CN114974773A - Cubic gadolinium-based double perovskite magnetic refrigeration material and preparation method thereof - Google Patents
Cubic gadolinium-based double perovskite magnetic refrigeration material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cubic gadolinium-based double-perovskite magnetic refrigeration material which comprises a cubic gadolinium-based double-perovskite magnetic refrigeration material, wherein the chemical formula of the cubic gadolinium-based double-perovskite magnetic refrigeration material is MBa 2 GdO 6 Wherein M is one or two of Nb, Ta and Bi. By reacting NbCl 5 Or TaCl 5 Or Bi (NO) 3 ) 3 ·5H 2 One or two of O and Ba (NO) 3 ) 2 、Gd 2 (NO 3 ) 3 ·6H 2 O and citric acid (C) 6 H 8 O 7 ) Mixing, heating and stirring, drying, calcining, annealing and cooling to obtain the finished product. According to the cubic gadolinium-based bicalcium ore magnetic refrigeration material and the preparation method thereof, the material is good in chemical stability, compared with a rare earth intermetallic compound, the preparation process is simple and effective compared with a solid phase method, and the synthesized powder particles are fineSmall size, high output, low cost and being suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of preparation of a double-perovskite magnetic refrigeration material, in particular to a cubic gadolinium-based double-perovskite magnetic refrigeration material and a preparation method thereof.
Background
At present, refrigeration technology is strongly demanded in the fields of daily life (such as refrigerators, air conditioners and the like), scientific research (such as spintronics, quantum computing, space science and the like), industrial application (such as low-temperature reagents, fuel liquefaction, low-temperature sensors and the like) and the like. At present traditional refrigeration technology can use halogenated material such as freon, and it is poisonous, easily leak, can cause ozone layer destruction in the atmosphere to the availability factor is low. Different from the traditional refrigeration technology, the magnetic refrigeration technology is to refrigerate by depending on the self-magnetocaloric effect of the magnetic material. The Magnetocaloric Effect (MCE) is an intrinsic property of a magnetic material, and means that the magnetic material changes in magnetic entropy when an external magnetic field changes, so that heat exchange occurs with the outside, and heat absorption and heat release are generated. The magnetic refrigeration also has the advantages of high efficiency and energy saving, and the efficiency of the magnetic refrigeration process can reach 60 to 70 percent of the Carnot cycle efficiency by the thermodynamic process of the magnetocaloric effect. Meanwhile, compared with the gas compression refrigeration technology, the magnetic refrigeration technology can be used in a wider temperature range. Particularly in the temperature range lower than 20K, the magnetic refrigeration technology has greater advantages, and the capacity of processing load cooling in the mW-kW range is particularly favored in a plurality of fields. Therefore, the giant magnetocaloric effect material system developed and applied to the low temperature region has excellent application prospect.
However, the conventional magnetic refrigeration material mainly uses a rare earth-based intermetallic compound, and the preparation process of the material is complicated, the conditions are severe, an accurate control flow is required, and the cost is high. The preparation method mainly adopts smelting, and the preparation method usually needs fine temperature and time, so that the preparation method has the difficulty which cannot be ignored in production. The magnetic refrigeration material mainly based on the rare earth-based oxide has simpler preparation process and lower cost. Therefore, the magnetic refrigeration material can effectively replace rare earth-based intermetallic compounds and is called as a working medium of a low-temperature magnetic refrigeration technology. However, although the current preparation method mainly based on the solid phase method is simple, the process is complicated, the particle size is large, and the performance is greatly influenced.
Disclosure of Invention
The invention aims to provide a cubic gadolinium-based double perovskite magnetic refrigeration material and a preparation method thereof, the material has good chemical stability, compared with a rare earth intermetallic compound, the preparation process is simple and effective, compared with a solid phase method, the preparation process has simple and effective process, the synthesized powder has fine particles, the yield is improved, the cost is reduced, and the material can be used for industrial batch production.
In order to achieve the purpose, the invention provides a cubic gadolinium-based double-perovskite magnetic refrigeration material which comprises a cubic gadolinium-based double-perovskite magnetic refrigeration material, wherein the chemical formula of the cubic gadolinium-based double-perovskite magnetic refrigeration material is MBa 2 GdO 6 Wherein M is one or two of Nb, Ta and Bi.
Preferably, MBa 2 GdO 6 Having a cubic crystal system, belong to
And (4) space group.
A preparation method of a cubic gadolinium-based double perovskite magnetic refrigeration material comprises the following steps:
s1, mixing M salt and Ba (NO) 3 ) 2 、Gd 2 (NO 3 ) 3 ·6H 2 O and citric acid (C) 6 H 8 O 7 ) Weighing according to the molar ratio of 2:4:1: 10-16, and dissolving in deionized water to obtain a mixed solution A;
s2, placing the mixed solution A on a constant-temperature magnetic heating stirrer to be stirred for 1-2 hours to obtain a mixed solution B;
and S3, drying the mixed solution B in a forced air drying oven for 4-5 hours to obtain a powdery compound.
And S4, calcining the powdery compound for 6 hours, grinding the calcined powder again, tabletting, annealing for 8 hours, and cooling to room temperature to obtain the finished product.
Preferably, the M salt in the step S1 is NbCl 5 Or TaCl 5 Or Bi (NO) 3 ) 3 ·5H 2 One or two of O.
Preferably, the heating and stirring temperature of the mixed solution a in the step S2 is 80 to 90 ℃, and the rotation speed is 500 rpm.
Preferably, the drying temperature of the mixed solution B in the step S3 is 110 to 120 ℃.
Preferably, the calcination temperature of the powder compound in the step S4 is 500 to 600 ℃, and the annealing temperature is 800 to 1400 ℃.
Preferably, the isothermal magnetic entropy of the prepared cubic gadolinium-based double perovskite magnetic refrigeration material is 10.1-20.2J/kg K under the change of a 0-2T magnetic field; under the change of a magnetic field of 0-5T, the isothermal magnetic entropy is changed to 18.6-28.1J/kg K; under the change of a magnetic field of 0-7T, the isothermal magnetic entropy is changed to 20.2-29.7J/kg K.
The invention adopts NbCl 5 Or TaCl 5 Or Bi (NO) 3 ) 3 ·5H 2 O、Ba(NO 3 ) 2 、Gd 2 (NO 3 ) 3 ·6H 2 O and citric acid (C) 6 H 8 O 7 ) Preparing cubic gadolinium-based double perovskite magnetic refrigeration material from raw materials, stirring and mixing at low temperature, drying and calcining to obtain MBa 2 GdO 6 The preparation method is simple, the preparation temperature is low, the preparation time is short, and the industrial production of the magnetic refrigeration material is favorably realized. After the powder is calcined, the powder is ground and tableted, which is beneficial to reducing the granularity of the cubic gadolinium-based double perovskite magnetic refrigeration material and obtaining the cubic gadolinium-based double perovskite magnetic refrigeration material with fine particles. Annealing the square gadolinium-based double perovskite magnetic refrigeration material at the temperature of 1300-1400 ℃, which is beneficial to obtaining the MBa with uniform components and tissues 2 GdO 6 A magnetic refrigeration material. The isothermal magnetic entropy of the prepared cubic gadolinium-based double perovskite magnetic refrigeration material is changed to 10.1-20.2J/kg K under the change of a 0-2T magnetic field; under the magnetic field change of 0-5T, the isothermal magnetic entropy is changed to 18.6-28.1J/kg K; under the change of a magnetic field of 0-7T, the isothermal magnetic entropy is changed to 20.2-29.7J/kg K.
Therefore, the cubic gadolinium-based double perovskite magnetic refrigeration material and the preparation method thereof have the advantages of good chemical stability, simple preparation process compared with a rare earth intermetallic compound, simple and effective preparation process compared with a solid phase method, fine synthesized powder particles, high yield, low cost and suitability for industrial batch production.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is an XRD pattern of a cubic gadolinium-based biscalcitanite magnetic refrigeration material and a preparation method thereof in example 1 according to the present invention;
FIG. 2 is a graph showing the entropy change at different temperatures and different magnetic field strengths of a cubic gadolinium-based bicalcite magnetic refrigeration material and a method for preparing the same according to example 1 of the present invention;
FIG. 3 is an XRD pattern of a cubic gadolinium-based biscalcitanite magnetic refrigeration material and a preparation method thereof in example 3 of the present invention;
fig. 4 is an entropy change diagram of a cubic gadolinium-based double perovskite magnetic refrigeration material and a preparation method thereof under different temperatures and different magnetic field strengths in example 3 of the invention.
Detailed Description
The invention provides a cubic gadolinium-based double-perovskite magnetic refrigeration material which comprises a cubic gadolinium-based double-perovskite magnetic refrigeration material, wherein the chemical formula of the cubic gadolinium-based double-perovskite magnetic refrigeration material is MBa 2 GdO 6 Wherein M is one or two of Nb, Ta and Bi. MBa 2 GdO 6 Having a cubic crystal system, belong to
And (4) space group.
A preparation method of a cubic gadolinium-based double perovskite magnetic refrigeration material comprises the following steps:
s1, mixing M salt and Ba (NO) 3 ) 2 、Gd 2 (NO 3 ) 3 ·6H 2 O and citric acid (C) 6 H 8 O 7 ) Weighing according to the molar ratio of 2:4:1: 10-16, and dissolving in deionized water to obtain a mixed solution A; wherein the M salt is NbCl 5 Or TaCl 5 Or Bi (NO) 3 ) 3 ·5H 2 One or two of O.
S2, placing the mixed solution A on a constant-temperature magnetic heating stirrer, and stirring for 1-2 hours at a stirring temperature of 80-90 ℃ and a rotation speed of 500rpm to obtain a mixed solution B;
and S3, drying the mixed solution B in a forced air drying oven at the drying temperature of 110-120 ℃ for 4-5 hours to obtain a powdery compound.
S4, calcining the powdery compound at 500-600 ℃ for 6 hours, then grinding the calcined powder again, tabletting, annealing at 800-1400 ℃ for 8 hours, and cooling to room temperature to obtain the finished product.
The isothermal magnetic entropy of the prepared cubic gadolinium-based double perovskite magnetic refrigeration material is changed to 10.1-20.2J/kg K under the change of a 0-2T magnetic field; under the change of a magnetic field of 0-5T, the isothermal magnetic entropy is changed to 18.6-28.1J/kg K; under the change of a magnetic field of 0-7T, the isothermal magnetic entropy is changed to 20.2-29.7J/kg K.
The technical solution of the present invention is further illustrated by the accompanying drawings and examples.
Example 1
Preparation of NbBa 2 GdO 6 Magnetic refrigeration material
Step 1: reacting NbCl 5 、Ba(NO 3 ) 2 、Gd 2 (NO 3 ) 3 ·6H 2 O and citric acid (C) 6 H 8 O 7 ) Weighing according to the molar ratio of 2:4:1:14 and dissolving in deionized water;
step 2: placing the mixed solution prepared from the raw materials in the step 1 on a constant-temperature magnetic heating stirrer, and stirring for 1-2 hours at the temperature of 80-90 ℃ and the rotating speed of 500 rpm;
and step 3: drying the stirred mixture prepared in the step 2 in a forced air drying oven at 120 ℃ for 4-5 hours to obtain a powdery compound;
and 4, step 4: and (3) calcining the powdery compound obtained in the step (3) at 600 ℃ for 6 hours, then grinding the calcined powder again, tabletting, annealing at 1350 ℃ for 8 hours, and cooling to room temperature to obtain a finished product.
FIG. 1 shows a cubic gadolinium-based dicalcium salt according to the present inventionXRD pattern of titanium ore magnetic refrigeration material and preparation method example 1. As shown, NbBa 2 GdO 6 After grinding, the powder was completely ground and the XRD pattern of the sample was measured at room temperature over a range of 10-90 deg.. Then refining the XRD image by using FULLPROF software, and finding out the peak position and the peak position of the sample
The space groups correspond. Namely, XRD diffraction results show that the prepared NbBa 2 GdO 6 The magnetic refrigeration material is
A monoclinic structure of the space group.
FIG. 2 is an entropy change diagram of a cubic gadolinium-based bicalcium ore magnetic refrigeration material and a preparation method of the invention under different temperatures and different magnetic field strengths in example 1, as shown in the figure, the isothermal magnetic entropy of the obtained finished product is 19.2J/kg K under the magnetic field change of 0-2T; under the change of a magnetic field of 0-5T, the isothermal magnetic entropy is changed to 27.4J/kg K; under the change of a magnetic field of 0-7T, the isothermal magnetic entropy is changed to 28.8J/kg K.
Example 2
Preparation of TaBa 2 GdO 6 Magnetic refrigeration material
Step 1: adding TaCl 5 、Ba(NO 3 ) 2 、Gd 2 (NO 3 ) 3 ·6H 2 O and citric acid (C) 6 H 8 O 7 ) Weighing according to the molar ratio of 2:4:1:14 and dissolving in deionized water;
step 2: placing the mixed solution prepared from the raw materials in the step 1 on a constant-temperature magnetic heating stirrer, and stirring for 1-2 hours at the temperature of 80-90 ℃ and the rotating speed of 500 rpm;
and step 3: drying the stirred mixture prepared in the step 2 in a forced air drying oven at 120 ℃ for 4-5 hours to obtain a powdery compound;
and 4, step 4: and (3) calcining the powdery compound obtained in the step (3) at 500 ℃ for 6 hours, then grinding the calcined powder again, tabletting, annealing at 1350 ℃ for 8 hours, and cooling to room temperature to obtain a finished product. Measuring that the isothermal magnetic entropy of the obtained finished product is 14.9J/kg K under the magnetic field change of 0-2T; under the change of a magnetic field of 0-5T, the isothermal magnetic entropy is changed into 21.5J/kg K; under the change of a magnetic field of 0-7T, the isothermal magnetic entropy is changed to 22.7J/kg K.
Example 3
Preparation of BiBa 2 GdO 6 Magnetic refrigeration material
Step 1: adding Bi (NO) 3 ) 3 ·5H 2 O、Ba(NO 3 ) 2 、Gd 2 (NO 3 ) 3 ·6H 2 O and citric acid (C) 6 H 8 O 7 ) Weighing according to the molar ratio of 2:4:1:14 and dissolving in deionized water;
and 2, step: placing the mixed solution prepared from the raw materials in the step 1 on a constant-temperature magnetic heating stirrer, and stirring for 1-2 hours at the temperature of 80-90 ℃ and the rotating speed of 500 rpm;
and step 3: drying the stirred mixture prepared in the step 2 in a forced air drying oven at 120 ℃ for 4-5 hours to obtain a powdery compound;
and 4, step 4: and (3) calcining the powdery compound obtained in the step (3) at 500 ℃ for 6 hours, then grinding the calcined powder again, tabletting, annealing at 870 ℃ for 8 hours, and cooling to room temperature to obtain a finished product.
Fig. 3 is an XRD chart of the cubic gadolinium-based biscalcitanite magnetic refrigeration material and the preparation method thereof in example 3 of the present invention. As shown, BiBa is added 2 GdO 6 After grinding, the powder was completely ground and the XRD pattern of the sample was measured at room temperature over a range of 10-90 deg.. Then refining the XRD image by using FULLPROF software, and finding out the peak position and the peak position of the sample
The space groups correspond. Namely XRD diffraction results show that the prepared BiBa 2 GdO 6 The magnetic refrigeration material is
A monoclinic structure of the space group.
FIG. 4 is an entropy change diagram of a cubic gadolinium-based bicalcium ore magnetic refrigeration material and a preparation method of the invention under different temperatures and different magnetic field strengths in example 3, as shown in the figure, the isothermal magnetic entropy of the obtained finished product is 11.4J/kg K under the magnetic field change of 0-2T; under the change of a magnetic field of 0-5T, the isothermal magnetic entropy is changed to 19.5J/kg K; under the change of a magnetic field of 0-7T, the isothermal magnetic entropy is changed to 21.1J/kg K.
Example 4
Preparation of Nb 0.75 Ta 0.25 Ba 2 GdO 6 Magnetic refrigeration material
Step 1: reacting NbCl 5 、TaCl 5 、Ba(NO 3 ) 2 、Gd 2 (NO 3 ) 3 ·6H 2 O and citric acid (C) 6 H 8 O 7 ) Weighing and dissolving the materials in deionized water according to the molar ratio of 1.5:0.5:4:1: 14;
step 2: placing the mixed solution prepared from the raw materials in the step 1 on a constant-temperature magnetic heating stirrer, and stirring for 1-2 hours at the temperature of 80-90 ℃ and the rotating speed of 500 rpm;
and step 3: drying the stirred mixture prepared in the step 2 in a forced air drying oven at 120 ℃ for 4-5 hours to obtain a powdery compound;
and 4, step 4: and (3) calcining the powdery compound obtained in the step (3) at 500 ℃ for 6 hours, then grinding the calcined powder again, tabletting, annealing at 1350 ℃ for 8 hours, and cooling to room temperature to obtain a finished product. Measuring that the isothermal magnetic entropy of the obtained finished product is 18.2J/kg K under the magnetic field change of 0-2T, and is 25.9J/kg K under the magnetic field change of 0-5T; under the change of a magnetic field of 0-7T, the isothermal magnetic entropy is changed to 27.3J/kg K.
Example 5
Preparation of Nb 0.5 Ta 0.5 Ba 2 GdO 6 Magnetic refrigeration material
Step 1: reacting NbCl 5 、TaCl 5 、Ba(NO 3 ) 2 、Gd 2 (NO 3 ) 3 ·6H 2 O and citric acid (C) 6 H 8 O 7 ) In a molar ratio of 1:1:4:1:14Weighing in proportion and dissolving in deionized water;
step 2: placing the mixed solution prepared from the raw materials in the step 1 on a constant-temperature magnetic heating stirrer, and stirring for 1-2 hours at the temperature of 80-90 ℃ and the rotating speed of 500 rpm;
and step 3: drying the stirred mixture prepared in the step 2 in a forced air drying oven at 120 ℃ for 4-5 hours to obtain a powdery compound;
and 4, step 4: and (3) calcining the powdery compound obtained in the step (3) at 500 ℃ for 6 hours, then grinding the calcined powder again, tabletting, annealing at 1350 ℃ for 8 hours, and cooling to room temperature to obtain a finished product. Measuring that the isothermal magnetic entropy of the obtained finished product is 17.1J/kg K under the magnetic field change of 0-2T; under the change of a magnetic field of 0-5T, the isothermal magnetic entropy is changed into 24.5J/kg K; under the change of a magnetic field of 0-7T, the isothermal magnetic entropy is changed to be 25.8J/kg K.
Example 6
Preparation of Nb 0.25 Ta 0.75 Ba 2 GdO 6 Magnetic refrigeration material
Step 1: reacting NbCl 5 、TaCl 5 、Ba(NO 3 ) 2 、Gd 2 (NO 3 ) 3 ·6H 2 O and citric acid (C) 6 H 8 O 7 ) Weighing and dissolving in deionized water according to the molar ratio of 0.5:1.5:4:1: 14;
step 2: placing the mixed solution prepared from the raw materials in the step 1 on a constant-temperature magnetic heating stirrer, and stirring for 1-2 hours at the temperature of 80-90 ℃ and the rotating speed of 500 rpm;
and step 3: drying the stirred mixture prepared in the step 2 in a forced air drying oven at 120 ℃ for 4-5 hours to obtain a powdery compound;
and 4, step 4: and (3) calcining the powdery compound obtained in the step (3) at 500 ℃ for 6 hours, then grinding the calcined powder again, tabletting, annealing at 1350 ℃ for 8 hours, and cooling to room temperature to obtain a finished product. Measuring that the isothermal magnetic entropy of the obtained finished product is changed into 16.2J/kg K under the magnetic field change of 0-2T; under the magnetic field change of 0-5T, the isothermal magnetic entropy is changed into 22.8J/kg K; under the change of a magnetic field of 0-7T, the isothermal magnetic entropy is changed to be 24.1J/kg K.
Therefore, the cubic gadolinium-based double perovskite magnetic refrigeration material and the preparation method thereof have the advantages of good chemical stability, simple preparation process compared with a rare earth intermetallic compound, simple and effective preparation process compared with a solid phase method, fine synthesized powder particles, improved yield, reduced cost and suitability for industrial batch production.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (8)
1. A cubic gadolinium-based double perovskite magnetic refrigeration material is characterized in that:
comprises a cubic gadolinium-based double perovskite magnetic refrigeration material, the chemical formula of the cubic gadolinium-based double perovskite magnetic refrigeration material is MBa 2 GdO 6 Wherein M is one or two of Nb, Ta and Bi.
2. The cubic gadolinium-based biscalcitanite magnetic refrigeration material according to claim 1, wherein: MBa 2 GdO 6 Has a cubic crystal system and belongs to Fm3m space group.
3. A method for preparing a cubic gadolinium-based bischofite magnetocaloric material according to any one of claims 1 to 2, comprising the steps of:
s1, mixing M salt and Ba (NO) 3 ) 2 、Gd 2 (NO 3 ) 3 ·6H 2 O and citric acid (C) 6 H 8 O 7 ) Weighing according to the molar ratio of 2:4:1: 10-16, and dissolving in deionized water to obtain a mixed solution A;
s2, placing the mixed solution A on a constant-temperature magnetic heating stirrer, and stirring for 1-2 hours to obtain a mixed solution B;
and S3, drying the mixed solution B in a forced air drying oven for 4-5 hours to obtain a powdery compound.
And S4, calcining the powdery compound for 6 hours, grinding the calcined powder again, tabletting, annealing for 8 hours, and cooling to room temperature to obtain the finished product.
4. The method for preparing a cubic gadolinium-based biscalcitanite magnetic refrigeration material according to claim 3, characterized in that: the M salt in the step S1 is NbCl 5 Or TaCl 5 Or Bi (NO) 3 ) 3 ·5H 2 One or two of O.
5. The method for preparing a cubic gadolinium-based biscalcitanite magnetic refrigeration material according to claim 3, characterized in that: the heating and stirring temperature of the mixed solution A in the step S2 is 80-90 ℃, and the rotating speed is 500 rpm.
6. The method for preparing a cubic gadolinium-based biscalcitanite magnetic refrigeration material according to claim 3, characterized in that: the drying temperature of the mixed solution B in the step S3 is 110-120 ℃.
7. The method for preparing a cubic gadolinium-based biscalcitanite magnetic refrigeration material according to claim 3, characterized in that: in the step S4, the calcination temperature of the powder compound is 500-600 ℃, and the annealing temperature is 800-1400 ℃.
8. The method for preparing a cubic gadolinium-based biscalcitanite magnetic refrigeration material according to claim 3, characterized in that: the isothermal magnetic entropy of the prepared cubic gadolinium-based double perovskite magnetic refrigeration material is changed to 10.1-20.2J/kg K under the change of a 0-2T magnetic field; under the change of a magnetic field of 0-5T, the isothermal magnetic entropy is changed to 18.6-28.1J/kg K; under the change of a magnetic field of 0-7T, the isothermal magnetic entropy is changed to 20.2-29.7J/kg K.
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| CN115557513A (en) * | 2022-10-17 | 2023-01-03 | 中国科学院理化技术研究所 | Gadolinium-based borate compound, preparation and application thereof |
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| CN115557513A (en) * | 2022-10-17 | 2023-01-03 | 中国科学院理化技术研究所 | Gadolinium-based borate compound, preparation and application thereof |
| CN115557513B (en) * | 2022-10-17 | 2024-01-23 | 中国科学院理化技术研究所 | Gadolinium-based borate compound, preparation and application thereof |
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