CN115947603A - Six-membered high-entropy transition metal boride ceramic powder and preparation method thereof - Google Patents
Six-membered high-entropy transition metal boride ceramic powder and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 29
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- 238000000034 method Methods 0.000 claims abstract description 25
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- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 13
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- 239000001103 potassium chloride Substances 0.000 claims abstract description 12
- 239000011780 sodium chloride Substances 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract description 9
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 9
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims abstract description 9
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- 239000012300 argon atmosphere Substances 0.000 claims abstract description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000423 chromium oxide Inorganic materials 0.000 claims abstract description 7
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 claims abstract description 7
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 7
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- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 6
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 6
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Abstract
The invention relates to six-element high-entropy transition metal boride ceramic powder and a preparation method thereof. The technical scheme is as follows: mixing any six of hafnium oxide powder, zirconium oxide powder, titanium oxide powder, tantalum oxide powder, niobium oxide powder, vanadium oxide powder, tungsten oxide powder, molybdenum oxide powder and chromium oxide powder with boron carbide powder and amorphous carbon powder according to the stoichiometric ratio of the synthesis reaction to obtain a mixture A. And mixing the mixture A, potassium chloride powder and sodium chloride powder uniformly to obtain a mixture B. And (3) placing the crucible filled with the mixture B into a sagger, then placing the crucible into a microwave heating furnace, preserving the heat under the conditions of vacuum, argon atmosphere and 1250-1450 ℃, naturally cooling, cleaning and drying to obtain the hexabasic high-entropy transition metal boride ceramic powder. The invention has the advantages of low cost, simple process, low reaction temperature and high stress rate, and the prepared product has high configuration entropy, high element distribution uniformity, uniform hexagonal plate-shaped single crystal structure and good sintering activity.
Description
Technical Field
The invention belongs to the technical field of high-entropy non-oxide ceramics. In particular to hexahydric high-entropy transition metal boride ceramic powder and a preparation method thereof.
Background
Compared with low-entropy and medium-entropy transition metal boride ceramics, the high-entropy transition metal boride ceramics have obvious advantages in the aspects of hardness, elastic modulus, oxidation resistance and the like, so that the high-entropy transition metal boride ceramics have the potential of being applied to extremely severe service environments. Moreover, the performance of the high-entropy transition metal boride ceramic is continuously enhanced along with the increase of the principal element number of the transition metal boride and the corresponding configuration entropy. However, due to the intrinsic strong covalent bond characteristic of the transition metal boride ceramic and the "delayed diffusion" effect of the high-entropy structure, the preparation of the high-entropy transition metal boride ceramic powder generally requires a high reaction temperature (1800-2200 ℃) and a long holding time (not less than 1 h) or a complex ball milling treatment process, so that not only is the energy consumption and the time cost of the preparation process too high, but also various negative effects such as non-uniformity of the composition/structure of the product powder, coarsening of particles, serious agglomeration phenomenon, deterioration of sintering performance and the like are aggravated. Therefore, the preparation of high-entropy transition metal boride ceramic powder with high purity, high composition/structure uniformity and good sintering performance at low cost and high efficiency is one of the concerns of those skilled in the art.
The existing methods for preparing high-entropy transition metal boride ceramic powder comprise a thermal reduction method, a wet chemical method and an elemental reaction method. The methods generally adopt expensive raw materials, not only have high raw material cost, large energy consumption, long production time and complex process, but also can only prepare quinary high-entropy transition metal boride ceramic and powder thereof, and can not prepare high-entropy transition metal boride ceramic and powder thereof with higher principal component number (six or more) and higher configuration entropy, such as:
the patent technology of ' a high-entropy boride micro-nano particle and a preparation method thereof ' (CN 202110958844.7) ' adopts titanium powder, vanadium powder, niobium powder, zirconium powder, boron powder and aluminum powder with higher price as raw materials, ball milling treatment is firstly carried out for 8-24 h, then the ball milling treatment is carried out for 900-1600 ℃, the heat preservation is carried out for 10-200 min, and finally, the extraction, impurity removal and drying treatment are carried out to obtain the quaternary element with wider particle size distribution (0.1-0.9 mu m)High entropy (Ti) a V b Nb c Zr d )B 2 And (3) powder.
"A high entropy transition metal diboride and its preparation method (CN 202210705781.9)" patent technology using HfO 2 、ZrO 2 、Ta 2 O 5 、V 2 O 5 、Nb 2 O 5 The boron carbide powder and the carbon powder are taken as raw materials, and are sequentially subjected to high-energy-consumption wet ball milling (ball milling rotation speed of 700-1200 rmp and ball milling time of 3-8 h) and high-temperature sintering treatment (sintering temperature of 1550-1650 ℃ and heat preservation time of 1-3 h) to prepare five-membered high entropy (Hf) 0.2 Zr 0.2 Ta 0.2 V 0.2 Nb 0.2 )B 2 A material.
'A high-density, high-strength and ultra-high-hardness boron carbide/high-entropy diboride complex phase ceramic and a preparation method thereof (CN 202210474395.3)' patent technology adopting ZrO 2 、HfO 2 、Nb 2 O 5 、Ta 2 O 5 、TiO 2 、MoO 3 、WO 3 、V 2 O 5 And Cr 2 O 3 Any five kinds of powder and carbon source powder are used as raw materials, and the five-element high-entropy transition metal boride-based multiphase ceramic is prepared by a discharge plasma sintering method (the sintering temperature is 1650-1950 ℃, the sintering pressure is 10-60 MPa and the heat preservation time is 1-10 min) and under the vacuum atmosphere condition.
In conclusion, the existing methods for preparing the high-entropy transition metal boride ceramic and the powder thereof generally have the defects of high raw material cost, complex process, high reaction temperature, low reaction rate, unsuitability for industrial production, environmental pollution, incapability of synthesizing the six-element high-entropy transition metal boride ceramic and the powder thereof, and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of six-membered high-entropy transition metal boride ceramic powder, which has the advantages of low cost, simple process, low reaction temperature and high reaction rate and is suitable for industrial production and environmental protection; the hexabasic high-entropy transition metal boride ceramic powder prepared by the method has a single-phase structure, high principal component number and high configuration entropy.
In order to achieve the purpose, the invention adopts the technical scheme that:
the six-membered high-entropy transition metal boride ceramic powder has a chemical formula as follows: (TM 1) 0.167 TM2 0.167 TM3 0.167 TM4 0.167 TM5 0.167 TM6 0.167 )B 2 (ii) a The TM1, the TM2, the TM3, the TM4, the TM5 and the TM6 respectively represent any one of transition metal elements Hf, zr, ti, ta, nb, V, W, mo and Cr, and the types of the TM1, the TM2, the TM3, the TM4, the TM5 and the TM6 are different from each other; the molar weights of the TM1, the TM2, the TM3, the TM4, the TM5 and the TM6 are all equal, and the ratio of the sum of the molar weights of the TM1, the TM2, the TM3, the TM4, the TM5 and the TM6 to the molar weight of the boron element is 1: 2.
The preparation method of the six-membered high-entropy transition metal boride ceramic powder comprises the following steps:
(1) And mixing the TM1 oxide powder, the TM2 oxide powder, the TM3 oxide powder, the TM4 oxide powder, the TM5 oxide powder, the TM6 oxide powder, the boron carbide powder and the amorphous carbon powder according to the stoichiometric ratio of the synthesis reaction to obtain a mixture A.
(2) Uniformly mixing 28-38 wt% of the mixture A, 32-42 wt% of potassium chloride powder and 24-34 wt% of sodium chloride powder to obtain a mixture B.
(3) And (3) filling the mixture B into a crucible, filling the crucible into a sagger, and filling a gap between the sagger and the crucible with silicon carbide powder.
(4) And placing the sagger filled with the gaps in a microwave heating furnace, heating to 1250-1450 ℃ at the speed of 10-50 ℃/min under the conditions of the vacuum degree of 10-50 Pa and the flowing argon atmosphere, preserving the temperature for 20-40 min, and naturally cooling to obtain the roughly-treated hexahydric high-entropy transition metal boride ceramic powder.
(5) And (3) washing the rough-treated powder with deionized water for 3-5 times, and preserving heat for 6-12 hours in a vacuum drying oven at the temperature of 65-80 ℃ to obtain the hexahydric high-entropy transition metal boride ceramic powder.
The six-membered high-entropy transition metal boride ceramic powder is single-phase and has a hexagonal crystal structure.
The purities of the TM1 oxide powder, the TM2 oxide powder, the TM3 oxide powder, the TM4 oxide powder, the TM5 oxide powder and the TM6 oxide powder are all industrial grade or analytical grade, and the average particle size is less than or equal to 30 mu m.
The TM1 oxide powder, the TM2 oxide powder, the TM3 oxide powder, the TM4 oxide powder, the TM5 oxide powder, and the TM6 oxide powder are any six of hafnium oxide powder, zirconium oxide powder, titanium oxide powder, tantalum oxide powder, niobium oxide powder, vanadium oxide powder, tungsten oxide powder, molybdenum oxide powder, and chromium oxide powder.
The purity of the boron carbide powder is industrial grade or analytical grade, and the average particle size is less than or equal to 30 mu m.
The purity of the amorphous carbon powder is industrial grade or analytical grade, and the average particle size is less than or equal to 30 mu m.
The purity of the sodium chloride powder is industrial grade or analytical grade, and the average particle size is less than or equal to 100 mu m.
The purity of the potassium chloride powder is industrial grade or analytical grade, and the average particle size is less than or equal to 100 mu m.
The purity of the silicon carbide powder is industrial grade or analytical grade, and the average particle size is less than or equal to 5mm.
Compared with the prior art, the invention has the following positive effects and prominent characteristics due to the adoption of the technical scheme:
1. the invention adopts the synergistic effect of microwave and molten salt synthesis conditions to prepare the hexabasic high-entropy transition metal boride ceramic powder which can not be prepared by the conventional molten salt method. Compared with quinary high-entropy transition metal boride ceramic powder, the hexabasic high-entropy transition metal boride ceramic powder prepared by the method has higher principal element number, higher configuration entropy and more excellent sintered ceramic performance.
2. The microwave/molten salt condition adopted by the invention has the following two important effects: on one hand, the average atomic diffusion distance of reactants is effectively reduced, and the diffusion rate can be improved, so that the synthesis rate of the hexatomic high-entropy transition metal boride is accelerated; on the other hand, growth of the hexabasic high-entropy transition metal boride is promoted to form a hexagonal plate-shaped morphology and a single crystal structure.
3. The hexabasic high-entropy transition metal boride ceramic powder prepared by the invention has uniform hexagonal plate-shaped appearance: the width is 300-900 nm, the thickness is 30-120 nm, and the specific surface area is 240-420 g/m 2 Therefore, the sintering activity is good.
4. The preparation method does not generate any solid phase by-product, so the six-membered high-entropy transition metal boride ceramic powder and the molten salt medium can be separated by simple and efficient water washing treatment, thereby being beneficial to the saving and utilization of water resources and the recovery and recycling of the molten salt medium and meeting the requirements of environmental protection.
Therefore, the method has the characteristics of low cost, simple process, low reaction temperature, high reaction rate, suitability for industrial production and environmental protection, and the prepared hexabasic high-entropy transition metal boride ceramic powder has high configuration entropy, high element distribution uniformity, uniform hexagonal plate-shaped single crystal structure and good sintering activity.
Drawings
FIG. 1 is an XRD (X-ray diffraction) pattern of six-element high-entropy transition metal boride ceramic powder prepared by the invention;
FIG. 2 is a TEM photograph of the hexabasic high-entropy transition metal boride ceramic powder shown in FIG. 1.
Detailed Description
The invention is further described with reference to the following figures and detailed description, without limiting its scope.
A six-membered high-entropy transition metal boride ceramic powder and a preparation method thereof.
The chemical formula of the hexahydric high-entropy transition metal boride powder in the embodiment is as follows: (TM 1) 0.167 TM2 0.16 7 TM3 0.167 TM4 0.167 TM5 0.167 TM6 0.167 )B 2 (ii) a The TM1, the TM2, the TM3, the TM4, the TM5 and the TM6 respectively represent any one of transition metal elements Hf, zr, ti, ta, nb, V, W, mo and Cr.
The preparation method of the six-membered high-entropy transition metal boride ceramic powder comprises the following steps:
(1) And mixing the TM1 oxide powder, the TM2 oxide powder, the TM3 oxide powder, the TM4 oxide powder, the TM5 oxide powder, the TM6 oxide powder, the boron carbide powder and the amorphous carbon powder according to the stoichiometric ratio of the synthesis reaction to obtain a mixture A.
(2) Uniformly mixing 28-38 wt% of the mixture A, 32-42 wt% of potassium chloride powder and 24-34 wt% of sodium chloride powder to obtain a mixture B.
(3) And (3) filling the mixture B into a crucible, filling the crucible into a sagger, and filling a gap between the sagger and the crucible with silicon carbide powder.
(4) And placing the sagger filled with the gaps in a microwave heating furnace, heating to 1250-1450 ℃ at the speed of 10-50 ℃/min under the conditions of the vacuum degree of 10-50 Pa and the flowing argon atmosphere, preserving the temperature for 20-40 min, and naturally cooling to obtain the roughly-treated hexahydric high-entropy transition metal boride ceramic powder.
(5) And (3) washing the rough-treated powder with deionized water for 3-5 times, and preserving heat for 6-12 hours in a vacuum drying oven at the temperature of 65-80 ℃ to obtain the hexahydric high-entropy transition metal boride ceramic powder.
The six-membered high-entropy transition metal boride ceramic powder is single-phase and has a hexagonal crystal structure.
In this embodiment:
the TM1, the TM2, the TM3, the TM4, the TM5 and the TM6 are different in type; the molar weight of TM1, TM2, TM3, TM4, TM5 and TM6 are all equal, and the ratio of the sum of the molar weight of TM1, TM2, TM3, TM4, TM5 and TM6 to the molar weight of boron is 1: 2.
The purities of the TM1 oxide powder, the TM2 oxide powder, the TM3 oxide powder, the TM4 oxide powder, the TM5 oxide powder and the TM6 oxide powder are all industrial grade or analytical grade, and the average particle size is less than or equal to 30 mu m.
The TM1 oxide powder, the TM2 oxide powder, the TM3 oxide powder, the TM4 oxide powder, the TM5 oxide powder, and the TM6 oxide powder are any six of hafnium oxide powder, zirconium oxide powder, titanium oxide powder, tantalum oxide powder, niobium oxide powder, vanadium oxide powder, tungsten oxide powder, molybdenum oxide powder, and chromium oxide powder.
The purity of the boron carbide powder is industrial grade or analytical grade, and the average particle size is less than or equal to 30 mu m.
The purity of the amorphous carbon powder is industrial grade or analytical grade, and the average particle size is less than or equal to 30 mu m.
The purity of the sodium chloride powder is industrial grade or analytical grade, and the average particle size is less than or equal to 100 mu m.
The purity of the potassium chloride powder is industrial grade or analytical grade, and the average particle size is less than or equal to 100 mu m.
The purity of the silicon carbide powder is industrial grade or analytical grade, and the average particle size is less than or equal to 5mm.
The detailed description is omitted in the embodiments.
Example 1
A six-membered high-entropy transition metal boride ceramic powder and a preparation method thereof.
In this embodiment, the chemical formula of the hexahydric high-entropy transition metal boride ceramic powder is:
(TM1 0.167 TM2 0.167 TM3 0.167 TM4 0.167 TM5 0.167 TM6 0.167 )B 2 the TM1, TM2, TM3, TM4, TM5 and TM6 sequentially represent transition metal elements Hf, zr, ti, ta, nb and V.
The preparation method of the six-membered high-entropy transition metal boride ceramic powder comprises the following steps:
(1) Mixing hafnium oxide powder, zirconium oxide powder, titanium oxide powder, tantalum oxide powder, niobium oxide powder, vanadium oxide powder, boron carbide powder and amorphous carbon powder according to the molar ratio of transition metal elements and the stoichiometric ratio of synthesis reaction to obtain a mixture A.
(2) Uniformly mixing the mixture A of 36wt%, the potassium chloride powder of 34wt% and the sodium chloride powder of 30wt% to obtain a mixture B.
(3) And (3) filling the mixture B into a crucible, filling the crucible into a sagger, and filling a gap between the sagger and the crucible with silicon carbide powder.
(4) Placing the sagger filled with the gap in a microwave heating furnace, heating to 1430 ℃ at the speed of 20 ℃/min under the conditions of the vacuum degree of 10Pa and the flowing argon atmosphere, preserving the temperature for 25min, and naturally cooling to obtain the roughly-treated hexahydric high-entropy transition metal (Zr) 0.167 Ta .167 Nb 0.167 W 0.167 Mo 0.167 Cr 0.167 )B 2 And (3) powder.
(5) Washing the roughly treated powder with deionized water for 5 times, and keeping the temperature in a vacuum drying oven at 65 ℃ for 12 hours to obtain the hexahydric high-entropy (Hf) 0.167 Zr 0.167 Ti 0.167 Ta 0.167 Nb 0.167 V 0.167 )B 2 And (3) powder.
Six-membered high entropy (Hf) prepared in this example 0.167 Zr 0.167 Ti 0.167 Ta 0.167 Nb 0.167 V 0.167 )B 2 The powder is single-phase and has the characteristics of hexagonal plate-shaped single crystal structure and high element distribution uniformity. Prepared hexahydric high entropy (Hf) 0.167 Zr 0.167 Ti 0.167 Ta 0.167 Nb 0.167 V 0.167 )B 2 Powder particles: a width of 840nm, a thickness of 100nm, a specific surface area of 270g/m 2 Therefore, the sintering activity is good.
Example 2
A six-membered high-entropy transition metal boride ceramic powder and a preparation method thereof.
In this embodiment, the chemical formula of the hexabasic high-entropy transition metal boride ceramic powder is:
(TM1 0.167 TM2 0.167 TM3 0.167 TM4 0.167 TM5 0.167 TM6 0.167 )B 2 wherein TM1, TM2, TM3, TM4, TM5 and TM6 sequentially represent transition metal elements Ti, ta, nb, V, M 0 And W.
The preparation method of the six-membered high-entropy transition metal boride ceramic powder comprises the following steps:
(1) Mixing titanium oxide powder, tantalum oxide powder, niobium oxide powder, vanadium oxide powder, molybdenum oxide powder, tungsten oxide powder, boron carbide powder and amorphous carbon powder according to the equal molar ratio of transition metal elements and the stoichiometric ratio of synthesis reaction to obtain a mixture A.
(2) And uniformly mixing 34wt% of the mixture A, 32wt% of potassium chloride powder and 34wt% of sodium chloride powder to obtain a mixture B.
(3) And (3) filling the mixture B into a crucible, filling the crucible into a sagger, and filling a gap between the sagger and the crucible with silicon carbide powder.
(4) Placing the sagger filled with the gap into a microwave heating furnace, heating to 1250 ℃ at the speed of 25 ℃/min under the conditions of vacuum degree of 40Pa and flowing argon atmosphere, preserving heat for 35min, and naturally cooling to obtain the roughly-treated hexahydric high-entropy (Ti) 0.167 Ta .167 Nb 0.167 V 0.167 Mo 0.167 W 0.167 )B 2 And (3) powder.
(5) Washing the roughly treated powder with deionized water for 4 times, and preserving heat in a vacuum drying oven at 70 ℃ for 10 hours to obtain hexahydric high-entropy (Ti) 0.167 Ta .167 Nb 0.167 V 0.167 Mo 0.167 W 0.167 )B 2 And (3) powder.
The six-membered high entropy (Ti) prepared in this example 0.167 Ta .167 Nb 0.167 V 0.167 Mo 0.167 W 0.167 )B 2 The powder is single-phase and has the characteristics of hexagonal plate-shaped single crystal structure and high element distribution uniformity. Prepared hexahydric high entropy (Hf) 0.167 Zr 0.167 Ti 0.167 Ta 0.167 Nb 0.167 V 0.167 )B 2 Powder particles: the width is 300nm, the thickness is 60nm, and the specific surface area is 240g/m 2 Therefore, the sintering activity is good.
Example 3
A six-membered high-entropy transition metal boride ceramic powder and a preparation method thereof.
The six-membered high entropy sieve described in this exampleThe chemical formula of the transition metal boride ceramic powder is as follows: (TM 1) 0.167 TM2 0.167 TM3 0.167 TM4 0.167 TM5 0.167 TM6 0.167 )B 2 The TM1, TM2, TM3, TM4, TM5 and TM6 sequentially represent transition metal elements Hf, zr, ta, nb, cr and W.
The preparation method of the six-membered high-entropy transition metal boride ceramic powder comprises the following steps:
(1) Mixing hafnium oxide powder, zirconium oxide powder, tantalum oxide powder, niobium oxide powder, chromium oxide powder, tungsten oxide powder, boron carbide powder and amorphous carbon powder according to the molar ratio of transition metal elements and the stoichiometric ratio of synthesis reaction to obtain a mixture A.
(2) And uniformly mixing 28wt% of the mixture A, 40wt% of potassium chloride powder and 32wt% of sodium chloride powder to obtain a mixture B.
(3) And (3) filling the mixture B into a crucible, filling the crucible into a sagger, and filling a gap between the sagger and the crucible with silicon carbide powder.
(4) Placing the sagger filled with the gap into a microwave heating furnace, heating to 1350 ℃ at the speed of 10 ℃/min under the conditions of the vacuum degree of 25Pa and the flowing argon atmosphere, preserving the heat for 30min, and naturally cooling to obtain the roughly-treated hexahydric high-entropy (Hf) 0.167 Zr .167 Ta 0.167 Nb 0.167 Cr 0.167 W 0.167 )B 2 And (3) powder.
(5) Washing the roughly treated powder with deionized water for 5 times, and keeping the temperature in a vacuum drying oven at 75 ℃ for 8 hours to obtain the hexahydric high-entropy (Hf) 0.167 Zr .167 Ta 0.167 Nb 0.167 Cr 0.167 W 0.167 )B 2 And (3) powder.
Six-membered high entropy (Hf) prepared in this example 0.167 Zr .167 Ta 0.167 Nb 0.167 Cr 0.167 W 0.167 )B 2 The powder is single-phase and has the characteristics of hexagonal plate-shaped single crystal structure and high element distribution uniformity. Prepared hexahydric high entropy (Hf) 0.167 Zr 0.167 Ti 0.167 Ta 0.167 Nb 0.167 V 0.167 )B 2 Powder particles: the width is 360nm, the thickness is 120nm, and the specific surface area is 420g/m 2 Therefore, the sintering activity is good.
Example 4
A six-membered high-entropy transition metal boride ceramic powder and a preparation method thereof.
In this embodiment, the chemical formula of the hexahydric high-entropy transition metal boride ceramic powder is:
(TM1 0.167 TM2 0.167 TM3 0.167 TM4 0.167 TM5 0.167 TM6 0.167 )B 2 the TM1, TM2, TM3, TM4, TM5 and TM6 sequentially represent transition metal elements Hf, zr, ti, ta, nb and Cr.
The preparation method of the six-membered high-entropy transition metal boride ceramic powder comprises the following steps:
(1) Mixing hafnium oxide powder, zirconium oxide powder, titanium oxide powder, tantalum oxide powder, niobium oxide powder, chromium oxide powder, boron carbide powder and amorphous carbon powder according to the molar ratio of transition metal elements and the stoichiometric ratio of synthesis reaction to obtain a mixture A.
(2) And uniformly mixing 30wt% of the mixture A, 42wt% of potassium chloride powder and 28wt% of sodium chloride powder to obtain a mixture B.
(3) And (3) filling the mixture B into a crucible, filling the crucible into a sagger, and filling a gap between the sagger and the crucible with silicon carbide powder.
(4) Placing the sagger filled with the gap in a microwave heating furnace, heating to 1300 ℃ at the speed of 50 ℃/min under the conditions of the vacuum degree of 50Pa and the flowing argon atmosphere, preserving the temperature for 40min, and naturally cooling to obtain the roughly-treated hexahydric high-entropy (Hf) 0.167 Zr .167 Ti 0.167 Ta 0.167 Nb 0.167 Cr 0.167 )B 2 And (3) powder.
(5) Washing the roughly treated powder with deionized water for 3 times, and keeping the temperature in a vacuum drying oven at 80 ℃ for 6 hours to obtain hexahydric high entropy (Hf) 0.167 Zr .167 Ti 0.167 Ta 0.167 Nb 0.167 Cr 0.167 )B 2 And (3) powder.
Six-membered high entropy (Hf) prepared in this example 0.167 Zr .167 Ti 0.167 Ta 0.167 Nb 0.167 Cr 0.167 )B 2 The powder is single-phase and has the characteristics of hexagonal plate-shaped single crystal structure and high element distribution uniformity. Prepared hexahydric high entropy (Hf) 0.167 Zr 0.167 Ti 0.167 Ta 0.167 Nb 0.167 V 0.167 )B 2 Powder particles: 900nm in width, 70nm in thickness and 390g/m in specific surface area 2 Therefore, the sintering activity is good.
Example 5
A six-membered high-entropy transition metal boride ceramic powder and a preparation method thereof.
In this embodiment, the chemical formula of the hexahydric high-entropy transition metal boride ceramic powder is:
(TM1 0.167 TM2 0.167 TM3 0.167 TM4 0.167 TM5 0.167 TM6 0.167 )B 2 the TM1, TM2, TM3, TM4, TM5 and TM6 sequentially represent transition metal elements Zr, ta, nb, W, mo and Cr.
The preparation method of the six-membered high-entropy transition metal boride ceramic powder comprises the following steps:
(1) Mixing zirconium oxide powder, tantalum oxide powder, niobium oxide powder, tungsten oxide powder, molybdenum oxide powder, chromium oxide powder, boron carbide powder and amorphous carbon powder according to the molar ratio of transition metal elements and the stoichiometric ratio of synthesis reaction to obtain a mixture A.
(2) Uniformly mixing 38wt% of the mixture A, 38wt% of potassium chloride powder and 24wt% of sodium chloride powder to obtain a mixture B.
(3) And (3) filling the mixture B into a crucible, filling the crucible into a sagger, and filling a gap between the sagger and the crucible with silicon carbide powder.
(4) Placing the sagger filled with the gap in a microwave heating furnace, heating to 1450 deg.C at 35 deg.C/min under the conditions of vacuum degree of 35Pa and flowing argon atmospherePreserving heat for 20min, and naturally cooling to obtain crude six-membered high entropy (Zr) 0.167 Ta .167 Nb 0.167 W 0.167 Mo 0.167 Cr 0.167 )B 2 And (3) powder.
(5) Washing the roughly treated powder with deionized water for 3 times, and preserving heat for 8 hours in a vacuum drying oven at 75 ℃ to obtain hexahydric high-entropy (Zr) 0.167 Ta .167 Nb 0.167 W 0.167 Mo 0.167 Cr 0.167 )B 2 And (3) powder.
Six-membered high entropy (Zr) prepared in this example 0.167 Ta .167 Nb 0.167 W 0.167 Mo 0.167 Cr 0.167 )B 2 The powder is single-phase and has the characteristics of hexagonal plate-shaped single crystal structure and high element distribution uniformity. Prepared hexahydric high entropy (Hf) 0.167 Zr 0.167 Ti 0.167 Ta 0.167 Nb 0.167 V 0.167 )B 2 Powder particles: the width is 750nm, the thickness is 30nm, and the specific surface area is 410g/m 2 Therefore, the sintering activity is good.
Compared with the prior art, the specific implementation mode has the following positive effects and outstanding characteristics:
1. the specific embodiment adopts the synergistic effect of microwave and molten salt synthesis conditions, and can prepare the hexabasic high-entropy transition metal boride ceramic powder which can not be prepared by the conventional molten salt method. Compared with quinary high-entropy transition metal boride ceramic powder, the hexabasic high-entropy transition metal boride ceramic powder prepared by the embodiment has higher principal element number, higher configuration entropy and more excellent sintered ceramic performance.
2. The microwave/molten salt conditions adopted by the embodiment have the following two important effects: on one hand, the average atomic diffusion distance of reactants is effectively reduced, and the diffusion rate can be improved, so that the synthesis rate of the hexatomic high-entropy transition metal boride is accelerated; on the other hand, growth of the hexabasic high-entropy transition metal boride is promoted to form a hexagonal plate-shaped morphology and a single crystal structure.
3. The six-membered high-entropy transition metal boride ceramic powder prepared by the specific embodimentAs shown in the attached drawings, FIG. 1 is a six-membered high entropy (Hf) prepared in example 1 0.167 Zr 0.167 Ti 0.167 Ta 0.167 Nb 0.167 V 0.167 )B 2 The XRD pattern of the powder can be seen from FIG. 1: the prepared hexahydric high-entropy transition metal boride ceramic powder is single-phase and high in purity; FIG. 2 is the six-membered high entropy (Hf) shown in FIG. 1 0.167 Zr 0.167 Ti 0.167 Ta 0.167 Nb 0.167 V 0.167 )B 2 And (3) TEM (transmission electron microscope) photos of the powder, wherein the prepared hexabasic high-entropy transition metal boride ceramic powder has a uniform hexagonal plate shape: a width of 840nm, a thickness of 100nm, a specific surface area of 270g/m 2 Therefore, the sintering activity is good.
The hexahydric high-entropy transition metal boride ceramic powders prepared in examples 1, 2, 3, 4 and 5 of the present embodiment are sequentially hexahydric high-entropy (Hf) 0.167 Zr 0.167 Ti 0.167 Ta 0.167 Nb 0.167 V 0.167 )B 2 Powder, hexahydric high entropy (Ti) 0.167 Ta .167 Nb 0.167 V 0.167 Mo 0.167 W 0.167 )B 2 Powder, hexahydric high entropy (Hf) 0.167 Zr .167 Ta 0.167 Nb 0.167 Cr 0.167 W 0.167 )B 2 Powder, hexahydric high entropy (Hf) 0.167 Zr .167 Ti 0.167 Ta 0.167 Nb 0.167 Cr 0.167 )B 2 High entropy of powder and hexahydric (Zr) 0.167 Ta .167 Nb 0.167 W 0.167 Mo 0.167 Cr 0.167 )B 2 The powder, the prepared hexahydric high-entropy transition metal boride ceramic powder has uniform hexagonal plate-shaped appearance: the width is 300-900 nm, the thickness is 30-120 nm, and the specific surface area is 240-420 g/m 2 Therefore, the sintering activity is good.
4. The preparation method of the embodiment does not produce any solid phase by-product, so that the prepared hexabasic high-entropy transition metal boride ceramic powder and the molten salt medium can be separated by simple and efficient washing treatment, thereby being beneficial to saving and utilizing water resources and recycling and reusing the molten salt medium and meeting the requirements of environmental protection.
Therefore, the specific embodiment has the characteristics of low cost, simple process, low reaction temperature, high reaction rate, suitability for industrial production and environmental protection, and the prepared hexabasic high-entropy transition metal boride ceramic powder has high configuration entropy, high element distribution uniformity, uniform hexagonal plate-shaped single crystal structure and good sintering activity.
Claims (8)
1. A preparation method of six-membered high-entropy transition metal boride ceramic powder is characterized by comprising the following steps:
the six-membered high-entropy transition metal boride ceramic powder has a chemical formula as follows:
(TM1 0.167 TM2 0.167 TM3 0.167 TM4 0.167 TM5 0.167 TM6 0.167 )B 2 (ii) a The TM1, the TM2, the TM3, the TM4, the TM5 and the TM6 respectively represent any one of transition metal elements Hf, zr, ti, ta, nb, V, W, mo and Cr, and the types of the TM1, the TM2, the TM3, the TM4, the TM5 and the TM6 are different from each other; the molar weights of the TM1, the TM2, the TM3, the TM4, the TM5 and the TM6 are all equal, and the ratio of the sum of the molar weights of the TM1, the TM2, the TM3, the TM4, the TM5 and the TM6 to the molar weight of the boron element is 1: 2;
the preparation method of the six-membered high-entropy transition metal boride ceramic powder comprises the following steps:
(1) Mixing the TM1 oxide powder, the TM2 oxide powder, the TM3 oxide powder, the TM4 oxide powder, the TM5 oxide powder, the TM6 oxide powder, the boron carbide powder and the amorphous carbon powder according to the stoichiometric ratio of the synthesis reaction to obtain a mixture A;
(2) Uniformly mixing 28-38 wt% of the mixture A, 32-42 wt% of potassium chloride powder and 24-34 wt% of sodium chloride powder to obtain a mixture B;
(3) Filling the mixture B into a crucible, filling the crucible into a sagger, and filling a gap between the sagger and the crucible with silicon carbide powder;
(4) Placing the sagger filled with the gaps in a microwave heating furnace, heating to 1250-1450 ℃ at the speed of 10-50 ℃/min under the conditions of the vacuum degree of 10-50 Pa and the flowing argon atmosphere, preserving the temperature for 20-40 min, and naturally cooling to obtain roughly-treated hexahydric high-entropy transition metal boride ceramic powder;
(5) Washing the crude treatment powder with deionized water for 3-5 times, and preserving heat for 6-12 h in a vacuum drying oven at the temperature of 65-80 ℃ to obtain hexahydric high-entropy transition metal boride ceramic powder;
the six-membered high-entropy transition metal boride ceramic powder is single-phase and has a hexagonal crystal structure.
2. The method for preparing hexabasic high-entropy transition metal boride ceramic powder according to claim 1, characterized in that the purities of TM1 oxide powder, TM2 oxide powder, TM3 oxide powder, TM4 oxide powder, TM5 oxide powder and TM6 oxide powder are all industrial grade or analytical grade, and the average particle size is less than or equal to 30 μm;
the TM1 oxide powder, the TM2 oxide powder, the TM3 oxide powder, the TM4 oxide powder, the TM5 oxide powder, and the TM6 oxide powder are any six of hafnium oxide powder, zirconium oxide powder, titanium oxide powder, tantalum oxide powder, niobium oxide powder, vanadium oxide powder, tungsten oxide powder, molybdenum oxide powder, and chromium oxide powder.
3. The method for preparing six-membered high entropy transition metal boride ceramic powder of claim 1, characterized in that the purity of the boron carbide powder is technical or analytical grade, the average particle size is less than or equal to 30 μm.
4. The method for preparing six-membered high entropy transition metal boride ceramic powder of claim 1, characterized in that the amorphous carbon powder has a purity of technical grade or analytical grade and an average particle size of not more than 30 μm.
5. The method for preparing hexahydric high-entropy transition metal boride ceramic powder according to claim 1, wherein the purity of the sodium chloride powder is industrial grade or analytical grade, and the average particle size is less than or equal to 100 μm.
6. The method for preparing six-membered high entropy transition metal boride ceramic powder of claim 1, characterized in that the purity of the potassium chloride powder is technical grade or analytical grade, and the average particle size is less than or equal to 100 μm.
7. The method for preparing six-membered high-entropy transition metal boride ceramic powder according to claim 1, characterized in that the purity of the silicon carbide powder is industrial grade or analytical grade, and the average particle size is less than or equal to 5mm.
8. A hexabasic high entropy transition metal boride ceramic powder, characterized in that the hexabasic high entropy transition metal boride ceramic powder is prepared according to the preparation method of the hexabasic high entropy transition metal boride ceramic powder of any one of claims 1-7.
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