CN111235494B - Near-room-temperature amorphous magnetic refrigeration material with magnetic entropy change platform and preparation method thereof - Google Patents

Near-room-temperature amorphous magnetic refrigeration material with magnetic entropy change platform and preparation method thereof Download PDF

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CN111235494B
CN111235494B CN202010147201.XA CN202010147201A CN111235494B CN 111235494 B CN111235494 B CN 111235494B CN 202010147201 A CN202010147201 A CN 202010147201A CN 111235494 B CN111235494 B CN 111235494B
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兰司
张汉鑫
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Nanjing University of Science and Technology
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    • B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
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Abstract

The invention discloses a near-room temperature amorphous magnetic refrigeration material with a magnetic entropy change platform and a preparation method thereof, belonging to the field of magnetic materials, wherein the material has a chemical formula general formula as follows: gd (Gd)45Dy5Co40Si10‑ xFexWherein x is atomic percent and satisfies 0-7. The amorphous magnetic refrigeration material has the advantages that the magnetic entropy change is slowly reduced near the room temperature and has a platform, so that the amorphous magnetic refrigeration material has a larger magnetic phase change temperature span, the refrigeration capacity can reach 611.4-823.2J/kg, and the Curie temperature can reach 148-286K. In addition, the Gd element content in the alloy material is low, the cost is low, the steps of heat treatment and the like are not needed in the preparation process, the preparation method is simple, and the method is suitable for industrial production.

Description

Near-room-temperature amorphous magnetic refrigeration material with magnetic entropy change platform and preparation method thereof
Technical Field
The invention belongs to the field of amorphous magnetic materials, and particularly relates to a Gd-based amorphous magnetic refrigeration material and a preparation method thereof.
Background
Refrigeration is closely related to life and production of modern human society, and plays an irreplaceable role in various fields, such as indoor air conditioning refrigeration, food refrigeration and freezing in life, material low-temperature treatment, low-temperature engineering and superconducting application in industrial production, organ and tissue freezing, low-temperature operation, cryoanesthesia operation and the like in modern medicine. At present, the traditional refrigeration mode is gas compression refrigeration, and the low temperature is achieved by means of a compression cycle method and a cold effect generated during gas throttling expansion. However, the conventional refrigeration method has very obvious disadvantages of low refrigeration efficiency, easy leakage of refrigerant and the like. The traditional gas compression refrigeration can only reach 5% -10% of Carnot cycle, and the prepared low temperature is limited and can not completely meet the requirements. Meanwhile, liquid refrigerants such as Freon and the like are easy to leak when being used, damage the atmospheric ozone layer, cause irreversible damage to the environment and threaten human health. With the attention of people on environmental protection, the united nations environmental planning agency signs the montreal protocol to limit the use of refrigerants such as freon and the like, and aims to protect the atmospheric ozone layer. Thus, scientists research and develop a fluorine-free alternative refrigerant which can solve the problem of destroying the ozone layer. However, the problems of greenhouse effect, low refrigeration efficiency and high energy consumption still exist in the traditional refrigeration, and the problems are not solved fundamentally.
Magnetic refrigeration technology is considered to be a poor candidate for replacing the traditional gas compression refrigeration technology, and due to the unique advantages of the magnetic refrigeration technology, the magnetic refrigeration technology attracts extensive attention and research. Compared with the traditional gas compression refrigeration, the magnetic working medium used in the magnetic refrigeration is generally a solid material, so that the problem of leakage is avoided, and the problem of environment damage such as ozone layer damage, greenhouse effect damage, flammability, explosiveness, toxicity and the like in the traditional refrigeration is solved, so that the magnetic refrigeration is regarded as an environment-friendly refrigeration technology. Meanwhile, the magnetic refrigeration thermodynamic process is highly reversible, the refrigeration efficiency can reach 30% -60% of Carnot cycle, and is even higher, and the magnetic refrigeration thermodynamic process has the characteristics of energy conservation and high efficiency. In addition, the magnetic refrigeration also has the characteristics of high magnetic entropy density of the solid magnetic working medium, simple structure of the refrigerator, no compressor, small volume, long service life, reliable operation, low vibration and noise and the like. Therefore, magnetic refrigeration is regarded as a novel high-efficiency green refrigeration technology, and has a great development and application space under the conditions of energy shortage and global temperature rise at present.
Since the phenomenon of magnetocaloric effect has been discovered, the magnetocaloric effect (MCE) of different materials has been studied intensively and continuously from the theoretical and practical application. In recent years, amorphous alloys have attracted attention because of their unique advantages in their application as magnetic refrigeration materials. Through continuous exploration, magnetic refrigeration is greatly developed in the room temperature range and the low temperature range, and a series of amorphous alloy materials such as rare earth base, transition group systems, high-entropy systems and the like are proved to be applicable to the field of magnetic refrigeration. The size of the MCE of a magnetic material, whether in the room temperature or low temperature range, is critical in determining its cooling capacity. Most rare earth based amorphous alloys have Curie temperature below room temperature and small application temperature range, so that magnetic refrigeration materials with wider application range need to be explored and developed.
Disclosure of Invention
The invention aims to provide a near-room-temperature amorphous magnetic refrigeration material which has large application temperature span, is environment-friendly and has a magnetic entropy change platform.
The invention also aims to provide a preparation method of the near-room-temperature amorphous magnetic refrigeration material with the magnetic entropy change platform.
The technical scheme for realizing the purpose of the invention is as follows:
the near-room temperature amorphous magnetic refrigeration material with a magnetic entropy change platform is a Gd-based amorphous magnetic refrigeration material, and the chemical general formula of the Gd-based amorphous magnetic refrigeration material is Gd45Dy5Co40Si10-xFex，0≤x≤7。
Preferably, the magnetic entropy of the material decreases slowly and has a plateau near room temperature (i.e., 50K-230K).
Preferably, the refrigerating capacity of the material is 611.4-823.2J/kg, and the Curie temperature is 148-286K.
The preparation method of the amorphous magnetic refrigeration material at the near room temperature comprises the following steps:
step 1, weighing raw materials according to the mass percentage of each element in the general formula of the material, and mixing;
step 2, repeatedly smelting the mixed raw materials in a smelting furnace to obtain a uniform alloy ingot;
and 3, crushing the obtained alloy ingot into small pieces, and preparing the Gd-based amorphous magnetic refrigeration strip by using a vacuum strip casting method to obtain the material.
Preferably, in the step 2, the smelting adopts a vacuum arc smelting method.
Preferably, in step 3, the preparation process is as follows: vacuum-pumping to 9.9X 10-4Pa, argon is used as protective gas, the tangential linear velocity of the copper roller is 50 m/s, and the pressure difference between the inside and the outside of the quartz tube in the melt-spinning process is 0.09 MPa.
Preferably, in the step 3, the bandwidth of the Gd-based amorphous magnetic refrigeration strip is 1.5-2 mm, and the thickness of the Gd-based amorphous magnetic refrigeration strip is 30-50 μm.
Compared with the prior art, the invention has the following advantages and effects:
(1) the preparation process adopted by the invention is simple, low in cost and suitable for industrial production.
(2) Gd thus prepared45Dy5Co40Si10-xFexWhen x =0, 5 and 7, typical ferromagnetic-to-paramagnetic secondary magnetic phase changes of the amorphous alloy occur near 148K, 250K and 286K, respectively, and under the action of a magnetic field with Δ H = 5T, the maximum magnetic entropy changes are 6.872, 3.670 and 2.805J/(kg · K), respectively; and the magnetic entropy change of the refrigerator in a low-temperature area is slowly reduced, even a platform appears, so that the refrigerator has larger magnetic transition temperature span and larger refrigerating capacity. Which refrigeratesThe quantity is 611.4, 748.7 and 823.2J/kg under the action of a magnetic field with the delta H = 5T, and the magnetic refrigeration working medium material is very suitable.
Drawings
FIG. 1 is Gd45Dy5Co40Si10-xFex(X =0, 5, 7) X-ray diffraction pattern of alloy strip at room temperature.
FIG. 2 is Gd45Dy5Co40Si10-xFex(x =0, 5, 7) DSC plot of alloy strip between 400K and 720K.
FIG. 3 is Gd45Dy5Co40Si10-xFex(x =0, 5, 7) magnetization versus temperature curve of the alloy strip.
FIGS. 4 (a), (b) and (c) are each Gd45Dy5Co40Si10、Gd45Dy5Co40Si5Fe5And Gd45Dy5Co40Si3Fe7Arrott curves of the alloy strips around the Curie temperature.
FIG. 5 is Gd45Dy5Co40Si10-xFex(x =0, 5, 7) isothermic magnetic entropy change of the alloy ribbon versus temperature.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Example 1
Gd45Dy5Co40Si10The preparation method comprises the following steps:
step 1: gd, Dy, Co and Si with the purity of not less than 99.9 percent are added according to the Gd45Dy5Co40Si10Weighing and mixing the elements in percentage by mass, wherein the nominal total weight of the sample is 10 g;
step 2: placing the above prepared raw materials into a vacuum arc melting furnace, adopting a sponge Ti absorption atmosphere crucible, and respectively vacuumizing to 8.0 × 10-4 Pa, adopting high-purity argon gas to cleanWashing a furnace chamber, filling high-purity argon gas with the pressure of about-0.03 MPa as protective gas, repeatedly smelting for 4 times, and cooling to obtain an alloy ingot with uniform components;
and step 3: crushing the smelted cast ingot, putting the crushed cast ingot into a quartz tube, adopting induction smelting, and vacuumizing to 9.9 multiplied by 10-4And Pa, cleaning the furnace chamber by adopting high-purity argon, using the argon as protective gas, wherein the tangential linear velocity of a copper roller is 50 m/s, and the pressure difference between the inside and the outside of a quartz tube in the process of strip casting is 0.09 MPa, so that the Gd-based amorphous magnetic refrigeration material with the width of 1.5-2 mm and the thickness of 30-50 mu m is obtained.
Example 2
Gd45Dy5Co40Si5Fe5The preparation method of (1) is the same as example 1; obtaining the Gd-based amorphous magnetic refrigeration material with the width of 1.5-2 mm and the thickness of 30-50 mu m.
Example 3
Gd45Dy5Co40Si3Fe7The preparation method of (1) is the same as example 1; obtaining the Gd-based amorphous magnetic refrigeration material with the width of 1.5-2 mm and the thickness of 30-50 mu m.
FIG. 1 is Gd of examples 1 to 345Dy5Co40Si10-xFex(X =0, 5, 7) band sample X-ray diffraction pattern. Analysis proves that diffraction peaks corresponding to crystals are not shown in the map, and the map shows that the crystal is of a completely amorphous structure.
FIG. 2 shows Gd elements of examples 1 to 345Dy5Co40Si10-xFex(x =0, 5, 7) DSC curve of the strip sample, the initial crystallization temperature is 617K, 605K and 576K respectively, which is far higher than the room temperature (300K), indicating that the amorphous sample can exist stably under the room temperature condition.
FIG. 3 is a graph M-T of magnetization versus temperature for a strip sample as measured by a comprehensive Physical Properties Measurement System (PPMS), where the material undergoes a ferromagnetic to paramagnetic magnetic phase transition near the Curie temperature, which corresponds to the temperature at which the minimum of the magnetization derivative with respect to temperature is found. Gd (Gd)45Dy5Co40Si10-xFexMagnetic field of (x =0, 5, 7)The linear transition temperatures were 148K (x = 0), 250K (x = 5) and 286K (x = 7), respectively.
According to the Landau theory, an Arrott curve of the sample at each temperature can be calculated according to the isothermal magnetization curve of the sample, and when the slope of the Arrott curve is positive, the corresponding phase change property is secondary phase change; on the contrary, the phase change property is first order phase change. FIGS. 4 (a), (b) and (c) are each Gd45Dy5Co40Si10-xFex(x =0, 5, 7) Arrott curve of amorphous strip, the slope of the curve in the figure is positive value, so the phase change of the sample is two-stage magnetic phase change, which shows that the used sample has only small thermal hysteresis near the phase change point, effectively avoids the problem of large thermal hysteresis near the first-stage phase change, and improves the utilization rate of energy.
According to the Maxwell relational expression, the isothermal magnetic entropy change and Gd of the amorphous alloy are calculated by using isothermal magnetization curves of different temperatures near the Curie temperature of the sample45Dy5Co40Si10-xFex(x =0, 5, 7) the maximum magnetic entropy changes corresponding to a magnetic field of 5T are 6.872J/(kg · K), 3.670J/(kg · K) and 2.805J/(kg · K), respectively, as shown in fig. 5. FIG. 5 shows that the amorphous alloy Gd45Dy5Co40Si5Fe5In the low temperature range, the magnetic entropy change is reduced slowly, and the same amorphous alloy Gd45Dy5Co40Si3Fe7Besides, the magnetic entropy change is slowly reduced in a low temperature range, a platform exists in a temperature range of 50-100K, and the slow reduction of the magnetic entropy change and the appearance of the platform mean that the amorphous sample doped with the Fe element has a wider magnetic phase transition temperature, and possibly has a larger magnetic refrigeration capacity.
For better evaluation of the refrigeration efficiency of the magnetic refrigerant, the refrigerating capacity RC is used as an evaluation parameter, according to the calculation formula:
Figure 544186DEST_PATH_IMAGE001
the refrigerating capacity of the amorphous alloy can be calculated, wherein delta SM pkFor maximum magnetic entropy change, Δ TFWHMIs half-height wide. Gd (Gd)45Dy5Co40Si10-xFex(x =0, 5, 7) the cooling capacity RC under a magnetic field of 5T was 611.4J/kg, 748.7J/kg and 823.2J/kg, respectively.
In a word, the material is of an amorphous structure, the magnetic entropy change is slowly reduced near room temperature, the material is provided with a platform, the two-stage magnetic phase change is shown in the magnetization process, the loss caused by magnetic hysteresis and thermal hysteresis is avoided, the material is provided with larger magnetic entropy change and refrigerating capacity, and the material is suitable for being used as a magnetic refrigeration material.

Claims (5)

1. The amorphous magnetic refrigeration material near room temperature is characterized in that the material is a Gd-based amorphous magnetic refrigeration material with a chemical general formula of Gd45Dy5Co40Si10-xFex，5≤x≤7；
The magnetic entropy of the material slowly decreases near room temperature and has a platform;
the temperature near room temperature is 50K-230K;
the refrigerating capacity of the material is 611.4-823.2J/kg, and the Curie temperature is 148-286K;
prepared by the following steps:
step 1, weighing raw materials according to the mass percentage of each element in the general formula of the material, and mixing;
step 2, repeatedly smelting the mixed raw materials in a smelting furnace to obtain a uniform alloy ingot;
step 3, crushing the obtained alloy ingot into small pieces, and preparing the Gd-based amorphous magnetic refrigeration strip by using a vacuum strip casting method to obtain the material;
in the step 3, the preparation process is as follows: vacuum-pumping to 9.9X 10-4Pa, argon is used as protective gas, the tangential linear velocity of the copper roller is 50 m/s, and the pressure difference between the inside and the outside of the quartz tube in the melt-spinning process is 0.09 MPa.
2. The method for preparing the near-room-temperature amorphous magnetic refrigeration material according to claim 1, which is characterized by comprising the following steps of:
step 1, weighing raw materials according to the mass percentage of each element in the general formula of the material, and mixing;
step 2, repeatedly smelting the mixed raw materials in a smelting furnace to obtain a uniform alloy ingot;
and 3, crushing the obtained alloy ingot into small pieces, and preparing the Gd-based amorphous magnetic refrigeration strip by using a vacuum strip casting method to obtain the material.
3. The method of claim 2, wherein in step 2, the melting is performed by vacuum arc melting.
4. The method of claim 2, wherein in step 3, the preparation process is as follows: vacuum-pumping to 9.9X 10-4Pa, argon is used as protective gas, the tangential linear velocity of the copper roller is 50 m/s, and the pressure difference between the inside and the outside of the quartz tube in the melt-spinning process is 0.09 MPa.
5. The method according to claim 2, wherein in step 3, the bandwidth of the Gd-based amorphous magnetic refrigeration strip is 1.5-2 mm, and the thickness is 30-50 μm.
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Citations (2)

* Cited by examiner, † Cited by third party
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JP2008133495A (en) * 2006-11-27 2008-06-12 Fuji Xerox Co Ltd Replacement product, authenticity determination apparatus, apparatus for permitting use of replacement, authenticity determination program, and program for permitting use of replacement product
CN106350690A (en) * 2015-07-17 2017-01-25 中国科学院物理研究所 Rare earth gadolinium-based amorphous alloy stripe used for magnetic refrigerant material in room temperature range, and preparation method of rare earth gadolinium-based amorphous alloy stripe

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008133495A (en) * 2006-11-27 2008-06-12 Fuji Xerox Co Ltd Replacement product, authenticity determination apparatus, apparatus for permitting use of replacement, authenticity determination program, and program for permitting use of replacement product
CN106350690A (en) * 2015-07-17 2017-01-25 中国科学院物理研究所 Rare earth gadolinium-based amorphous alloy stripe used for magnetic refrigerant material in room temperature range, and preparation method of rare earth gadolinium-based amorphous alloy stripe

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