CN112062565B - Preparation method of PSINT-based high-entropy ceramic electrocaloric refrigeration material - Google Patents
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- 239000000919 ceramic Substances 0.000 title claims abstract description 47
- 239000000463 material Substances 0.000 title claims abstract description 19
- 238000005057 refrigeration Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 21
- 239000002245 particle Substances 0.000 claims abstract description 21
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000011812 mixed powder Substances 0.000 claims abstract description 6
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 13
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 11
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 11
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 11
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 11
- YADSGOSSYOOKMP-UHFFFAOYSA-N lead dioxide Inorganic materials O=[Pb]=O YADSGOSSYOOKMP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000003889 chemical engineering Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 10
- 238000005303 weighing Methods 0.000 description 6
- 238000000465 moulding Methods 0.000 description 3
- 210000002568 pbsc Anatomy 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 229910010252 TiO3 Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
The invention relates to a preparation method of a PSINT-based high-entropy ceramic electrocaloric refrigeration material, belonging to the technical field of chemical engineering. A preparation method of a PSINT-based high-entropy ceramic electrocaloric refrigeration material comprises ball-milling raw materials and alcohol, drying and pressing the obtained mixed powder; calcining and synthesizing the obtained raw material blocks, and grinding to obtain ceramic particles; pressing into a ceramic blank; sintering under the coverage of the obtained ceramic particles; annealing to obtain the required ceramic material. The preparation method can obtain excellent electric card performance at room temperature and below; meanwhile, the structure and the performance of the ceramic can be controlled by changing the multielement high entropy principle, the annealing time and the temperature. The preparation method is relatively simple, and is a convenient and rapid preparation technology.
Description
Technical Field
The invention relates to a preparation method of a PSINT-based high-entropy ceramic electrocaloric refrigeration material, belonging to the technical field of chemical engineering.
Background
At present, in the process of a compressor refrigeration method, a large amount of gas is released by the added Freon, so that the environment is directly damaged, and a very important task is to find a new economic and environment-friendly refrigeration mode to replace the traditional compression refrigeration technology. The electrocaloric effect refers to a phenomenon that polarization state changes in a polar material due to application or removal of an electric field so as to cause change of adiabatic temperature or isothermal entropy of the material, and the effect can be used for development of novel solid refrigeration materials. The electric card refrigeration material has the advantages of environmental protection, high efficiency, easy miniaturization and the like. While the ferroelectric material has excellent electric card effect, the research on the electric card effect of the ferroelectric material is mainly focused on the research field of ceramics and thin films using Si-based semiconductors as substrates, for example, the research on PbxSc1-xTiO3Electrocaloric effects of components in the system, e.g. study of PbxCaySr(1-x-y)TiO3Pyroelectric response and temperature-dependent effect.
Disclosure of Invention
The invention aims to provide a preparation method of a PSINT-based high-entropy ceramic electrocaloric refrigeration material. The PSINT is a good electrocaloric effect ferroelectric material which stimulates the temperature entropy change of the material according to the multi-element high entropy principle, and the PSINT ceramic material which can be prepared by a solid phase sintering method has a good electrocaloric effect, and the electrocaloric performance of the ceramic can be regulated and controlled by changing the annealing time.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a PSINT-based high-entropy ceramic electrocaloric refrigeration material comprises the following steps:
1) ball-milling prepared PSINT raw materials and alcohol, drying the mixed powder obtained by grinding, and pressing a column to prepare a raw material block, wherein the prepared PSINT raw materials comprise PbO2、Ta2O5、Sc2O3、In2O3And Nb2O5The PSINT has a general formula of PbScxInyNb0.5-xTa0.5- yO3Wherein x is more than 0 and less than 0.5, and y is more than 0 and less than 0.5;
2) calcining and synthesizing the raw material blocks obtained in the step 1), and grinding to obtain ceramic particles;
3) pressing the ceramic particles into a ceramic blank;
4) sintering the obtained ceramic blank under the covering of the particles obtained in the step 2), wherein the sintering temperature is 1200-1300 ℃, and the heat preservation is carried out for 8-10 hours;
5) annealing the product obtained in the step 4) to obtain the required ceramic material.
Preferably, the rotation speed of the ball milling in the step 1) is 400-600rpm, and the ball milling time is 10-16 hours.
Preferably, the drying temperature in step 1) is 100-150 ℃.
Preferably, the calcination temperature in the step 2) is 800-900 ℃, and the calcination time is 2-4 hours.
Preferably, the pressing in step 3) is carried out under the condition of cold isostatic pressing of 25-30MPa for 4-8 minutes.
Preferably, the annealing temperature in the step 5) is 1100-1200 ℃, and the annealing time is any one of 8-10h, 18-20h, 28-30h, 38-40h and 48-50 h.
The invention has the beneficial effects that: the preparation method can obtain excellent electric card performance at room temperature and below; meanwhile, the structure and the performance of the ceramic can be controlled by changing the multielement high entropy principle, the annealing time and the temperature. The preparation method is relatively simple, and is a convenient and rapid preparation technology.
Drawings
FIG. 1 is a graph comparing electrical card performance at different annealing times for PSINT ceramics obtained in examples 1-5 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited to the scope of the examples. These examples are intended to illustrate the invention only and are not intended to limit the scope of the invention. In addition, various modifications may occur to those skilled in the art upon reading the present disclosure, and such equivalent variations are within the scope of the present invention as defined in the appended claims.
Example 1
(1) Will need excessive PbO2、Ta2O5、Sc2O3、In2O3And Nb2O5Drying the raw material and weighing PbO2 13g、Ta2O5 3g、Sc2O3 2g、In2O3 1g、Nb2O51g, keeping the temperature of a laboratory at the vicinity of room temperature and keeping the humidity below 40%;
(2) weighing the excessive PbO weighed in the step (1)2、Ta2O5、Sc2O3、In2O3And Nb2O5Performing ball milling in a ball milling pot with a proper amount of alcohol, wherein the rotating speed is set to 400rpm, and the ball milling time is 10 hours;
(3) the PbSc which is ball-milled in the step (2) is treated0.1In0.1Nb0.4Ta0.4O3And drying and pressing the mixed powder to obtain a raw material block. The drying temperature is controlled at 100 ℃;
(4) calcining the raw material blocks obtained in the step (3) at 800 ℃ for 2 hours to synthesize the ceramic particles, and grinding the ceramic particles;
(5) and (4) ball-milling the sample particles obtained in the step (4) under alcohol, sieving and drying. Taking a proper amount of sample, pre-pressing and molding the sample in a mold, and then placing the sample in a cold isostatic press at 25MPa for 4 minutes to press the sample into a ceramic blank;
(6) covering and sintering the PSINT ceramic blank obtained in the step (7) under the particles obtained in the step (4), wherein the sintering temperature is 1200 ℃, and the temperature is kept for 8 hours to obtain a ceramic material with excellent electrocaloric effect;
(7) and (4) annealing the PSINT ceramic material obtained in the step (6) in a 1100 ℃ tube furnace for 10 hours to obtain the required ceramic material.
Example 2
(1) Will need excessive PbO2、Ta2O5、Sc2O3、In2O3And Nb2O5Drying the raw material and weighing PbO2 12g、Ta2O5 2g、Sc2O3 1g、In2O3 0.3g、Nb2O50.3g, keeping the temperature of a laboratory at the vicinity of room temperature and keeping the humidity below 40%;
(2) weighing the excessive PbO weighed in the step (1)2、Ta2O5、Sc2O3、In2O3And Nb2O5Performing ball milling in a ball milling pot with a proper amount of alcohol, wherein the rotating speed is set to 500 revolutions per minute, and the ball milling time is 15 hours;
(3) the PbSc which is ball-milled in the step (2) is treated0.1In0.1Nb0.4Ta0.4O3And drying and pressing the mixed powder to obtain a raw material block. The drying temperature is controlled at 120 ℃;
(4) calcining the raw material blocks obtained in the step (3) at 850 ℃ for 3 hours to synthesize the ceramic particles, and grinding the ceramic particles to obtain ceramic particles;
(5) and (4) ball-milling the sample particles obtained in the step (4) under alcohol, sieving and drying. Taking a proper amount of sample, pre-pressing and molding the sample in a mold, and then placing the sample in a cold isostatic press under 26MPa for 5 minutes to press the sample into a ceramic blank;
(6) covering and sintering the PSINT ceramic blank obtained in the step (7) under the particles obtained in the step (4), wherein the sintering temperature is 1250 ℃, and the temperature is kept for 9 hours to obtain a ceramic material with excellent electrocaloric effect;
(7) and (4) annealing the PSINT ceramic material obtained in the step (6) in a tubular furnace at 1150 ℃ for 20 hours to obtain the required ceramic material.
Example 3
(1) Will need excessive PbO2、Ta2O5、Sc2O3、In2O3And Nb2O5Drying the raw material and weighing PbO2 12g、Ta2O5 2g、Sc2O3 1g、In2O3 0.3g、Nb2O50.3g, keeping the temperature of a laboratory at the vicinity of room temperature and keeping the humidity below 40%;
(2) weighing the excessive PbO weighed in the step (1)2、Ta2O5、Sc2O3、In2O3And Nb2O5Performing ball milling in a ball milling pot with a proper amount of alcohol, wherein the rotating speed is set to 600rpm, and the ball milling time is 16 hours;
(3) the PbSc which is ball-milled in the step (2) is treated0.1In0.1Nb0.4Ta0.4O3And drying and pressing the mixed powder to obtain a raw material block. The drying temperature is controlled at 150 ℃;
(4) calcining the raw material blocks obtained in the step (3) at 900 ℃ for 4 hours to synthesize the ceramic particles, and grinding the ceramic particles;
(5) and (4) ball-milling the sample particles obtained in the step (4) under alcohol, sieving and drying. Taking a proper amount of sample, pre-pressing and molding the sample in a mold, and then placing the sample in a cold isostatic press for pressing into a ceramic blank body under the pressure of 30MPa for 8 minutes;
(6) covering and sintering the PSINT ceramic blank obtained in the step (7) under the particles obtained in the step (4), wherein the sintering temperature is 1300 ℃, and the temperature is kept for 10 hours to obtain a ceramic material with excellent electrocaloric effect;
(7) and (4) annealing the PSINT ceramic material obtained in the step (6) in a tube furnace at 1200 ℃ for 30 hours to obtain the required ceramic material.
Example 4
The same method as in example 1 was used to prepare a ceramic material required for ceramics, except that the annealing time in step (7) was 40 hours.
Example 5
The same method as in example 1 was used to prepare a ceramic material required for ceramics, except that the annealing time in step (7) was 50 hours.
Example 6
The same method as in example 1 was used to prepare the ceramic material required for the ceramic, except that the annealing time in step (7) was 8 hours.
Example 7
The same method as in example 1 was used to prepare a ceramic material required for ceramics, except that the annealing time in step (7) was 18 hours.
Example 8
The same method as in example 1 was used to prepare a ceramic material required for ceramics, except that the annealing time in step (7) was 28 hours.
Example 9
The same process as in example 1 was used to prepare the ceramic material required for the ceramic, except that the annealing time in step (7) was 38 hours.
Example 10
The same method as in example 1 was used to prepare a ceramic material required for ceramics, except that the annealing time in step (7) was 48 hours.
Claims (4)
1. A preparation method of a PSINT-based high-entropy ceramic electrocaloric refrigeration material is characterized by comprising the following steps of:
1) ball-milling PSINT raw material and alcohol, and grindingDrying the mixed powder, and pressing to obtain a raw material block, wherein the raw material for preparing PSINT comprises PbO2、Ta2O5、Sc2O3、In2O3And Nb2O5The PSINT has a general formula of PbScxInyNb0.5-xTa0.5-yO3Wherein x is more than 0 and less than 0.5, and y is more than 0 and less than 0.5;
2) calcining and synthesizing the raw material blocks obtained in the step 1), and grinding to obtain ceramic particles;
3) pressing the ceramic particles into a ceramic blank;
4) sintering the obtained ceramic blank under the covering of the particles obtained in the step 2), wherein the sintering temperature is 1200-1300 ℃, and the heat preservation is carried out for 8-10 hours;
5) annealing the product obtained in the step 4) to prepare the required ceramic material;
step 2) the calcination temperature is 800-900 ℃, the calcination time is 2-4 hours, step 5) the annealing temperature is 1100-1200 ℃, and the annealing time is any one of 8-10 hours, 18-20 hours, 28-30 hours, 38-40 hours and 48-50 hours.
2. The method for preparing the PSINT-based high-entropy ceramic electrical card refrigeration material as claimed in claim 1, wherein the rotation speed of the ball milling in the step 1) is 400-600rpm, and the ball milling time is 10-16 hours.
3. The method for preparing the PSINT-based high-entropy ceramic electrical card refrigeration material as claimed in claim 1, wherein the drying temperature in the step 1) is 100-150 ℃.
4. The method for preparing the PSINT-based high-entropy ceramic electrocaloric refrigeration material according to claim 1, wherein the pressing in the step 3) is performed under a cold isostatic pressure of 25-30MPa for 4-8 minutes.
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