problems: 1. introducing into the boride an amount of a silicide such as SiC [ V.Guerrineau, A.Julian-Jankowia, Oxidation mechanisms under water vapor conditions of ZrB2-SiC and HfB2-SiC based materials up to 2400℃.Journal of the European Ceramic Society 38(2018)421-432]，MoSi2[L.Silvestroni,K.Stricker,D.Sciti,H.Kleebe,Understanding the oxidation behavior of a ZrB2-MoSi2composite at ultra-high temperatures.Acta Materialia 151(2018)216-228]. 2. Based on the minimization of Gibbs free energy (G ═ H-TS, where H is enthalpy, S is entropy, and T is temperature), the entropy of the material is increased, and thus the material is thermodynamically more stable (particularly, the material is thermodynamically more stable)Which is at high temperature), and then high entropy boride ceramic materials have been developed. For example (Hf)0.2Zr0.2Ta0.2Nb0.2Ti0.2)B2,(Hf0.2Zr0.2Ta0.2Mo0.2Ti0.2)B2,(Hf0.2Zr0.2Mo0.2Nb0.2Ti0.2)B2,(Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2,(Mo0.2Zr0.2Ta0.2Nb0.2Ti0.2)B2,(Hf0.2Zr0.2Ta0.2Cr0.2Ti0.2)B2[J.Gild,Y.Y.Zhang,T.Harrington,S.C.Jiang,T.Hu,M.C.Quinn,W.M.Mellor,N.X.Zhou,K.Vecchio,J.Luo,High-Entropy Metal Diborides:A New Class of High-Entropy Materials and a New Type of Ultrahigh Temperature Ceramics.Scientific Reports.6(1)(2016)37946-37956.]. Preliminary research shows that the hardness and the oxidation resistance of the high-entropy ceramic prepared by the same process are superior to those of single-phase boride ceramic prepared by the same process.
Due to the high melting point and strong covalent bonding of the ultra-high temperature ceramics, special ceramic preparation processes, such as Spark Plasma Sintering (SPS), are often required, which have high requirements on equipment and high cost. Even so, the density of the prepared high-entropy pottery is about 92%, and the high-entropy pottery still has a promotion space. In addition, the research on the high-entropy ceramics is not deep enough, and the evaluation on the mechanical properties of the ceramics is less. Based on this, the high-entropy ceramic with high density and good mechanical property is prepared by adopting a low-cost process, and the method has important significance.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides an ultrahigh-temperature ceramic composite material and a preparation method thereof, wherein the (Hf) is prepared by adopting a boron thermal reduction method0.25Ta0.25Zr0.25Ti0.25)B2Ceramic powder, then evenly mixed with SiC and prepared by compression molding (Hf)0.25Ta0.25Zr0.25Ti0.25)B2-SiC green compact, finally prepared by the gas phase siliconizing process (Hf)0.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si composite material.
Technical scheme
An ultrahigh-temperature ceramic composite material is characterized in that the molecular formula is as follows: (Hf)0.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si。
Preparing the (Hf) by a gas phase siliconizing method0.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si composite material, characterized by the following steps:
step 1: mixing TiO with the molar ratio of 1:1:1:12Powder, ZrO2Powder, HfO2Powder and Ta2O5Powder and boron powder as raw materials, ethanol as solvent, ZrO2Ball milling is carried out on a planetary ball mill by using balls as a ball milling medium to obtain uniformly mixed powder A; the molar ratio of the total amount of the four oxides to the boron powder is 1: 4-5;
step 2: transferring the mixed powder A into a graphite crucible, and placing the graphite crucible into a high-temperature atmosphere sintering furnace for heat treatment in an argon atmosphere to obtain a product B; the heat treatment system comprises the following steps: temperature is 1973-2173K, processing time is 1-2 h, and heating rate is 5-10K/min;
and step 3: uniformly mixing the obtained product B and SiC powder in an agate mortar according to the volume ratio of 4-9: 1 to obtain mixture powder C;
and 4, step 4: adding the powder C into a mold, and molding under the mold pressing pressure of 8-12 Mpa to obtain a green body D;
and 5: weighing a certain amount of silicon blocks, placing the silicon blocks into a graphite crucible with a porous graphite plate, placing a green compact D on the porous graphite plate, sealing the graphite crucible, placing the graphite crucible into a high-temperature atmosphere sintering furnace for gas-phase siliconizing under the argon atmosphere, wherein the temperature is 2073-2273K, the processing time is 10-20 min, and the heating rate is 5-10K/min to obtain (Hf)0.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si composite material.
The ball milling time in the step 1 is 6-12 h.
Advantageous effects
The invention provides an ultrahigh-temperature ceramic composite material and a preparation method thereof, and particularly relates to (Hf)0.25Ta0.25Zr0.25Ti0.25)B2The preparation method of the-SiC-Si composite material comprises the steps of firstly preparing (Hf) by taking transition metal oxide and boron powder as raw materials through a boron thermal reaction0.25Ta0.25Zr0.25Ti0.25)B2Ceramic powder, the powder is smaller than boride sold in the market, the purity is high and the components are uniform; SiC is introduced as an additive, so that the sintering of the high-entropy ceramic is promoted, the sintering temperature is reduced, and the growth of crystal grains is inhibited; the gas phase siliconizing process can effectively fill the defects of pores and the like in the ceramic through the infiltration of Si vapor, and finally, the high-density (Hf) can be quickly formed0.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si composite material.
Drawings
FIG. 1 is (Hf) synthesized in example 10.25Ta0.25Zr0.25Ti0.25)B2XRD pattern of powder.
FIG. 2 is (Hf) synthesized in example 10.25Ta0.25Zr0.25Ti0.25)B2SEM photograph of the powder.
FIG. 3 is (Hf) prepared in example 10.25Ta0.25Zr0.25Ti0.25)B2XRD pattern of-SiC-Si composite material.
FIG. 4 is (Hf) prepared in example 10.25Ta0.25Zr0.25Ti0.25)B2SEM photograph of SiC-Si.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1:
(1) weighing a certain amount of TiO according to the molar ratio of 1:1:1:12Powder, ZrO2Powder, HfO2Powder, Ta2O5Powder, and then the total amount of the four oxides and B (boron) powderThe molar ratio is 1: 4 weighing B powder as raw material, ethanol as solvent and ZrO2Ball milling is carried out on a planetary ball mill for 8 hours by using balls as ball milling media to obtain uniformly mixed powder A;
(2) transferring the mixed powder A into a graphite crucible, and placing the graphite crucible into a high-temperature atmosphere sintering furnace for heat treatment in an argon atmosphere, wherein the heat treatment system is as follows: the temperature is 1973K, the processing time is 2h, and the heating rate is 5K/min, so that a product B is obtained;
(3) and mixing the obtained product B with SiC powder in a volume ratio of 4: 1 in an agate mortar to obtain mixture powder C;
(4) adding the powder C into a die for compression molding, wherein the pressure is 10Mpa, and obtaining a green body D;
(5) weighing a certain amount of silicon blocks, placing the silicon blocks in a graphite crucible with a porous graphite plate, placing a green body D on the porous graphite plate, sealing the graphite crucible, placing the graphite crucible in a high-temperature atmosphere sintering furnace to perform gas phase siliconizing under the argon atmosphere, wherein the heat treatment system is as follows: temperature 2173K, processing time 15min, heating rate 5K/min to obtain (Hf)0.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si composite material.
Example 2:
(1) weighing a certain amount of TiO according to the molar ratio of 1:1:1:12Powder, ZrO2Powder, HfO2Powder, Ta2O5And (3) grinding the mixture, wherein the molar ratio of the total amount of the four oxides to the B (boron) powder is 1: 4.5 weighing B powder as raw material, ethanol as solvent, ZrO2Ball milling is carried out on a planetary ball mill for 6 hours by using balls as ball milling media to obtain uniformly mixed powder A;
(2) transferring the mixed powder A into a graphite crucible, and placing the graphite crucible into a high-temperature atmosphere sintering furnace for heat treatment in an argon atmosphere, wherein the heat treatment system is as follows: the temperature is 2073K, the processing time is 1.5h, and the heating rate is 8K/min, so that a product B is obtained;
(3) and mixing the obtained product B with SiC powder according to the volume ratio of 6: 1 in an agate mortar to obtain mixture powder C;
(4) adding the powder C into a die for compression molding, wherein the pressure is 10Mpa, and obtaining a green body D;
(5) weighing a certain amount of silicon blocks, placing the silicon blocks in a graphite crucible with a porous graphite plate, placing a green body D on the porous graphite plate, sealing the graphite crucible, placing the graphite crucible in a high-temperature atmosphere sintering furnace to perform gas phase siliconizing under the argon atmosphere, wherein the heat treatment system is as follows: temperature 2073K, processing time 20min, heating rate 8K/min to obtain (Hf)0.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si composite material.
Example 3:
(1) weighing a certain amount of TiO according to the molar ratio of 1:1:1:12Powder, ZrO2Powder, HfO2Powder, Ta2O5And (3) grinding the mixture, wherein the molar ratio of the total amount of the four oxides to the B (boron) powder is 1: 4 weighing B powder as raw material, ethanol as solvent and ZrO2Ball milling is carried out on a planetary ball mill for 12 hours by taking balls as ball milling media to obtain uniformly mixed powder A;
(2) transferring the mixed powder A into a graphite crucible, and placing the graphite crucible into a high-temperature atmosphere sintering furnace for heat treatment in an argon atmosphere, wherein the heat treatment system is as follows: the temperature is 2173K, the processing time is 1h, and the heating rate is 10K/min, so that a product B is obtained;
(3) and mixing the obtained product B with SiC powder according to the volume ratio of 9: 1 in an agate mortar to obtain mixture powder C;
(4) adding the powder C into a die for compression molding, wherein the pressure is 12Mpa, and obtaining a green body D;
weighing a certain amount of silicon blocks, placing the silicon blocks in a graphite crucible with a porous graphite plate, placing a green body D on the porous graphite plate, sealing the graphite crucible, placing the graphite crucible in a high-temperature atmosphere sintering furnace to perform gas phase siliconizing under the argon atmosphere, wherein the heat treatment system is as follows: temperature 2273K, treatment time 10min, heating rate 10K/min to obtain (Hf)0.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si composite material.
Claims (3)
1. An ultrahigh-temperature ceramic composite material is characterized in that the molecular formula is as follows: (Hf)0.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si。
2. A vapor phase siliconizing process to prepare (Hf) as defined in claim 10.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si composite material, characterized by the following steps:
step 1: mixing TiO with the molar ratio of 1:1:1:12Powder, ZrO2Powder, HfO2Powder and Ta2O5Powder and boron powder as raw materials, ethanol as solvent, ZrO2Ball milling is carried out on a planetary ball mill by using balls as a ball milling medium to obtain uniformly mixed powder A; the molar ratio of the total amount of the four oxides to the boron powder is 1: 4-5;
step 2: transferring the mixed powder A into a graphite crucible, and placing the graphite crucible into a high-temperature atmosphere sintering furnace for heat treatment in an argon atmosphere to obtain a product B; the heat treatment system comprises the following steps: temperature is 1973-2173K, processing time is 1-2 h, and heating rate is 5-10K/min;
and step 3: uniformly mixing the obtained product B and SiC powder in an agate mortar according to the volume ratio of 4-9: 1 to obtain mixture powder C;
and 4, step 4: adding the powder C into a mold, and molding under the mold pressing pressure of 8-12 Mpa to obtain a green body D;
and 5: weighing a certain amount of silicon blocks, placing the silicon blocks into a graphite crucible with a porous graphite plate, placing a green compact D on the porous graphite plate, sealing the graphite crucible, placing the graphite crucible into a high-temperature atmosphere sintering furnace for gas-phase siliconizing under the argon atmosphere, wherein the temperature is 2073-2273K, the processing time is 10-20 min, and the heating rate is 5-10K/min to obtain (Hf)0.25Ta0.25Zr0.25Ti0.25)B2-SiC-Si composite material.
3. The method of claim 2, wherein: the ball milling time in the step 1 is 6-12 h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773089A (en) * | 2021-08-27 | 2021-12-10 | 郑州大学 | High-entropy disilicide and preparation method thereof |
| CN114605154A (en) * | 2022-03-31 | 2022-06-10 | 大连理工大学 | High-entropy ceramic material based on metal pre-alloying and preparation method thereof |
| CN115057709A (en) * | 2022-06-21 | 2022-09-16 | 山东大学 | High-entropy transition metal diboride and preparation method thereof |
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| CN114605154A (en) * | 2022-03-31 | 2022-06-10 | 大连理工大学 | High-entropy ceramic material based on metal pre-alloying and preparation method thereof |
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| CN116199515B (en) * | 2023-02-23 | 2024-02-06 | 广东工业大学 | Silicon carbide/high-entropy carbonitride composite powder and preparation method and application thereof |
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