CN115073183A - High-entropy boride nano powder and sol-gel preparation method thereof - Google Patents
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Abstract
The invention provides a high-entropy transition metal diboride material and a sol-gel liquid phase preparation method thereof, belonging to the technical field of preparation of ultrahigh-temperature ceramic materials. The nominal molecular formula of the high-entropy transition metal diboride material is (Hf) 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 And the proportion of the transition metal elements can be regulated and controlled according to actual requirements. The high-entropy transition metal diboride material has the characteristics of high purity, small particle size and uniform element distribution, and has a good application prospect in the field of ultrahigh-temperature materials.Meanwhile, the sol-gel preparation method adopted by the invention belongs to a liquid phase method, and can realize the atomic-level mixing of different metal ions. And the process is simple, and the high-entropy boride powder with the particle size of nanometer can be produced, so that the method has good practical application value.
Description
Technical Field
The invention belongs to the technical field of preparation of ultra-high temperature structural materials and nano materials, and particularly relates to high-entropy boride nano powder and a sol-gel preparation method thereof.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
The high-entropy transition metal diboride ceramic belongs to ultrahigh-temperature ceramic, has excellent characteristics of high melting point (more than 3000 ℃), high hardness, high melting point, high conductivity, oxidation resistance, corrosion resistance, high-temperature stability and the like, can be used in a high-temperature environment of 2000 ℃, and has very wide application prospects in the fields of machining, aerospace, wear-resistant coatings and the like. Compared with boride ceramics with single component, the high-entropy transition metal diboride ceramics have more excellent performances such as higher hardness and better oxidation resistance due to the high-entropy effect, the delayed diffusion effect, the lattice distortion effect and the cocktail effect. However, as with other ceramic materials, high entropy transition metal diboride ceramics suffer from their intrinsic brittleness.
The transition metal diboride high-entropy ceramic generally has a hexagonal crystal structure, in the c-axis direction, transition metal atomic layers and boron atomic layers are alternately arranged, five transition metal elements randomly occupy sites of the metal atomic layers, the five transition metal elements are combined in the boron atomic layers in a covalent bond mode, and the boron atomic layers are combined with the metal atomic layers in an ionic bond mode. Because of the extremely strong chemical bond, the transition metal diboride high-entropy ceramic has very high melting point and low self-diffusion coefficient, so the preparation of single-phase powder and the sintering conditions of the ceramic are extremely strict, and extremely high temperature or extremely high pressure is required. This makes the preparation of nano high-entropy transition metal diboride powders more difficult.
At present, with respect to high entropy transition metalsThe diboride materials are prepared by a number of methods, including borothermic reduction, borothermic/carbothermic reduction, molten salt processes, self-propagating high temperature sintering, SPS direct sintering, and high pressure sintering. However, the high entropy transition metal diboride powders prepared by these methods are all relatively coarse in particle size or only the preparation of four-component high entropy borides is reported, with oxygen impurities and other impurities. The sol-gel method is a liquid phase preparation method capable of efficiently producing nano powder, but the inventor finds that the research on the preparation of the high-entropy transition metal diboride powder by the sol-gel method is not available at present, and the high entropy (Hf) of the high-entropy transition metal diboride powder is not available 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 Research and report of nano powder.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide high-entropy boride nano-powder and a sol-gel preparation method thereof. The invention takes transition metal chloride or organic precursor as a metal source, boric acid and sorbitol as a boron source and a carbon source respectively, and citric acid and glycol as complexing agents, realizes solid solution at a lower temperature by regulating and controlling the calcination temperature and the heat preservation time of the powder, forms single-phase powder with a nanometer size, and has good value in practical application.
In order to achieve the purpose, the invention is realized by the following technical scheme:
in a first aspect of the invention there is provided a high entropy transition metal diboride material having a nominal molecular formula of (Hf) 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 。
It should be noted that the proportion of elements in the same position of the high-entropy transition metal diboride material can be regulated according to actual requirements, the high-entropy transition metal diboride material has a hexagonal structure, a unit cell is formed by alternately stacking transition metal atomic layers and B atomic layers in the c direction, and five transition metal atoms are randomly distributed in the transition metal atomic layers.
In a second aspect of the present invention, there is provided a sol-gel process for the preparation of the above high entropy transition metal diboride material, said process comprising:
dissolving Hf source, Nb source, Cr source, Ta source, Mo source, B source and carbon source in organic solvent, and fully dissolving to form transparent solution, wherein the molar ratio of Hf, Nb, Cr, Ta and Mo is 0.1-1:0.1-1:0.1-1:0.1-1:0.1-1, and the molar ratio of the total of transition metals to boron is 1: 2-3;
adding citric acid and ethylene glycol into the transparent solution, and continuing heating for complex reaction to obtain transparent sol;
drying the transparent sol to obtain dry gel, grinding the dry gel, and calcining to obtain the transparent sol;
each metal source is a chloride of each metal element or an organic precursor; the boron source is boric acid and the carbon source is sorbitol.
The beneficial effects achieved by one or more of the embodiments of the invention described above are as follows:
1) according to the technical scheme, five transition metal chlorides, an organic precursor, boric acid powder and sorbitol are used as raw materials, and single-phase formation of high-entropy boride is realized through dissolution, stirring, heating, drying and calcination. The obtained high-entropy transition metal diboride material has the advantages of high purity, small particle size and uniform element distribution;
2) the sol-gel preparation method adopted by the invention belongs to a liquid phase method, can realize the atomic-level mixing of different metal ions, has simple process, and can produce the high-entropy boride powder with the grain diameter of nanometer level, thereby having good practical application value.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 shows high entropy (Hf) prepared in example 1 of the present invention 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 X-ray diffraction pattern of the powder;
FIG. 2 is a graph of a polymer prepared in example 1 of the present inventionHigh entropy (Hf) 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 Scanning electron micrographs of the powders.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise. It is to be understood that the scope of the invention is not to be limited to the specific embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention.
In a first aspect, the invention provides a sol-gel preparation method of high-entropy boride nano-powder, which comprises the following steps:
dissolving Hf source, Nb source, Cr source, Ta source, Mo source, B source and carbon source in organic solvent, and fully dissolving to form transparent solution, wherein the molar ratio of Hf, Nb, Cr, Ta and Mo is 0.1-1:0.1-1:0.1-1:0.1-1:0.1-1, and the molar ratio of the total of transition metals to boron is 1: 2-3;
adding citric acid and ethylene glycol into the transparent solution, and continuing heating for complex reaction to obtain transparent sol;
drying the transparent sol to obtain dry gel, grinding the dry gel, and calcining to obtain the transparent sol;
each metal source is a chloride of each metal element or an organic precursor; the boron source is boric acid and the carbon source is sorbitol.
The reaction is carbothermic reduction of boron, and a carbon source is used as a reducing agent.
In some embodiments, the molar ratio of Hf, Nb, Cr, Ta, and Mo is from 0.2 to 1:0.2 to 1;
preferably, the mole ratio of Hf, Nb, Cr, Ta and Mo is 1:1:1:1: 1.
In some embodiments, the organic solvent is absolute ethanol.
In some embodiments, the heat is continuously stirred during the complexation. The stirring mode is manual stirring or magnetic stirring.
Preferably, the temperature of the complexation reaction is 50-180 ℃.
In some embodiments, the molar ratio of the sum of the transition metals, boron, and carbon in sorbitol is from 1:2 to 3:8 to 12.
In some embodiments, the temperature at which the transparent sol is dried is 100-300 ℃.
In some embodiments, after the xerogel is ground, the method further comprises the step of dry-pressing the xerogel powder into a shape, and calcining the dry-pressed shape.
Preferably, the pressure for dry-pressing is 1 to 20 MPa. For example, it may be 1MPa, 2MPa, 3MPa, 4MPa, 5MPa, 6MPa, 7MPa, 8MPa, 9MPa, 10MPa, 11MPa, 12MPa, 13MPa, 14MPa, 15MPa, 16MPa, 17MPa, 18MPa, 19MPa, or 20 MPa.
Preferably, the calcining temperature is 1500-.
Preferably, the calcination is carried out in an inert atmosphere, or under vacuum conditions.
In a second aspect, the invention provides high-entropy boride nano-powder, which is prepared by the sol-gel preparation method.
Preferably, the molecular formula of the high-entropy boride nano powder is (Hf) 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 。
The high-entropy transition metal diboride material prepared by the invention has the advantages that the element proportion in the same position can be regulated and controlled according to actual requirements, the material has a hexagonal crystal structure, a unit cell is formed by alternately stacking transition metal atomic layers and B atomic layers in the c direction, and five transition metal atoms are randomly distributed in the transition metal atomic layers.
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are test methods in which specific conditions are indicated, and are generally carried out under conventional conditions.
Example 1:
in this example, a nanometer high entropy (Hf) was prepared 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 A material. The method comprises the following specific steps:
1) weighing raw materials according to a molar ratio of Hf to Nb to Cr to Ta to Mo to B to C of 1:1:1:1:15:40, wherein metal sources are respectively hafnium chloride, niobium chloride, chromium chloride, tantalum chloride and molybdenum acetylacetonate, a boron source is boric acid, a carbon source is sorbitol, and each weighed metal element is 0.003 mol;
2) dissolving the raw materials weighed in the step 1) in 40ml of absolute ethyl alcohol, stirring and heating the mixture on a magnetic stirring heating table to 80 ℃ to fully dissolve the raw materials to form a transparent solution;
3) adding 0.02mol of citric acid and 2.5g of glycol as complexing agents into the transparent solution obtained in the step 2), and continuously heating and stirring until the transparent solution becomes transparent sol;
4) drying the transparent sol formed in the step 3) in a vacuum drying oven at 130 ℃ to form xerogel;
5) grinding the xerogel formed in the step 4) and performing dry pressing forming under 2MPa to obtain a cylindrical powder block;
6) calcining the cylindrical powder block obtained in the step 5) at 1650 ℃, and keeping the temperature for 3 h. The phase information and the micro morphology of the obtained nano high-entropy boride powder refer to an X-ray diffraction spectrum and a scanning electron microscope photo shown in figures 1 and 2 respectively.
Example 2:
in this example, a nanohorn was preparedEntropy (Hf) 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 A material. The method comprises the following specific steps:
1) weighing raw materials according to a molar ratio of Hf to Nb to Cr to Ta to Mo to B to C of 1:1:1:1:15:40, wherein metal sources are respectively hafnium chloride, niobium chloride, chromium chloride, tantalum chloride and molybdenum acetylacetonate, a boron source is boric acid, a carbon source is sorbitol, and each weighed metal element is 0.003 mol;
2) dissolving the raw materials weighed in the step 1) in 50ml of absolute ethyl alcohol, stirring and heating the mixture on a magnetic stirring heating table to 90 ℃ to fully dissolve the raw materials to form a transparent solution;
3) adding 0.02mol of citric acid and 2.5g of glycol as complexing agents into the transparent solution obtained in the step 2), and continuously heating and stirring until the transparent solution becomes transparent sol;
4) drying the transparent sol formed in the step 3) in a vacuum drying oven at 150 ℃ to form xerogel;
5) grinding the xerogel formed in the step 4) and dry-pressing and forming under 5MPa to obtain a cylindrical powder block;
6) calcining the cylindrical powder block obtained in the step 5) at 1700 ℃, and keeping the temperature for 2 h. High entropy (Hf) can be obtained 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 And (3) powder.
Example 3:
in this example, a nanometer high entropy (Hf) was prepared 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 A material. The method comprises the following specific steps:
1) weighing raw materials according to a molar ratio of Hf to Nb to Cr to Ta to Mo to B to C of 1:1:1:1:15:38, wherein each metal ion is weighed to be 0.003 mol;
2) dissolving the raw materials weighed in the step 1) in 45ml of absolute ethyl alcohol, stirring and heating the mixture on a magnetic stirring heating table to 85 ℃ to fully dissolve the raw materials to form a transparent solution;
3) adding 0.02mol of citric acid and 3.0g of glycol as complexing agents into the transparent solution obtained in the step 2), and continuously heating and stirring until the transparent solution becomes transparent sol;
4) drying the transparent sol formed in the step 3) in a vacuum drying oven at 160 ℃ to form xerogel;
5) grinding the xerogel formed in the step 4) and performing dry pressing forming under 4MPa to obtain a cylindrical powder block;
6) calcining the cylindrical powder block obtained in the step 5) at 1650 ℃, and keeping the temperature for 4 h. High entropy (Hf) can be obtained 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 And (3) powder.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A sol-gel preparation method of high-entropy boride nano-powder is characterized by comprising the following steps: the method comprises the following steps:
dissolving Hf source, Nb source, Cr source, Ta source, Mo source, B source and carbon source in organic solvent, and fully dissolving to form transparent solution, wherein the molar ratio of Hf, Nb, Cr, Ta and Mo is 0.1-1:0.1-1:0.1-1:0.1-1:0.1-1, and the molar ratio of the total of transition metals to boron is 1: 2-3;
adding citric acid and ethylene glycol as complexing agents into the transparent solution, and continuously heating and stirring to promote reaction to obtain transparent sol;
drying the transparent sol to obtain dry gel, grinding the dry gel, and calcining to obtain the transparent sol;
each metal source is a chloride of each metal element or an organic precursor; the boron source is boric acid and the carbon source is sorbitol.
2. The sol-gel preparation method of high-entropy boride nanopowder of claim 1, characterized in that: hf. The mol ratio of Nb to Cr to Ta to Mo is 0.2-1:0.2-1:0.2-1:0.2-1: 0.2-1;
preferably, the mole ratio of Hf, Nb, Cr, Ta and Mo is 1:1:1:1: 1.
3. The sol-gel preparation method of high-entropy boride nanopowder of claim 1, characterized in that: the organic solvent is absolute ethyl alcohol.
4. The sol-gel preparation method of high-entropy boride nanopowder of claim 1, characterized in that: continuously stirring in the heating and complexing process;
preferably, the temperature of the complexation reaction is 50-180 ℃.
5. The sol-gel preparation method of high-entropy boride nanopowder of claim 1, characterized in that: the molar ratio of the sum of the transition metals, the boron element and the carbon element in the sorbitol is 1:2-3: 8-12.
6. The sol-gel preparation method of high-entropy boride nanopowder of claim 1, characterized in that: the temperature for drying the transparent sol is 100-300 ℃.
7. The sol-gel preparation method of high-entropy boride nanopowder of claim 1, characterized in that: after the dry gel is ground, the dry gel powder is pressed and formed, and the dry pressed and formed block is calcined;
preferably, the pressure for dry-pressing is 1 to 20 MPa.
8. The sol-gel preparation method of high-entropy boride nanopowder of claim 1, characterized in that: the calcining temperature is 1500-;
preferably, the calcination is carried out in an inert atmosphere, or under vacuum conditions.
9. A high-entropy boride nano-powder is characterized in that: prepared by the sol-gel preparation method of any one of claims 1 to 8.
10. The high entropy boride nanopowder of claim 9 having the formula (Hf) 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 。
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| CN117466649B (en) * | 2023-11-13 | 2024-04-09 | 中国科学院兰州化学物理研究所 | Preparation method of multifunctional high-entropy boride |
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