CN114907121A - High-entropy ceramic with thermal conductivity adjustable and controllable along with temperature and preparation method thereof - Google Patents
High-entropy ceramic with thermal conductivity adjustable and controllable along with temperature and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-entropy ceramic with adjustable and controllable thermal conductivity along with temperature, which is prepared from a raw material HfO 2 、ZrO 2 、SnO 2 、TiO 2 With CeO 2 /MnO 2 The high-entropy ceramic is synthesized through a high-temperature solid-phase reaction, the thermal conductivity of the high-entropy ceramic in the temperature range from room temperature to 1200 ℃ has an extreme value, and the thermal conductivity shows a trend of increasing firstly and then decreasing; the preparation method of the high-entropy ceramic comprises the following steps: ball-milling the raw materials, drying, grinding, sieving, and sintering for high-temperature solid-phase reaction. According to the invention, five metal oxides are subjected to high-temperature solid-phase reaction synthesis to obtain the high-entropy ceramic, under the action of a component recovery mechanism, the low thermal conductivity of the high-entropy ceramic is increased along with the increase of the temperature when the high-entropy ceramic is subjected to heat treatment at a lower temperature, and the thermal conductivity of the high-entropy ceramic is reduced along with the increase of the temperature when the high-entropy ceramic is subjected to heat treatment at a higher temperature, namely the thermal conductivity of the high-entropy ceramic is adjustable along with the temperature, so that the application field of the high-entropy ceramic is widened; the invention relates to a method for preparing high-entropy ceramicsThe preparation method is simple and easy to control, and is easy for industrial production and application.
Description
Technical Field
The invention belongs to the technical field of high-entropy material preparation, and particularly relates to high-entropy ceramic with adjustable and controllable thermal conductivity along with temperature and a preparation method thereof.
Background
The high-entropy ceramic is a novel ceramic appearing in recent years, and is a material with more than 5 kinds of elements, no dominant elements and the content of all the elements between 5% and 35%. Due to the lattice distortion of the material after the high-entropy ceramic is subjected to high-entropy transformation, the high-entropy ceramic has the properties of low thermal conductivity, high melting point, good corrosion resistance, good biocompatibility, good electrochemical performance and the like, and has great development potential in the fields of ultrahigh temperature, biomedicine, energy and the like.
In a high-entropy ceramic system with uniform components, the lattice structure stability of the high-entropy ceramic system is caused by the fact that the Gibbs free energy of the system is reduced due to the increase of the mixed entropy of the system, so that the system can spontaneously form a stable uniform phase. However, simultaneously, since the Gibbs free energy is also directly related to the ambient temperature, the product of the temperature and the entropy jointly affects the Gibbs free energy of the whole system, which means that when the ambient temperature is lower, the joint action of the mixed entropy and the temperature of the system is not enough to enable the high-entropy system to form a uniform solid solution, so that segregation or compounds and the like exist in the system, and when the ambient temperature is increased again, the system spontaneously re-dissolves, namely, the component recovery phenomenon along with the temperature change exists. The heat conduction mechanism of the ceramic is mostly phonon vibration transmission heat conduction, so that the component change of the high-entropy ceramic along with the temperature change can change a phonon vibration mode, the heat conductivity of the material is changed, and the purpose of controlling the heat conductivity of the material through the component change is realized. Considering the application of the high-entropy ceramics in multiple adaptability under future extreme environments, the thermal conductivity change of the high-entropy ceramics from room temperature to 1200 ℃ is of particular concern. By regulating and controlling the thermal conductivity, the method is beneficial to expanding the selection range and the use scene of the nuclear high-entropy structural material.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a high-entropy ceramic with adjustable thermal conductivity along with temperature, aiming at the defects of the prior art. The high-entropy ceramic is synthesized by five metal oxides through high-temperature solid-phase reaction, so that the lattices of the metal oxides are rearranged into a densely arranged cubic lattice structure, under the action of a component recovery mechanism of the high-entropy ceramic, the thermal conductivity is reduced due to the distortion degree of the lattices when the high-entropy ceramic is subjected to heat treatment at a lower temperature and is increased along with the increase of the temperature, and the thermal conductivity is increased due to the increase of the distortion degree of the lattices when the high-entropy ceramic is subjected to heat treatment at a higher temperature, so that the thermal conductivity of the high-entropy ceramic is adjustable along with the temperature.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a high-entropy ceramic with thermal conductivity adjustable with temperature is characterized in that the ceramic is prepared from HfO as raw material 2 、ZrO 2 、SnO 2 、TiO 2 With CeO 2 /MnO 2 The high-entropy ceramic is synthesized through a high-temperature solid-phase reaction, the thermal conductivity of the high-entropy ceramic in the temperature range from room temperature to 1200 ℃ has an extreme value, and the thermal conductivity shows a trend of increasing firstly and then decreasing.
The invention adopts five metal oxides HfO 2 、ZrO 2 、SnO 2 、TiO 2 With CeO 2 /MnO 2 The high-entropy ceramic is synthesized by high-temperature solid-phase reaction as a raw material, when the five metal oxides are subjected to high-temperature solid solution, the increase of the configuration entropy promotes the rearrangement of the lattice of the metal oxides into a densely arranged cubic lattice structure, after the high-entropy ceramic is subjected to heat treatment at a lower temperature, namely a temperature lower than the solid solution temperature, the configuration entropy of the high-entropy ceramic is not high enough and cannot form a uniform solid solution, so that segregation, compounds and even single component phases appear in a system, the component recovery mechanism of the high-entropy ceramic promotes the precipitation of a second phase, the lattice distortion degree of the whole system is reduced, the thermal conductivity of the high-entropy ceramic is increased along with the increase of the temperature, when the high-entropy ceramic is subjected to a higher temperature, namely a temperature is increased to the solid solution temperature, the solid solution is started in the high-entropy ceramic system, the lattice distortion of the whole system is increased, the thermal conductivity of the high-entropy ceramic is reduced along with the increase of the temperature, therefore, the thermal conductivity of the high-entropy ceramic is extreme at a solid solution starting temperature corresponding to the temperature range from room temperature to 1200 ℃, and the thermal conductivity of the high-entropy ceramic tends to increase first and then decrease, namely the thermal conductivity of the high-entropy ceramic can be regulated and controlled along with the temperature, so that the application field of the high-entropy ceramic is widened.
The high-entropy ceramic with the thermal conductivity adjustable and controllable along with the temperature is characterized in that the high-entropy ceramic is single-phase ceramic with a fluorite structure.
The high-entropy ceramic with adjustable and controllable thermal conductivity along with temperature is characterized in that the thermal conductivity of the high-entropy ceramic is increased below the solid solution temperature, and the thermal conductivity of the high-entropy ceramic is decreased above the solid solution temperature.
In addition, the invention also provides a method for preparing the high-entropy ceramic with adjustable and controllable thermal conductivity along with temperature, which is characterized by comprising the following steps: the raw material HfO 2 、ZrO 2 、SnO 2 、TiO 2 With CeO 2 Or with MnO 2 Placing the mixture into a ball milling tank, adding analytically pure ethanol for ball milling for 12-24 h, drying, grinding, sieving, sintering and carrying out high-temperature solid-phase reaction to obtain high-entropy ceramic; the sintering temperature is 1400-1600 ℃, and the sintering time is 1-4 h. According to the invention, each raw material is directly subjected to wet ball milling to refine the size of the raw material and promote the raw material to be fully mixed, drying, grinding and sieving are combined to further refine and mix the raw material uniformly, sintering is carried out to carry out high-temperature solid-phase reaction forming to obtain the high-entropy ceramic, the raw materials are arranged into a densely arranged cubic lattice structure by controlling the sintering temperature and time, complete solid solution is ensured, and the characteristic that the thermal conductivity of the high-entropy ceramic can be regulated along with the temperature is further ensured.
The method is characterized in that the high-entropy ceramic block product is obtained by sieving, then performing compression molding, sintering and performing high-temperature solid-phase reaction. Through carrying out compression molding and sintering after sieving, the requirements of high-entropy ceramic block products with different sizes and different shapes are met, the sintering density is improved, and the quality of the high-entropy ceramic block products is improved.
The room temperature in the present invention is usually 25 ℃ to 35 ℃.
Compared with the prior art, the invention has the following advantages:
1. the invention synthesizes five metal oxides through high-temperature solid phase reaction to obtain the high-entropy ceramic, and rearranges the lattices of the metal oxides into a densely-arranged cubic lattice structure, so that the thermal conductivity is increased along with the increase of the temperature due to the reduction of the lattice distortion degree when the high-entropy ceramic is subjected to heat treatment at a lower temperature, and the thermal conductivity is reduced along with the increase of the temperature due to the increase of the lattice distortion degree when the high-entropy ceramic is subjected to heat treatment at a higher temperature, namely the thermal conductivity of the high-entropy ceramic is adjustable along with the temperature, and the application field of the high-entropy ceramic is widened.
2. The preparation method of the high-entropy ceramic with the thermal conductivity adjustable and controllable along with the temperature is simple and easy to control, and is easy for industrial production and application.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is an XRD (X-ray diffraction) spectrum of a high-entropy ceramic block body with adjustable thermal conductivity along with temperature in embodiments 1-2 of the invention.
FIG. 2 is a graph showing the variation trend of the thermal conductivity of the high-entropy ceramic block body with adjustable and controllable thermal conductivity along with the temperature in the range from room temperature to 1200 ℃ in examples 1-2 of the present invention.
Detailed Description
Example 1
The high-entropy ceramic with adjustable and controllable thermal conductivity along with temperature in the embodiment is prepared from the following components in a molar mass ratio of 1: 1: 1: 1: 1 HfO as a raw material 2 、ZrO 2 、SnO 2 、TiO 2 With CeO 2 Synthesized by high-temperature solid-phase reaction.
The preparation method of the high-entropy ceramic with the adjustable and controllable thermal conductivity along with the temperature comprises the following steps: 10.2488g of HfO as a raw material was charged 2 6g of ZrO 2 7.3380g of SnO 2 3.8893g of TiO 2 With 8.38g of CeO 2 Placing the mixture into a ball milling tank, adding analytically pure ethanol for ball milling for 24 hours, drying and grinding the mixture in an oven at 80 ℃, sieving the mixture with a 250-mesh sieve, performing cold isostatic pressing for forming, sintering the mixture at 1400 ℃ for 2 hours for high-temperature solid-phase reaction to obtain (Hf, Zr, Sn, Ti, Ce) O with adjustable and controllable thermal conductivity along with temperature 2 High entropy ceramic blocks.
Example 2
The high-entropy ceramic with adjustable and controllable thermal conductivity along with temperature in the embodiment is prepared from the following components in a molar mass ratio of 1: 1: 1: 1: 1 HfO as a raw material 2 、ZrO 2 、SnO 2 、TiO 2 And MnO with MnO 2 Synthesized by high-temperature solid-phase reaction.
The preparation method of the high-entropy ceramic with the adjustable and controllable thermal conductivity along with the temperature comprises the following steps: 10.2488g of HfO as a raw material was charged 2 6g of ZrO 2 7.3380g of SnO 2 3.8893g of TiO 2 M with 4.233gnO 2 Placing the mixture into a ball milling tank, adding analytically pure ethanol for ball milling for 12h, drying and grinding the mixture in a 120 ℃ oven in sequence, sieving the mixture with a 250-mesh sieve, performing cold isostatic pressing for forming, sintering the mixture at 1550 ℃ for 4h to perform high-temperature solid-phase reaction to obtain (Hf, Zr, Sn, Ti, Mn) O with adjustable and controllable thermal conductivity along with temperature 2 High entropy ceramic blocks.
The high-entropy ceramic blocks with adjustable and controllable thermal conductivity along with temperature in the embodiments 1 to 2 of the present invention are subjected to X-ray diffraction analysis, and the obtained XRD patterns are shown in fig. 1, and it can be seen from fig. 1 that the high-entropy ceramic blocks with adjustable and controllable thermal conductivity along with temperature in the embodiments 1 to 2 of the present invention all have a cubic fluorite structure.
The thermal conductivity of the high-entropy ceramic block with the thermal conductivity adjustable along with the temperature in the embodiments 1 to 2 of the invention is tested in the temperature range from room temperature to 1200 ℃, and the result is shown in fig. 2, as can be seen from fig. 2, the thermal conductivity of the high-entropy ceramic block in the embodiment 1 is slowly increased below 900 ℃, and starts to be decreased when the temperature is 900 ℃, that is, the thermal conductivity of the high-entropy ceramic block corresponding to the solid solution temperature of 900 ℃ is an extreme value; the thermal conductivity of the high-entropy ceramic block of example 2 slowly increases below 1000 ℃, and starts to decrease as soon as 1000 ℃, that is, the thermal conductivity of the high-entropy ceramic block at the solid solution temperature of 1000 ℃ is an extreme value.
Example 3
The high-entropy ceramic with adjustable and controllable thermal conductivity along with temperature in the embodiment is prepared from the following components in a molar mass ratio of 1: 1: 1: 1: 1 HfO as a raw material 2 、ZrO 2 、SnO 2 、TiO 2 With CeO 2 Synthesized by high-temperature solid-phase reaction.
The preparation method of the high-entropy ceramic with the adjustable and controllable thermal conductivity along with the temperature comprises the following steps: 10.2488g of HfO as a raw material was charged 2 6g of ZrO 2 7.3380g of SnO 2 3.8893g of TiO 2 With 8.38g of CeO 2 Placing the mixture into a ball milling tank, adding analytically pure ethanol for ball milling for 24 hours, drying and grinding the mixture in an oven at 80 ℃, sieving the mixture with a 250-mesh sieve, performing cold isostatic pressing for forming, sintering the mixture at 1400 ℃ for 1 hour for high-temperature solid-phase reaction to obtain (Hf, Zr, Sn, Ti, Ce) O with adjustable and controllable thermal conductivity along with temperature 2 High entropy ceramic blocks.
Through detection, the lattice structure of the high-entropy ceramic block body with the thermal conductivity adjustable and controllable along with the temperature is a single-phase fluorite structure, the thermal conductivity in the temperature range from room temperature to 1200 ℃ shows the trend of increasing firstly and then decreasing, and the thermal conductivity of the high-entropy ceramic block body corresponding to the solid solution temperature of 900 ℃ is an extreme value.
Example 4
The high-entropy ceramic with adjustable and controllable thermal conductivity along with temperature in the embodiment is prepared from the following components in a molar mass ratio of 1: 1: 1: 1: 1 HfO as a raw material 2 、ZrO 2 、SnO 2 、TiO 2 With CeO 2 Synthesized by high-temperature solid-phase reaction.
The preparation method of the high-entropy ceramic with the adjustable and controllable thermal conductivity along with the temperature comprises the following steps: 10.2488g of HfO as a raw material 2 6g of ZrO 2 7.3380g of SnO 2 3.8893g of TiO 2 With 8.38g of CeO 2 Placing the mixture into a ball milling tank, adding analytically pure ethanol for ball milling for 24 hours, drying and grinding the mixture in an oven at 80 ℃, sieving the mixture with a 250-mesh sieve, performing cold isostatic pressing for forming, sintering the mixture at 1600 ℃ for 1 hour for high-temperature solid-phase reaction to obtain (Hf, Zr, Sn, Ti, Ce) O with adjustable and controllable thermal conductivity along with temperature 2 High entropy ceramic blocks.
Through detection, the lattice structure of the high-entropy ceramic block body with the thermal conductivity adjustable and controllable along with the temperature is a single-phase fluorite structure, the thermal conductivity in the temperature range from room temperature to 1200 ℃ shows the trend of increasing firstly and then decreasing, and the thermal conductivity of the high-entropy ceramic block body corresponding to the solid solution temperature of 900 ℃ is an extreme value.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (5)
1. A high-entropy ceramic with thermal conductivity adjustable with temperature is characterized in that the ceramic is prepared from HfO as raw material 2 、ZrO 2 、SnO 2 、TiO 2 With CeO 2 /MnO 2 The high-entropy ceramic is synthesized through a high-temperature solid-phase reaction, the thermal conductivity of the high-entropy ceramic in the temperature range from room temperature to 1200 ℃ has an extreme value, and the thermal conductivity shows a trend of increasing firstly and then decreasing.
2. A high-entropy ceramic having a thermal conductivity controllable with temperature according to claim 1, wherein the high-entropy ceramic is a single-phase ceramic having a fluorite structure.
3. The high-entropy ceramic with adjustable and controllable thermal conductivity along with temperature of claim 1, wherein the thermal conductivity of the high-entropy ceramic is increased below a solid solution temperature, the thermal conductivity of the high-entropy ceramic is decreased above the solid solution temperature, and the corresponding thermal conductivity of the high-entropy ceramic at the solid solution temperature is an extreme value.
4. A method for preparing a high-entropy ceramic having a thermal conductivity controllable with temperature according to any one of claims 1 to 3, which comprises: the raw material HfO 2 ,ZrO 2 ,SnO 2 、TiO 2 With CeO 2 Or with MnO 2 Placing the mixture into a ball milling tank, adding analytically pure ethanol for ball milling for 12-24 h, drying, grinding, sieving, sintering and carrying out high-temperature solid-phase reaction to obtain high-entropy ceramic; the sintering temperature is 1400-1600 ℃, and the time is 1-4 h.
5. The method according to claim 4, wherein the sieving is followed by press forming and sintering for high temperature solid phase reaction to obtain the high entropy ceramic block product.
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