CN115073183B - 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 Wherein the proportion of the transition metal element 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 excellent 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 grade 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 ultra-high temperature ceramic, has excellent characteristics of high melting point (higher 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. The high entropy transition metal diboride ceramic has more excellent properties, such as higher hardness and better oxidation resistance, than the single component boride ceramic 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 which transition metal atomic layers and boron atomic layers are alternately arranged in the c-axis direction, five transition metal elements randomly occupy sites of the metal atomic layers, the boron atomic layers are combined in a covalent bond manner, and the boron atomic layers are combined with the metal atomic layers in an ionic bond manner. Because of extremely strong chemical bonds, the transition metal diboride high-entropy ceramic has very high melting point and low self-diffusion coefficient, so that the preparation of single-phase powder and the sintering condition of the ceramic are extremely harsh, such as extremely high temperature or extremely high pressure. This makes the preparation of nano high entropy transition metal diboride powder more difficult.
At present, there are many preparation methods of high-entropy transition metal diboride materials, mainly comprising a boron thermal reduction method, a boron/carbon thermal reduction method, a molten salt method, a self-propagating high-temperature sintering method, an SPS direct sintering method, a high-pressure sintering method and the like. However, the particle sizes of the high-entropy transition metal diboride powder prepared by the methods are relatively coarse or only four-component high-entropy boride preparation is reported, and the powder has oxygen impurities and other impurities. The sol-gel method is a liquid phase preparation method capable of efficiently producing nano powder, but the inventor discovers that no research on the sol-gel method preparation of high-entropy transition metal diboride powder exists at present, and no research on the high entropy (Hf) 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 existing in the prior art, the invention aims to provide high-entropy boride nano powder and a sol-gel preparation method thereof. According to the invention, transition metal chloride or organic precursor is used as a metal source, boric acid and sorbitol are respectively used as a boron source and a carbon source, citric acid and ethylene glycol are used as complexing agents, and solid solution of the powder at a lower temperature is realized by regulating and controlling the calcination temperature and the heat preservation time of the powder, so that nano-sized single-phase powder is formed, and the method has good practical application value.
In order to achieve the above object, the present invention is realized by the following technical scheme:
in a first aspect of the present invention, there is provided a high entropy transition metal diboride material having a nominal molecular formula (Hf 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 。
The high-entropy transition metal diboride material has a hexagonal crystal structure, wherein the element proportion in the same position can be regulated and controlled according to actual requirements, the unit cells are formed by alternately stacking transition metal atomic layers and B atomic layers in the direction c, 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 preparing the above high entropy transition metal diboride material, the process comprising:
dissolving a Hf source, a Nb source, a Cr source, a Ta source, a Mo source, a B source and a carbon source in an organic solvent, fully dissolving to form a transparent solution, wherein the molar ratio of Hf, nb, cr, ta to Mo is 0.1-1:0.1-1:0.1-1:0.1-1:0.1-1, and the molar ratio of the sum of transition metals to boron is 1:2-3;
adding citric acid and ethylene glycol into the transparent solution, and continuing to heat and carry out complexation reaction to obtain transparent sol;
drying the transparent sol to obtain xerogel, grinding the xerogel, and calcining to obtain the transparent sol;
each metal source is chloride or organic precursor of each metal element; the boron source is boric acid and the carbon source is sorbitol.
The beneficial effects achieved by one or more embodiments of the present invention described above are as follows:
1) According to the technical scheme, five transition metal chlorides, organic precursors, boric acid powder and sorbitol are taken as raw materials, and the single-phase formation of the 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 high-entropy boride powder with the particle size of nanometer, thus having good practical application value.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 shows the 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 An X-ray diffraction pattern of the powder;
FIG. 2 shows the 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 Scanning electron microscope pictures of the powder.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. 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 present invention. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof. It is to be understood that the scope of the invention is not limited to the specific embodiments described below; it is also to be understood that the terminology used in the examples of the invention is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the invention.
In a first aspect, the present invention provides a sol-gel method for preparing high entropy boride nano powder, comprising the steps of:
dissolving a Hf source, a Nb source, a Cr source, a Ta source, a Mo source, a B source and a carbon source in an organic solvent, fully dissolving to form a transparent solution, wherein the molar ratio of Hf, nb, cr, ta to Mo is 0.1-1:0.1-1:0.1-1:0.1-1:0.1-1, and the molar ratio of the sum of transition metals to boron is 1:2-3;
adding citric acid and ethylene glycol into the transparent solution, and continuing to heat and carry out complexation reaction to obtain transparent sol;
drying the transparent sol to obtain xerogel, grinding the xerogel, and calcining to obtain the transparent sol;
each metal source is chloride or organic precursor of each metal element; the boron source is boric acid and the carbon source is sorbitol.
The reaction is boron carbothermic reduction, and a carbon source is used as a reducing agent.
In some embodiments, the molar ratio of Hf, nb, cr, ta to Mo is 0.2-1:0.2-1:0.2-1:0.2-1:0.2-1;
preferably, the molar ratio of Hf, nb, cr, ta to Mo is 1:1:1:1:1.
In some embodiments, the organic solvent is absolute ethanol.
In some embodiments, agitation is maintained during the heating 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 element, and carbon element in sorbitol is 1:2-3:8-12.
In some embodiments, the transparent sol is dried at a temperature of 100-300 ℃.
In some embodiments, the xerogel is ground and then further comprises the step of dry-compacting the xerogel powder and calcining the dry-compacted mass.
Preferably, the dry press molding is carried out at a pressure of 1 to 20MPa. For example, it may be 1MPa, 2MPa, 3MPa, 4MPa, 5MPa, 6MPa, 7MPa, 8MPa, 9MPa, 10MPa, 11MPa, 12MPa, 13MPa, 14MPa, 15MPa, 16MPa, 17MPa, 18MPa, 19MPa, 20MPa.
Preferably, the calcination temperature is 1500-1800 ℃, the temperature rising rate is 5-8 ℃/min, and the calcination time is 1-5h.
Preferably, the calcination is performed in an inert atmosphere, or under vacuum.
In a second aspect, the invention provides a high entropy boride nano powder prepared by the sol-gel preparation method.
Preferably, the high entropy boride nano powder has a molecular formula of (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 system structure, the unit cells are formed by alternately stacking transition metal atomic layers and B atomic layers in the direction c, 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. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. The following examples are test methods in which specific conditions are noted, and are generally conducted under conventional conditions.
Example 1:
in this example, a nano high entropy (Hf 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 A material. The specific steps are as follows:
1) Weighing raw materials according to a molar ratio of Hf to Nb to Cr to Ta to Mo to B, wherein C=1:1:1:1:1:15:40, respectively weighing hafnium chloride, niobium chloride, chromium chloride, tantalum chloride and molybdenum acetylacetonate, boric acid as a boron source, sorbitol as a carbon source, and weighing 0.003mol of each metal element;
2) Dissolving the raw materials weighed in the step 1) in 40ml of absolute ethyl alcohol, stirring on a magnetic stirring heating table, and heating to 80 ℃ to fully dissolve the raw materials and form transparent solution;
3) Adding 0.02mol of citric acid and 2.5g of ethylene glycol as complexing agents into the transparent solution obtained in the step 2), and continuing heating and stirring until the transparent solution becomes transparent sol;
4) Placing the transparent sol formed in the step 3) in a vacuum drying oven at 130 ℃ for drying to form xerogel;
5) Grinding the xerogel formed in the step 4) and dry-pressing and forming under 2MPa to obtain cylindrical powder blocks;
6) And 5) calcining the cylindrical powder block obtained in the step 5) at 1650 ℃ for 3 hours. The phase information and the microscopic morphology of the obtained nano high-entropy boride powder are respectively referred to an X-ray diffraction pattern and a scanning electron microscope photo shown in fig. 1 and 2.
Example 2:
in this example, a nano high entropy (Hf 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 A material. The specific steps are as follows:
1) Weighing raw materials according to a molar ratio of Hf to Nb to Cr to Ta to Mo to B, wherein C=1:1:1:1:1:15:40, respectively weighing hafnium chloride, niobium chloride, chromium chloride, tantalum chloride and molybdenum acetylacetonate, boric acid as a boron source, sorbitol as a carbon source, and weighing 0.003mol of each metal element;
2) Dissolving the raw materials weighed in the step 1) in 50ml of absolute ethyl alcohol, stirring on a magnetic stirring heating table, and heating to 90 ℃ to fully dissolve the raw materials to form transparent solution;
3) Adding 0.02mol of citric acid and 2.5g of ethylene glycol as complexing agents into the transparent solution obtained in the step 2), and continuing heating and stirring until the transparent solution becomes transparent sol;
4) Placing the transparent sol formed in the step 3) in a vacuum drying oven at 150 ℃ for drying to form xerogel;
5) Grinding the xerogel formed in the step 4) and dry-pressing and forming under 5MPa to obtain cylindrical powder blocks;
6) Calcining the cylindrical powder block obtained in the step 5) at 1700 ℃ for 2 hours. Thus obtaining high entropy (Hf) 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 nano high entropy (Hf 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 A material. The specific steps are as follows:
1) Weighing raw materials according to a molar ratio of Hf to Nb to Cr to Ta to Mo to B to C=1:1:1:1:1:15:38, wherein each metal ion is 0.003mol;
2) Dissolving the raw materials weighed in the step 1) in 45ml of absolute ethyl alcohol, stirring on a magnetic stirring heating table, and heating to 85 ℃ to fully dissolve the raw materials to form transparent solution;
3) Adding 0.02mol of citric acid and 3.0g of ethylene glycol as complexing agents into the transparent solution obtained in the step 2), and continuing heating and stirring until the transparent solution becomes transparent sol;
4) Placing the transparent sol formed in the step 3) in a vacuum drying oven at 160 ℃ for drying to form xerogel;
5) Grinding the xerogel formed in the step 4) and dry-pressing and forming under 4MPa to obtain cylindrical powder blocks;
6) And 5) calcining the cylindrical powder block obtained in the step 5) at 1650 ℃ for 4 hours. Thus obtaining high entropy (Hf) 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 And (3) powder.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A sol-gel preparation method of high-entropy boride nano powder is characterized by comprising the following steps of: the method comprises the following steps:
dissolving a Hf source, a Nb source, a Cr source, a Ta source, a Mo source, a B source and a carbon source in an organic solvent, and fully dissolving to form a transparent solution, wherein the molar ratio of Hf, nb, cr, ta to Mo is 1:1:1; adding citric acid and glycol as complexing agents into the transparent solution, and continuing heating and stirring to promote the reaction to obtain transparent sol;
drying the transparent sol to obtain xerogel, grinding the xerogel, and calcining to obtain the transparent sol;
each metal source is chloride or organic precursor of each metal element; the boron source is boric acid, and the carbon source is sorbitol;
the mole ratio of the sum of the transition metals, boron element and carbon element in sorbitol is 1:2-3:8-12;
the method comprises the steps of grinding xerogel, dry-pressing the xerogel powder to form a block, and calcining the block formed by dry-pressing;
the pressure of dry press molding is 1-20Mpa;
the calcination temperature is 1650-1700 ℃, the temperature rising rate is 5-8 ℃/min, and the calcination time is 1-5h;
the calcination is performed in an inert atmosphere or under vacuum.
2. The sol-gel process for preparing high entropy boride nano-powder according to claim 1, wherein: the organic solvent is absolute ethyl alcohol.
3. The sol-gel process for preparing high entropy boride nano-powder according to claim 1, wherein: stirring continuously in the heating and complexing process;
the temperature of the complexation reaction is 50-180 ℃.
4. The sol-gel process for preparing high entropy boride nano-powder according to claim 1, wherein: the temperature of the transparent sol is 100-300 ℃.
5. The high-entropy boride nano powder is characterized in that: prepared by the sol-gel preparation method of any one of claims 1 to 4.
6. The high-entropy boride nano-powder of claim 5, which has a molecular formula (Hf) 0.2 Nb 0.2 Cr 0.2 Ta 0.2 Mo 0.2 )B 2 。
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| CN110002879A (en) * | 2019-03-22 | 2019-07-12 | 广东工业大学 | A kind of superhard high entropy boride ceramics and its preparation method and application of densification |
| CN110627508A (en) * | 2019-08-28 | 2019-12-31 | 广东工业大学 | High-entropy boride-based ceramic and preparation method and application thereof |
| CN110735076A (en) * | 2019-09-04 | 2020-01-31 | 广东工业大学 | high-entropy metal ceramics and preparation method and application thereof |
| CN111848177A (en) * | 2020-07-08 | 2020-10-30 | 北京理工大学 | Ultrahigh-temperature high-entropy boride ceramic powder and preparation method thereof |
| CN112159234A (en) * | 2020-08-31 | 2021-01-01 | 广东工业大学 | High-entropy ceramic powder and preparation method and application thereof |
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