CN115057709A - High-entropy transition metal diboride and preparation method thereof - Google Patents
High-entropy transition metal diboride and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of preparation of ultrahigh-temperature structural materials, provides a high-entropy transition metal diboride material and a preparation method thereof, and belongs 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 Zr 0.2 Ta 0.2 V 0.2 Nb 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 boron/carbon thermal reduction method adopted by the invention has the advantages of simple process, high production efficiency, low energy consumption and good repeatability, and not only solves the problem of mass production, but also has good practical application value.
Description
Technical Field
The invention belongs to the technical field of preparation of ultra-high temperature structural materials, and particularly relates to a high-entropy transition metal diboride single-phase material and a preparation method thereof.
Background
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The ultra-high temperature ceramic is a ceramic material which has a melting point higher than 3000 ℃ and can be used in a high-temperature environment of 2000 ℃. The transition metal diboride ceramic is one of the important systems of ultrahigh temperature ceramic, has the excellent characteristics of high hardness, high melting point, high conductivity, oxidation resistance, corrosion resistance, high temperature stability and the like, and has wide application prospects in the fields of machining, aerospace, wear-resistant coatings and the like. However, the transition metal boride ceramic is also troubled by the intrinsic brittleness of the ceramic, and with the continuous development of scientific technology, the requirements for the material are gradually increased, the traditional single-component transition metal boride ceramic cannot meet the current requirements, and new materials need to be developed.
The high-entropy effect plays an important role in improving the performance of the material, the high-entropy material has four core effects, namely the high-entropy effect, the delayed diffusion effect, the lattice distortion effect and the cocktail effect, and the four effects endow the high-entropy material with excellent physical and chemical properties such as high hardness, high strength, high-temperature stability, good corrosion resistance and the like. The high entropy transition metal diboride ceramic has superior properties, such as higher hardness and better oxidation resistance, compared to single component boride ceramics. The high-entropy transition metal diboride is formed by alternately arranging transition metal atomic layers and boron atomic layers in the C-axis direction and has AlB 2 A compound of type hexagonal crystal structure (P6/mmm). The components have an important influence on the properties of the high-entropy transition metal diborides.
To date, numerous scholars have explored the composition and mechanical properties of high entropy transition metal diborides. It has been found that high entropy transition metal diborides tend to have excellent stability and ultra-high hardness, such as high entropy ceramics (Ta) 0.2 Nb 0.2 Zr 0.2 Cr 0.2 Ti 0.2 )B 2 And (Ta) 0.167 Nb 0.167 Zr 0.167 Hf 0.167 Ti 0.167 Cr 0.167 )B 2 Can keep phase stability under the ultrahigh pressure of 0-52.7GPa, (Cr) 0.2 Hf 0.2 Ta 0.2 Ti 0.2 Zr 0.2 )B 2 The hardness was measured at a load of 0.49N to be 48.3. + -. 2.3 GPa. The high-entropy transition metal diboride with different components often shows larger difference in microstructure and performance, so that the regulation and control of the performance of the high-entropy transition metal diboride material system through component adjustment have important significance. However, the high-performance high-entropy transition metal diboride and the preparation method thereof still need to be researched.
Disclosure of Invention
In order to overcome the above technical problems, the present invention provides (Hf) 0.2 Zr 0.2 Ta 0.2 V 0.2 Nb 0.2 )B 2 The high entropy transition metal diboride material of (1). The invention takes metal oxide powder, boron carbide and carbon powder as raw materials, realizes solid solution at lower temperature by regulating and controlling the proportion and the mixing mode of precursors, forms single-phase powder, and has good value in practical application.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the invention there is provided a high entropy transition metal diboride having a nominal formula of (Hf) 0.2 Zr 0.2 Ta 0.2 V 0.2 Nb 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 method for preparing a high-entropy transition metal diboride, comprising:
to mix HfO 2 、ZrO 2 、Ta 2 O 5 、V 2 O 5 、Nb 2 O 5 Boron carbide powder and carbon powder according to the nominal chemical formula (Hf) of the high-entropy transition metal diboride material 0.2 Zr 0.2 Ta 0.2 V 0.2 Nb 0.2 )B 2 Determining the dosage and weighing for later use;
carrying out wet ball milling on the powder to obtain slurry;
and drying and calcining the slurry to obtain the catalyst.
The invention has the advantages of
(1) According to the technical scheme, five kinds of metal oxide powder, boron carbide powder and carbon powder are used as raw materials, and through ball milling treatment and calcination, the in-situ generation and solid solution diffusion of diboride are realized. The obtained high-entropy transition metal diboride material has the advantages of high purity, small particle size and uniform element distribution;
(2) the preparation method provided by the technical scheme selects the boron/carbon thermal reduction method, has simple process and high production efficiency, solves the problem of mass production, and has low energy consumption and good repeatability, thereby having good practical application value.
(3) The preparation method is simple, strong in practicability and easy to popularize.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
FIG. 1 is a scanning electron micrograph of a ball-milled precursor prepared in example 1 of the present invention;
FIG. 2 is an X-ray diffraction pattern of a high entropy transition metal diboride material prepared according to example 1 of the present invention;
FIG. 3 is a scanning electron micrograph of the high entropy transition metal diboride material prepared in example 1 of the present invention.
FIG. 4 is an X-ray diffraction pattern of a high entropy transition metal diboride material prepared according to example 2 of the present invention;
FIG. 5 is a scanning electron micrograph of a high-entropy transition metal diboride material prepared according to example 2 of the present invention; wherein (a) the magnification is 5000 times; (b) the magnification is 50000 times.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. 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 application belongs.
As mentioned above, there is currently no high entropy (Hf) 0.2 Zr 0.2 Ta 0.2 V 0.2 Nb 0.2 )B 2 Research and report on the preparation of phase powder.
In view of the above, the present invention provides a composition of (Hf) 0.2 Zr 0.2 Ta 0.2 V 0.2 Nb 0.2 )B 2 The high-entropy transition metal diboride material and the preparation method thereof have the characteristics of rich raw material sources, simple process, flexible operation process and the like.
In particular, in one exemplary embodiment of the invention, a high entropy transition metal diboride material is provided having a nominal formula of (Hf) 0.2 Zr 0.2 Ta 0.2 V 0.2 Nb 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, and a unit cell is formed by alternately stacking transition metal atomic layers and B atomic layers in the c direction.
In another embodiment of the present invention, the molar ratio of the five transition metals may be 0.1-1: 0.1-1; preferably 1:1:1:1: 1.
In another embodiment of the present invention, there is provided a method for preparing the high-entropy transition metal diboride material described above, the method comprising:
s1, determining the required amount of powder containing each element according to the stoichiometric ratio of each element in the nominal chemical formula of the high-entropy transition metal diboride material, wherein the powder comprises five kinds of metal oxide powder, boron carbide powder and carbon powder;
s2, ball-milling and mixing the six kinds of powder in the step S1, and adding 5-15ml of absolute ethyl alcohol as a medium to carry out wet milling;
s3, drying and dry-pressing the slurry mixed in the step S2;
s4, calcining the powder in the step S3.
In another embodiment of the present invention, in step S1, the molar ratio of the total of the five transition metal elements to the boron carbide and the carbon powder is 10:5 to 6:18 to 19 or 10:7.6 to 9: 0;
in another embodiment of the present invention, in step S2, in order to facilitate the mixing, absolute ethanol or other organic liquid may be used as the ball milling medium;
in another embodiment of the present invention, in step S2, the ball milling rotation speed is 700 to 1200rmp, the ball milling time is 3 to 8 hours, and the ball-to-material ratio is 3 to 6: 1;
sintering is carried out under a protective atmosphere (such as argon) or under vacuum conditions, and the sintering treatment conditions comprise: the sintering temperature is controlled to be 1550-1650 ℃, and the sintering time is 1-3 h.
In another embodiment of the present invention, the preparation method further comprises the step of simply grinding the product (loose block) obtained after the calcination in the step S4 to obtain the high-entropy transition metal diboride material.
The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
Example 1:
in this example, a high entropy transition metal diboride material was prepared. The method comprises the following specific steps:
1) according to a molar ratio HfO 2 :ZrO 2 :Ta 2 O 5 :V 2 O 5 :Nb 2 O 5 :B 4 Preparing powder from C, 2:1.85:1:1: 1.5: 18;
2) ball-milling and mixing all the powder in the step 1), adding 10ml of absolute ethyl alcohol as a medium, and carrying out wet milling, wherein the ball-milling rotation speed is 800rmp, the ball-milling time is 5 hours, and the ball-material ratio is 3: 1;
3) placing the mixed slurry obtained in the step 2) in a culture dish, and drying for 12 hours in a drying oven at 50 ℃;
4) dry-pressing the powder obtained in the step 3), placing the powder in a corundum crucible, heating to 1600 ℃ at the heating speed of 5 ℃/min under the Ar atmosphere, keeping the temperature for 2.5 hours, and cooling along with the furnace;
5) grinding the calcined powder in the step 4) for characterization.
The obtained micro-morphology of the ball-milled precursor, and the phase structure and the micro-morphology of the calcined high-entropy transition metal diboride material refer to a scanning electron micrograph, an X-ray diffraction pattern and a scanning electron micrograph shown in FIGS. 1, 2 and 3, respectively.
Example 2:
in this example, a high entropy transition metal diboride material was prepared. The method comprises the following specific steps:
1) according to a molar ratio HfO 2 :ZrO 2 :Ta 2 O 5 :V 2 O 5 :Nb 2 O 5 :B 4 C, preparing powder from 2:1.9:1:1:1:1.5.25: 18;
2) ball-milling and mixing all the powder in the step 1), adding 9ml of absolute ethyl alcohol as a medium, and carrying out wet milling, wherein the ball-milling rotation speed is 800rmp, the ball-milling time is 4 hours, and the ball-material ratio is 3: 1;
3) placing the mixed slurry obtained in the step 2) in a culture dish, and drying for 14 hours in a drying oven at 50 ℃;
4) dry-pressing the powder obtained in the step 3) to form, placing the powder in a corundum crucible, heating to 1600 ℃ at a heating rate of 5 ℃/min under an Ar atmosphere, preserving heat for 2 hours, and then cooling along with the furnace;
5) grinding the calcined powder in the step 4) for characterization.
The phase structure and the microstructure of the obtained high-entropy transition metal diboride material refer to an X-ray diffraction spectrum and a scanning electron microscope photo shown in FIGS. 4 and 5 respectively.
Example 3:
in this example, a high entropy transition metal diboride material was prepared. The method comprises the following specific steps:
1) according to a molar ratio HfO 2 :ZrO 2 :Ta 2 O 5 :V 2 O 5 :Nb 2 O 5 :B 4 Preparing powder from C, 2:1.88:1:1:1:1.5: 18;
2) ball-milling and mixing all the powder in the step 1), adding 12ml of absolute ethyl alcohol as a medium, and carrying out wet milling, wherein the ball-milling rotation speed is 900rmp, the ball-milling time is 4 hours, and the ball-material ratio is 3: 1;
3) placing the mixed slurry obtained in the step 2) in a culture dish, and drying for 14 hours in a drying oven at 50 ℃;
4) dry-pressing the powder obtained in the step 3) to form, placing the powder in a corundum crucible, heating to 1650 ℃ at a heating rate of 5 ℃/min under the Ar atmosphere, preserving heat for 1.5h, and cooling along with the furnace;
5) and (5) grinding the calcined powder in the step 4) for characterization.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. A high entropy transition metal diboride having a nominal molecular formula of (Hf) 0.2 Zr 0.2 Ta 0.2 V 0.2 Nb 0.2 )B 2 。
2. A preparation method of high-entropy transition metal diboride is characterized by comprising the following steps:
to mix HfO 2 、ZrO 2 、Ta 2 O 5 、V 2 O 5 、Nb 2 O 5 Boron carbide powder and carbon powder according to the nominal chemical formula (Hf) of the high-entropy transition metal diboride material 0.2 Zr 0.2 Ta 0.2 V 0.2 Nb 0.2 )B 2 Determining the dosage and weighing for later use;
carrying out wet ball milling on the powder to obtain slurry;
and drying and calcining the slurry to obtain the catalyst.
3. The method of producing a high-entropy transition metal diboride according to claim 2, wherein HfO 2 、ZrO 2 、Ta 2 O 5 、V 2 O 5 、Nb 2 O 5 The molar ratio of (A) to (B) is 0.1-1: 0.1-1.
4. The method for producing a high-entropy transition metal diboride according to claim 2, wherein the molar ratio of the total of transition metal elements to boron carbide and carbon powder is 10:5 to 6:18 to 19 or 10:7.6 to 9: 0.
5. A method for producing a high-entropy transition metal diboride compound as claimed in claim 2, wherein the medium of the wet ball milling is absolute ethanol;
or the volume of the ball milling medium is 5-15 ml.
6. The method for preparing a high-entropy transition metal diboride according to claim 2, wherein the rotation speed of the wet ball milling is 700-1200 rmp, the ball milling time is 3-8 hours, and the ball-to-material ratio is 3-6: 1.
7. A process for the preparation of a high entropy transition metal diboride compound according to claim 2 wherein the drying time is from 6 to 15 hours.
8. A method for producing a high-entropy transition metal diboride compound according to claim 2, wherein after the drying treatment, the dry-pressing is performed, followed by calcination.
9. A method for producing a high-entropy transition metal diboride according to claim 2, wherein the calcination is carried out under inert atmosphere or vacuum conditions.
10. The method for preparing a high-entropy transition metal diboride according to claim 2, wherein the sintering temperature is controlled to 1550 ℃ to 1650 ℃, the temperature rise rate is 5 ℃/min to 8 ℃/min, and the sintering time is 1 h to 3 h.
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