CN114163232A - Single crystal high-entropy ceramic powder and preparation method thereof - Google Patents

Single crystal high-entropy ceramic powder and preparation method thereof Download PDF

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CN114163232A
CN114163232A CN202111526884.0A CN202111526884A CN114163232A CN 114163232 A CN114163232 A CN 114163232A CN 202111526884 A CN202111526884 A CN 202111526884A CN 114163232 A CN114163232 A CN 114163232A
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ceramic powder
entropy ceramic
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董红英
韩欣欣
马文
郝家京
赵敏
刘璐
王少琨
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Inner Mongolia University of Technology
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Abstract

The invention discloses a single crystal high-entropy ceramic powder and a preparation method thereof, wherein the powder has a hollow spherical structure and a chemical formula A2B2O7The A site is trivalent rare earth element, the B site is tetravalent metal element; the trivalent rare earth element is lanthanum, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, ytterbium, yttrium or lutetium; the tetravalent metal element is titanium, cerium, tin, zirconium or hafnium. The preparation method comprises the following steps: step A: mixing nitrate of trivalent rare earth elements and acetate of tetravalent metal elements to obtain mixed solid powder; and B: adding deionized water into the mixed solid powder, and uniformly stirring to obtain a mixed dispersion system; and C: filtering the mixed dispersion system by using a standard sieve to remove undissolved impurities to obtain a mixed solution; step D: and uniformly spraying the mixed solution into water by using a three-electrode plasma spray gun, and performing centrifugal drying after naturally settling the mixed solution sprayed into the water. The preparation method of the invention has simple operation, and the prepared powder is relativelyUniform and not easy to agglomerate.

Description

Single crystal high-entropy ceramic powder and preparation method thereof
Technical Field
The invention relates to the technical field of single crystal high-entropy ceramic preparation. In particular to single crystal high-entropy ceramic powder and a preparation method thereof.
Background
The high-entropy ceramic is a new concept which introduces a high-entropy theory into the field of inorganic nonmetal on the basis of the research of high-entropy alloy, and is generally formed by solid solution of a plurality of components in an equal proportion or a nearly equal proportion, wherein a system in which the solid solution is carried out in a five-component equal proportion mode is more. Because the high-entropy ceramic material shows huge dielectric constant, ultrafast ion conductor ability, good catalytic performance and excellent capacity retention, the high-entropy ceramic material is expected to be used for catalysts and secondary batteries and improves related performance, and in addition, the high entropy ceramic material is also favorable for improving the oxidation resistance of carbide ceramic, and the mechanical property of the high-entropy non-oxide ceramic is excellent [ Chenkexi, Li Zi, Majinxu, the research progress and prospect of the high-entropy ceramic material ], and the research significance of the high-entropy ceramic material is profound.
The preparation method of the high-entropy ceramic powder has various methods, including a solid-phase synthesis method, a sol-gel method, a chemical coprecipitation method, a hydrothermal reaction method and a combustion method, and the methods have advantages and disadvantages respectively. The nano original powder prepared by the combustion method is easy to generate serious agglomeration due to large specific surface area; the chemical coprecipitation method has the advantages that the reaction temperature is low, the obtained powder has small particle size and uniform components and performance, and is suitable for mass production, and the defects that the powder is easy to agglomerate in the washing, filtering and drying processes and even the dispersibility of the powder is poor; the hydrothermal reaction method has the defects that the yield is too low and the requirement of industrial production is difficult to meet; the powder prepared by the sol-gel method has small particle size and controllable components, but the preparation process consumes longer time and has higher raw material cost, and the powder is difficult to be used for batch production; the solid-phase synthesis method is the most common method for preparing high-entropy powder, the synthesis steps are simpler, the cost is low, the process is simple, the powder is free from agglomeration, the filling property is good, but the prepared powderUneven particle size distribution, slow reaction rate, large powder particle size, easy impurity mixing, severe component segregation and the like, which also affects sintering of ceramic blocks pressed with the powder. Vacuum sintering for the purpose of solving the problem of serious agglomeration of powder (Zengjian Jun, Zkuibao, Chendaimeng, etc.)0.2Nd0.2Sm0.2Gd0.2Er0.2)2Zr2O7High-entropy transparent ceramics, inorganic materials science and newspaper, and the high-entropy transparent ceramics is prepared by combining a combustion method with vacuum sintering.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a single crystal high-entropy ceramic powder with a hollow spherical structure; the method adopts a plasma spraying process to prepare the ceramic powder with the hollow spherical structure, and the preparation method is simple; solves the problems of easy agglomeration, irregular shape, easy impurity mixing, uneven distribution and the like of the high-entropy ceramic powder prepared by the prior process.
In order to solve the technical problems, the invention provides the following technical scheme:
a single crystal high-entropy ceramic powder has a hollow spherical structure and a chemical formula A2B2O7The A site is trivalent rare earth element, the B site is tetravalent metal element; the trivalent rare earth element is lanthanum, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, ytterbium, yttrium or lutetium; the tetravalent metal element is titanium, cerium, tin, zirconium or hafnium. The hollow spherical structure can reduce the density and the thermal conductivity of the single crystal high-entropy ceramic, can be used as a candidate material of a thermal barrier coating, can also be applied to the fields of catalysts, secondary batteries and the like, and has a spatial structure for improving the thermoelectric performance of the single crystal high-entropy ceramic used for thermoelectric materials.
In the single crystal high-entropy ceramic powder, the A site is composed of 5-7 trivalent rare earth elements. In a high-entropy system, the atomic size of each component is different or the number of main elements is too large, so that the internal crystal lattice of the high-entropy ceramic material is seriously distorted and generates a second phase, and the distortion is more serious when the atomic size difference of each component is larger. At present, the radius sizes of the selected trivalent rare earth elements are similar, and when the types of the rare earth elements are 5-7, a stable high-entropy system can be obtained, and the occurrence of lattice distortion can be avoided to the greatest extent.
The chemical formula of the single crystal high-entropy ceramic powder is (Me 1)aMe2bMe3cMe4dMe5e)2B2O7A + b + c + d + e is 1 and a is c is d; me1, Me2, Me3, Me4 and Me5 are all one of lanthanum, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, ytterbium, yttrium or lutetium, and Me1, Me2, Me3, Me4 and Me5 are different from each other.
The chemical formula of the single crystal high-entropy ceramic powder is (Me 1)aMe2bMe3cMe4dMe5eMe6f)2B2O7A + b + c + d + e + f is 1 and a is c is d is e is f; me1, Me2, Me3, Me4, Me5 and Me6 are all one of lanthanum, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, ytterbium, yttrium or lutetium, and Me1, Me2, Me3, Me4, Me5 and Me6 are different from each other.
The chemical formula of the single crystal high-entropy ceramic powder is (Me 1)aMe2bMe3cMe4dMe5eMe6fMe7g)2B2O7A + b + c + d + e + f + g is 1 and a-b-c-d-e-f-g; me1, Me2, Me3, Me4, Me5, Me6 and Me7 are all one of lanthanum, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, ytterbium, yttrium or lutetium, and Me1, Me2, Me3, Me4, Me5, Me6 and Me7 are different from each other.
A preparation method of single crystal high-entropy ceramic powder is characterized by comprising the following steps:
step A: mixing a nitrate solution of a trivalent rare earth element and an acetate solution of a tetravalent metal element to obtain a mixed dispersion system A; the selection of the types of the salts of the trivalent rare earth elements and the tetravalent metal elements has a direct influence on the performance of the single crystal high-entropy ceramic powder, and if the unsuitable salts are selected as raw materials, impurity ions can be introduced, so that the generation of a second phase is caused, and the performance of the prepared single crystal high-entropy ceramic powder is further influenced. The invention selects nitrate as trivalent diluentThe reason for the earth element salt is: NO at high temperature during spraying3 -The solution is changed into gas to volatilize, new ions can not be introduced, but if the solution is changed into sulfate and chloride, ions in the solution are difficult to volatilize, so that impurity ions exist in the single crystal high-entropy ceramic powder, and the powder performance is influenced. Acetate was chosen as the tetravalent metal salt because: the acetate solution is an organic solution, can play a good slow release role in the spraying process, and if nitrate is selected, powder with a uniform structure and a hollow spherical structure can not be obtained due to violent reaction in the spraying process.
And B: adding deionized water into the mixed dispersion system A, and uniformly stirring to obtain a mixed dispersion system B;
and C: filtering the mixed dispersion system B by using a standard sieve to remove undissolved impurities to obtain a mixed dispersion system C;
step D: uniformly spraying the mixed dispersion system C into water by using a three-electrode plasma spray gun, and centrifugally drying after naturally settling liquid drops sprayed into the water to obtain the single-crystal high-entropy ceramic powder with the hollow spherical structure; the chemical formula of the single crystal high-entropy ceramic powder is A2B2O7The A site is trivalent rare earth element, the B site is tetravalent metal element; the trivalent rare earth element is lanthanum, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, ytterbium, yttrium or lutetium; the tetravalent metal element is titanium, cerium, tin, zirconium or hafnium.
In the preparation method of the single-crystal high-entropy ceramic powder, in the step C, the dynamic viscosity of the mixed dispersion system C is 4.00-9.00 mPa.s, and the surface tension is 40.00-60.00 mN/m. Too low dynamic viscosity is not beneficial to the formation of single crystal high-entropy ceramic powder particles, and too high viscosity can affect normal liquid conveying. In addition, the surface tension of the solution can influence the atomization and crushing mechanism of the liquid drops in the spray gun, so that the structure of the powder is influenced, larger liquid drops can be obtained due to larger surface tension, the liquid drops can enter a high-temperature area of the plasma arc, but the insufficient heat obtained by the liquid drops can be caused, so that small lath crystals cannot be formed; in the experiment, the invention discovers that when the dynamic viscosity of the mixed dispersion system C is 4.00-9.00 mPa.s and the surface tension is 40.00-60.00 mN/m, the prepared single crystal high-entropy ceramic powder has small particle size, good particle size uniformity and regular shape, and the powder particles are not easy to agglomerate.
In the step D, the power of the spray gun is 70-120 kW, and the liquid conveying speed is 20-70 mL/min. The spray gun is operated by delivering the mixed dispersion C to an atomizing nozzle through a liquid delivery device, atomizing the liquid into fine particles under gas pressure at a suitable power, and solidifying into a phase after undergoing a series of physical and chemical changes in an arc, such as evaporation, decomposition, precipitation, pyrolysis, sintering, and melting. The power of the spray gun has a certain influence on the structure of the powder, when the power is too low, part of the solution does not reach the molten state, so that the delivered droplets cannot be solidified to the best structure and particle size, and when the power is too high, the solution can reach the molten state too quickly, so that the components in the mixed dispersion system C cannot react sufficiently and are aggregated.
In the preparation method of the single crystal high-entropy ceramic powder, in the step A, 5-7 kinds of nitrates of trivalent rare earth elements are used, and the molar ratio of the 5-7 kinds of nitrates of trivalent rare earth elements is 1: 1.
In the preparation method of the single crystal high-entropy ceramic powder, in the step C, the standard sieve is 325 meshes or 400 meshes. The mesh opening of the 325-mesh standard sieve is 0.0450mm, and the mesh opening of the 400-mesh standard sieve is 0.0374 mm. The reason for selecting the standard screen of 325 mesh or 400 mesh is: the filtering effect of the mixed dispersion system can influence the structure and the particle size of the prepared powder, if the filtering effect is not carried out or the aperture size for filtering is larger than 0.0450mm, impurities exist in the mixed dispersion system, the spraying effect of the spray gun is obviously influenced, the uniformity of the prepared powder particles is poor, and the structure is not ideal.
The technical scheme of the invention achieves the following beneficial technical effects:
the invention uses nitrate of each rare earth oxide to prepare solution according to equal molar ratio to mix with acetate solution of tetravalent metal element, and keeps the surface tension and dynamic viscosity of the mixed solution in a proper specific range, sprays into water at a specific speed by plasma spraying, then separates liquid and powder by natural sedimentation, centrifugation and drying, the single crystal high entropy ceramic powder prepared by the method has a uniform hollow spherical structure, and the hollow rate of the powder particles is 8% -15% (the hollow rate is the volume of the hollow part of the hollow spherical structure powder accounts for the total volume of the whole hollow spherical structure powder). The density of the high-entropy ceramic block and the coating prepared by the single-crystal high-entropy ceramic powder with the hollow spherical structure can be reduced to a certain degree, so that the thermal conductivity of the block or the coating is effectively reduced. The preparation method provided by the invention is simple to operate, and the prepared powder is relatively uniform and is not easy to agglomerate.
Drawings
FIG. 1A single-crystal high-entropy ceramic powder (La) prepared in example 1 of the present invention1/5Sm1/5Gd1/5Nd1/5Yb1/5)2Zr2O7XRD pattern of (a);
FIG. 2 shows single crystal high entropy ceramic powder (La) prepared in example 1 of the present invention1/5Sm1/5Gd1/5Nd1/5Yb1/5)2Zr2O7TEM image of (1 μm);
FIG. 3 shows single crystal high entropy ceramic powder (La) prepared in example 1 of the present invention1/5Sm1/5Gd1/5Nd1/5Yb1/5)2Zr2O7HRTEM image of (A);
FIG. 4 shows single crystal high entropy ceramic powder (La) prepared in example 1 of the present invention1/5Sm1/5Gd1/5Nd1/5Yb1/5)2Zr2O7The SAED pattern of (A);
FIG. 5 Single-crystal high-entropy ceramic powder (La) prepared in example 1 of the present invention1/5Sm1/5Gd1/5Nd1/5Yb1/5)2Zr2O7SEM image (2 μm);
FIG. 6A single-crystal high-entropy ceramic powder (La) prepared in example 1 of the present invention1/5Sm1/5Gd1/5Nd1/5Yb1/5)2Zr2O7SEM image (4 μm);
FIG. 7 Single-crystal high-entropy ceramic powder (La) prepared in example 1 of the present invention1/5Sm1/5Gd1/5Nd1/5Yb1/5)2Zr2O7The distribution curve of the particle size of (2).
Since the single-crystal high-entropy ceramic powders prepared in examples 2 to 6 and example 1 have similar structures, the structures of the powders in examples 2 to 6 are not further characterized.
Detailed Description
Example 1
In this example, the chemical formula of the single crystal high entropy ceramic powder is (La)1/5Sm1/5Gd1/5Nd1/5Yb1/5)2Zr2O7(ii) a The preparation method comprises the following steps:
step A: adding La (NO)3)3·6H2O、Sm(NO3)3·6H2O、Gd(NO3)3·6H2O、Nd(NO3)3·6H2O and Yb (NO)3)3·6H2Fully mixing O five nitrates according to the molar ratio of 1:1:1:1:1, adding a proper amount of deionized water for dissolving to obtain a mixed nitrate solution, and then mixing the mixed nitrate solution with Zr (CH)3COO)4Mixing the solutions to obtain a mixed dispersion system A; in the mixed dispersion A, Zr (CH)3COO)4And La (NO)3)3·6H2The molar ratio of O is 5: 1;
and B: adding a proper amount of deionized water into the mixed dispersion system A, and uniformly stirring to obtain a mixed dispersion system B;
and C: filtering the mixed dispersion system B by using a standard sieve to remove undissolved impurities to obtain a mixed dispersion system C; the standard sieve is 325 meshes, and the size of the sieve pore is 0.0450 mm; in the step B, the addition amount of water is such that the dynamic viscosity of the mixed dispersion system C is within the range of 4.00-9.00 mPa · s, and the surface tension is within the range of 40.00-60.00 mN/m; in this example, the dynamic viscosity of the mixed dispersion C was measured to be 7.69 mPas by a viscometer, and the surface tension thereof was measured to be 52.46mN/m by a surface tension meter;
step D: and (3) uniformly spraying the mixed dispersion system C into water by using a three-electrode plasma spray gun, wherein the power of the spray gun is 90kW, and the liquid drop sprayed into the water at the liquid delivery rate of 24 mL/min is subjected to natural sedimentation and centrifugal drying to obtain the single crystal high-entropy ceramic powder with the hollow spherical structure.
The distribution of the particle sizes of the powder prepared by the embodiment is shown in fig. 7, and it can be seen from the figure that the median particle size of the powder particles is between 0.6 and 0.7 μm, and the proportion of the slurry powder particles with the particle size of less than 2.5 μm reaches 82.12%; fig. 1 shows that the powder prepared in this example is a target product, fig. 2 and fig. 3 show that the powder prepared in this example does not have an agglomeration phenomenon, and fig. 4 shows that the powder prepared in this example by using a plasma process is a single crystal. The average particle diameter of the powder prepared in this example was 0.631. mu.m, and the average porosity of the powder was 9%. The preparation method of the embodiment shows that no agglomeration phenomenon occurs in the powder prepared by the preparation method, the prepared powder has a regular hollow spherical structure (see fig. 5 and 6), and the uniformity is good, and the powder with the hollow spherical structure can be used for preparing a high-entropy ceramic block or coating, thereby being beneficial to reducing the density and the thermal conductivity of the high-entropy ceramic block or coating to a certain extent.
Example 2
In this example, the chemical formula of the single crystal high entropy ceramic powder is (La)1/5Sm1/5Gd1/5Nd1/5Eu1/5)2Zr2O7(ii) a The preparation method comprises the following steps:
step A: adding La (NO)3)3·6H2O、Sm(NO3)3·6H2O、Gd(NO3)3·6H2O、Nd(NO3)3·6H2O and Eu (NO)3)3·6H2Fully mixing O five nitrates according to the molar ratio of 1:1:1:1:1, adding a proper amount of deionized water for dissolving to obtain a mixed nitrate solution, and then mixing the mixed nitrate solution with Zr (CH)3COO)4Mixing the solutions to obtain a mixed dispersion system A; mixingIn dispersion A, Zr (CH)3COO)4And La (NO)3)3·6H2The molar ratio of O is 5: 1;
and B: adding a proper amount of deionized water into the mixed dispersion system A, and uniformly stirring to obtain a mixed dispersion system B;
and C: filtering the mixed dispersion system B by using a standard sieve to remove undissolved impurities to obtain a mixed dispersion system C; the standard sieve is 400 meshes, and the size of the sieve pore is 0.0374 mm; in the step B, the addition amount of water is such that the dynamic viscosity of the mixed dispersion system C is within the range of 4.00-9.00 mPa · s, and the surface tension is within the range of 40.00-60.00 mN/m; in this example, the dynamic viscosity of the mixed dispersion system C was measured by a viscometer to be 5.24 mPas, and the surface tension thereof was measured by a surface tension meter to be 46.99 mN/m;
step D: and (3) uniformly spraying the mixed dispersion system C into water by using a three-electrode plasma spray gun, wherein the power of the spray gun is 100kW, the liquid drop sprayed into the water at the liquid delivery rate of 50 mL/min is naturally settled and then centrifugally dried, and the single-crystal high-entropy ceramic powder with the hollow spherical structure is obtained, wherein the average particle size of the powder is 0.772 mu m, and the average hollow rate of the powder is 11%.
Example 3
In this example, the chemical formula of the single crystal high entropy ceramic powder is (La)1/6Sm1/6Gd1/6Nd1/6Eu1/6Yb1/6)2Zr2O7(ii) a The preparation method comprises the following steps:
step A: adding La (NO)3)3·6H2O、Sm(NO3)3·6H2O、Gd(NO3)3·6H2O、Nd(NO3)3·6H2O、Eu(NO3)3·6H2O and Yb (NO)3)3·6H2Fully mixing six nitrates O according to the molar ratio of 1:1:1:1:1:1, adding a proper amount of deionized water to dissolve the mixed nitrates to obtain a mixed nitrate solution, and then mixing the mixed nitrate solution with Zr (CH)3COO)4Mixing the solutions to obtain a mixed dispersion system A; in the mixed dispersion A, Zr (CH)3COO)4And La (NO)3)3·6H2The molar ratio of O is 6: 1;
and B: adding a proper amount of deionized water into the mixed dispersion system A, and uniformly stirring to obtain a mixed dispersion system B; (ii) a
And C: filtering the mixed dispersion system B by using a standard sieve to remove undissolved impurities to obtain a mixed dispersion system C; the standard sieve is 325 meshes, and the size of the sieve pore is 0.0450 mm; in the step B, the addition amount of water is such that the dynamic viscosity of the mixed dispersion system C is within the range of 4.00-9.00 mPa · s, and the surface tension is within the range of 40.00-60.00 mN/m; in this example, the dynamic viscosity of the mixed dispersion C was measured by a viscometer to be 7.85 mPas, and the surface tension thereof was measured by a surface tension meter to be 55.73mN/m
Step D: and (3) uniformly spraying the mixed dispersion system C into water by using a three-electrode plasma spray gun, wherein the power of the spray gun is 80kW, the liquid drop sprayed into the water at the liquid delivery rate of 35 mL/min is naturally settled and then centrifugally dried, and the single-crystal high-entropy ceramic powder with a hollow spherical structure is obtained, wherein the average particle size of the powder is 0.696 mu m, and the average hollow rate of the powder is 12%.
Example 4
In this example, the chemical formula of the single crystal high entropy ceramic powder is (La)1/6Sm1/6Gd1/6Nd1/6Eu1/6Er1/6)2Zr2O7(ii) a The preparation method comprises the following steps:
step A: adding La (NO)3)3·6H2O、Sm(NO3)3·6H2O、Gd(NO3)3·6H2O、Nd(NO3)3·6H2O、Eu(NO3)3·6H2O and Er (NO)3)3·6H2Fully mixing six nitrates O according to the molar ratio of 1:1:1:1:1:1, adding a proper amount of deionized water to dissolve the mixed nitrates to obtain a mixed nitrate solution, and then mixing the mixed nitrate solution with Zr (CH)3COO)4Mixing the solutions to obtain a mixed dispersion system A; in the mixed dispersion A, Zr (CH)3COO)4And La (NO)3)3·6H2The molar ratio of O is 6: 1;
and B: adding a proper amount of deionized water into the mixed dispersion system A, and uniformly stirring to obtain a mixed dispersion system B;
and C: filtering the mixed dispersion system B by using a standard sieve to remove undissolved impurities to obtain a mixed dispersion system C; the standard sieve is 325 meshes, and the size of the sieve pore is 0.0450 mm; in the step B, the addition amount of water is such that the dynamic viscosity of the mixed dispersion system C is within the range of 4.00-9.00 mPa · s, and the surface tension is within the range of 40.00-60.00 mN/m; in this example, the dynamic viscosity of the mixed dispersion C was measured to be 6.28 mPas by a viscometer, and the surface tension thereof was measured to be 47.61mN/m by a surface tension meter;
step D: and (3) uniformly spraying the mixed dispersion system C into water by using a three-electrode plasma spray gun, wherein the power of the spray gun is 110kW, the liquid drop sprayed into the water at the liquid delivery rate of 40 mL/min is naturally settled and then centrifugally dried, and the single-crystal high-entropy ceramic powder with the hollow spherical structure is obtained, wherein the average particle size of the powder is 0.734 mu m, and the average hollow rate of the powder is 15%.
Example 5
In this example, the chemical formula of the single crystal high entropy ceramic powder is (La)1/7Sm1/7Gd1/7Nd1/7Eu1/7Yb1/7Er1/7)2Zr2O7(ii) a The preparation method comprises the following steps:
step A: adding La (NO)3)3·6H2O、Sm(NO3)3·6H2O、Gd(NO3)3·6H2O、Nd(NO3)3·6H2O、Eu(NO3)3·6H2O、Yb(NO3)3·6H2O and Er (NO)3)3·6H2Fully mixing seven nitrates of O according to the molar ratio of 1:1:1:1:1:1:1, adding a proper amount of deionized water to dissolve the mixed nitrates to obtain a mixed nitrate solution, and then mixing the mixed nitrate solution with Zr (CH)3COO)4Mixing the solutions to obtain a mixed dispersion system A; in the mixed dispersion A, Zr (CH)3COO)4And La (NO)3)3·6H2The molar ratio of O is 7: 1;
and B: adding a proper amount of deionized water into the mixed dispersion system A, and uniformly stirring to obtain a mixed dispersion system B;
and C: filtering the mixed dispersion system B by using a standard sieve to remove undissolved impurities to obtain a mixed dispersion system C; the standard sieve is 325 meshes, and the size of the sieve pore is 0.0450 mm; in the step B, the addition amount of water is such that the dynamic viscosity of the mixed dispersion system C is within the range of 4.00-9.00 mPa · s, and the surface tension is within the range of 40.00-60.00 mN/m; in this example, the dynamic viscosity of the mixed dispersion C was measured to be 8.87 mPas by a viscometer, and the surface tension thereof was measured to be 57.98mN/m by a surface tension meter;
step D: and (3) uniformly spraying the mixed dispersion system C into water by using a three-electrode plasma spray gun, wherein the power of the spray gun is 120kW, the liquid drop sprayed into the water at a liquid delivery rate of 50 mL/min is naturally settled and then centrifugally dried, and the single-crystal high-entropy ceramic powder with a hollow spherical structure is obtained, wherein the average particle size of the powder is 0.605 mu m, and the average hollow rate of the powder is 8%.
Example 6
In this example, the chemical formula of the single crystal high entropy ceramic powder is (La)1/7Sm1/7Gd1/7Nd1/7Eu1/7Y1/7Er1/7)2Zr2O7(ii) a The preparation method comprises the following steps:
step A: adding La (NO)3)3·6H2O、Sm(NO3)3·6H2O、Gd(NO3)3·6H2O、Nd(NO3)3·6H2O、Eu(NO3)3·6H2O、Y(NO3)3·6H2O and Er (NO)3)3·6H2Fully mixing seven nitrates of O according to the molar ratio of 1:1:1:1:1:1:1, adding a proper amount of deionized water to dissolve the mixed nitrates to obtain a mixed nitrate solution, and then mixing the mixed nitrate solution with Zr (CH)3COO)4Mixing the solutions to obtain a mixed dispersion system A; mixed dispersionIn system A, Zr (CH)3COO)4And La (NO)3)3·6H2The molar ratio of O is 7: 1;
and B: adding a proper amount of deionized water into the mixed dispersion system A, and uniformly stirring to obtain a mixed dispersion system B;
and C: filtering the mixed dispersion system B by using a standard sieve to remove undissolved impurities to obtain a mixed dispersion system C; the standard sieve is 325 meshes, and the size of the sieve pore is 0.0450 mm; in the step B, the adding amount of water is determined according to the standards that the dynamic viscosity of the mixed dispersion system C is in the range of 4.00-9.00 mPa.s, and the surface tension is in the range of 40.00-60.00 mN/m; in this example, the dynamic viscosity of the mixed dispersion C was measured to be 4.21 mPas using a viscometer, and the surface tension thereof was measured to be 42.89mN/m using a surface tension meter;
step D: and (3) uniformly spraying the mixed dispersion system C into water by using a three-electrode plasma spray gun, wherein the power of the spray gun is 70kW, the liquid drop sprayed into the water at the liquid delivery rate of 30 mL/min is naturally settled and then centrifugally dried, and the single-crystal high-entropy ceramic powder with the hollow spherical structure is obtained, wherein the average particle size of the powder is 0.682 mu m, and the average hollow rate of the powder is 9%.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are possible which remain within the scope of the appended claims.

Claims (10)

1. A single crystal high entropy ceramic powder is characterized in that the powder has a hollow spherical structure and a chemical formula A2B2O7The A site is trivalent rare earth element, the B site is tetravalent metal element; the trivalent rare earth element is lanthanum, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, ytterbium, yttrium or lutetium; the tetravalent metal element is titanium, cerium, tin, zirconium or hafnium.
2. The single-crystal high-entropy ceramic powder of claim 1, wherein the A site is composed of 5 to 7 trivalent rare earth elements.
3. The single-crystal high-entropy ceramic powder of claim 2, wherein the chemical formula is (Me 1)aMe2bMe3cMe4dMe5e)2B2O7A + b + c + d + e is 1 and a is c is d; me1, Me2, Me3, Me4 and Me5 are all one of lanthanum, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, ytterbium, yttrium or lutetium, and Me1, Me2, Me3, Me4 and Me5 are different from each other.
4. The single-crystal high-entropy ceramic powder of claim 2, wherein the chemical formula is (Me 1)aMe2bMe3cMe4dMe5eMe6f)2B2O7A + b + c + d + e + f is 1 and a is c is d is e is f; me1, Me2, Me3, Me4, Me5 and Me6 are all one of lanthanum, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, ytterbium, yttrium or lutetium, and Me1, Me2, Me3, Me4, Me5 and Me6 are different from each other.
5. The single-crystal high-entropy ceramic powder of claim 2, wherein the chemical formula is (Me 1)aMe2bMe3cMe4dMe5eMe6fMe7g)2B2O7A + b + c + d + e + f + g is 1 and a-b-c-d-e-f-g; me1, Me2, Me3, Me4, Me5, Me6 and Me7 are all one of lanthanum, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, ytterbium, yttrium or lutetium, and Me1, Me2, Me3, Me4, Me5, Me6 and Me7 are different from each other.
6. A preparation method of single crystal high-entropy ceramic powder is characterized by comprising the following steps:
step A: mixing a nitrate solution of a trivalent rare earth element and an acetate solution of a tetravalent metal element to obtain a mixed dispersion system A;
and B: adding deionized water into the mixed dispersion system A, and uniformly stirring to obtain a mixed dispersion system B;
and C: filtering the mixed dispersion system B by using a standard sieve to remove undissolved impurities to obtain a mixed dispersion system C;
step D: uniformly spraying the mixed dispersion system C into water by using a three-electrode plasma spray gun, and centrifugally drying after naturally settling liquid drops sprayed into the water to obtain the single-crystal high-entropy ceramic powder with the hollow spherical structure; the chemical formula of the single crystal high-entropy ceramic powder is A2B2O7The A site is trivalent rare earth element, the B site is tetravalent metal element; the trivalent rare earth element is lanthanum, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, ytterbium, yttrium or lutetium; the tetravalent metal element is titanium, cerium, tin, zirconium or hafnium.
7. The method for preparing single-crystal high-entropy ceramic powder according to claim 6, wherein in step C, the dynamic viscosity of the mixed dispersion system C is 4.00 to 9.00mPa · s, and the surface tension is 40.00 to 60.00 mN/m.
8. The preparation method of the single crystal high-entropy ceramic powder body as claimed in claim 6, wherein in the step D, the power of the spray gun is 70-120 kW, and the liquid delivery rate is 20-70 mL/min.
9. The preparation method of the single-crystal high-entropy ceramic powder body as claimed in claim 6, wherein in the step A, 5 to 7 kinds of nitrates of the trivalent rare earth elements are contained, and the molar ratio of the 5 to 7 kinds of nitrates of the trivalent rare earth elements is 1: 1.
10. The method for preparing single-crystal high-entropy ceramic powder according to claim 6, wherein in step C, the standard sieve is 325 mesh or 400 mesh.
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