CN109108227B - High-flux preparation method of LaFeSi-based magnetic refrigeration material - Google Patents
High-flux preparation method of LaFeSi-based magnetic refrigeration material Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/22—Moulds for peculiarly-shaped castings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22C9/06—Permanent moulds for shaped castings
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/18—Hardening; Quenching with or without subsequent tempering
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- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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- C21D6/00—Heat treatment of ferrous alloys
- C21D6/008—Heat treatment of ferrous alloys containing Si
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
Abstract
The invention discloses a high-flux preparation method of a LaFeSi-based magnetic refrigeration material. In the method, a wedge-shaped copper mold is adopted in the process of casting a raw material melt into an alloy ingot, so that the cooling rate of the melt in the height direction is changed in a gradient manner to obtain a wedge-shaped alloy ingot with a gradient solidified alloy structure, and then annealing treatment is carried out to obtain the NaZn13The magnetocaloric effect of the LaFeSi-based bulk magnetic refrigeration material with the type structure has gradient. The microstructure obtained by different cooling rates in the same sample is preferably characterized by utilizing a scanning electron microscope with high flux, and the corresponding relation among different tissue structures, magnetocaloric effects and copper mold widths is obtained by combining a magnetocaloric performance test, so that the method can be used for rapidly screening required sample preparation parameters and the like.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a high-flux preparation method of a LaFeSi-based magnetic refrigeration material.
Background
With the development of modern society, refrigeration technology plays a vital role in improving the living standard and working environment of people. Refrigeration appliances such as refrigerators, air conditioners and the like enter household, and the annual energy consumption of the refrigeration industry accounts for more than 15% of the total energy consumption of the whole society according to statistics. The highest efficiency of the currently generally used gas compression refrigeration technology is only 25%, and the gas compression refrigeration technology has the defects of harmful gas emission, high noise, large volume and the like. Therefore, the exploration of a novel refrigeration technology which is environment-friendly, efficient and energy-saving becomes a problem which needs to be solved urgently at present.
The magnetic refrigeration technology is a green refrigeration technology which takes a magnetic material as a working medium and utilizes the magnetocaloric effect of the material to refrigerate. Compared with the traditional compressed gas expansion refrigeration technology, the magnetic refrigeration technology has the following advantages: (1) refrigerants such as Freon, ammonia and the like are not used, so that the environment pollution is avoided; (2) the magnetic refrigeration material is in a solid state, the entropy density of the magnetic refrigeration material is far greater than that of gas, and the refrigeration efficiency is high; (3) the magnetic heat effect is utilized for refrigeration, large-amplitude gas compression movement is not needed, additional energy consumption is avoided, and meanwhile, the refrigerating machine is small in size and stable and reliable in operation. This refrigeration technology has thus received wide attention worldwide.
In recent years, china, the united states, the netherlands, japan, etc. have found several classes of materials that have a giant magnetocaloric effect in the room temperature range, such as: Gd-Si-Ge, Ni-Mn-Ga, Mn-Fe-P-As, MnAs, La (Fe, Si)13And the like. The materials have the common characteristic that magnetic phase change is accompanied with remarkable change of a crystal structure, and the magnetocaloric effect of the materials is obviously higher than that of traditional magnetic refrigeration materials Gd. In these new magnetic refrigeration materials, NaZn13La (Fe, Si) of type structure13The compound is one of the most important materials with the magnetocaloric effect because of the advantages of no toxicity, small hysteresis, low phase-change driving field, low price of raw materials, easy adjustment of Curie temperature and the like.
La (Fe, Si) is used in magnetic refrigeration prototypes of a plurality of laboratories around the world13The base material is used as a magnetic working medium. As such, La (Fe, Si)13Magnetic refrigeration materials have shown great application prospect, but form a single block NaZn13Type structure La (Fe, Si)13The compound needs high-temperature annealing for seven days or even several weeks, which not only wastes energy, but also has an ultra-long production period, thus greatly restricting the industrial application of the compound.
Some studies have shown that the rapid solidification process can shorten La (Fe, Si)13The preparation period of the magnetic refrigeration material is limited, but the research on the cooling rate is only limited to the research under the fixed solidification condition, namely, the research on the solidification under the fixed cooling environment is carried out once, but the preparation method of one furnace at one time has low efficiency, and melt elements in different smelting environments are volatilized differently, so that the problem that the melt elements are easy to causeThe comparison results are unreliable. Therefore, a preparation method for efficiently obtaining different alloy structures and properties in the same sample at high throughput is one of the problems to be solved at present.
Disclosure of Invention
The invention aims to provide a high-flux preparation method of a LaFeSi-based magnetic refrigeration material, and the solidification microstructure and the magnetocaloric effect of the LaFeSi-based magnetic refrigeration material prepared by the method have gradient.
In order to achieve the technical purpose, the invention adopts the technical scheme that: high-flux preparation method of LaFeSi-based magnetic refrigeration material, wherein the LaFeSi-based magnetic refrigeration material has NaZn13A structural phase, the preparation method comprising the steps of:
(1) preparing raw materials according to the chemical formula of the LaFeSi-based magnetic refrigeration material;
(2) casting the melt to obtain an alloy ingot with uniform components;
(3) annealing the alloy ingot to obtain the alloy ingot containing NaZn13The LaFeSi-based block magnetic refrigeration material with the type structure;
the method is characterized in that: and (3) in the step (2), obtaining a wedge-shaped alloy ingot by adopting a wedge-shaped copper die.
The wedge-shaped copper die is characterized in that the cross section area of the copper die is gradually increased or decreased along the height direction of the copper die from the bottom of the copper die. The cross section of the wedge-shaped copper die is not limited, and comprises a rectangle, a circle and the like.
Preferably, the LaFeSi-based magnetic refrigeration material has a chemical formula of La1+xFe13-ySiyWherein x is more than 0 and less than or equal to 1, and y is more than or equal to 1.0 and less than or equal to 1.8.
Preferably, in the step (2), the melt casting is performed under the protection of high-purity inert gas.
Preferably, in the step (2), the melt is blown and cast by high-purity inert gas to obtain the wedge-shaped alloy ingot.
Preferably, in the step (2), the raw materials are put into an electric arc or induction smelting furnace, vacuumized and cleaned by high-purity inert gas,smelting under the protection of high-purity inert gas to obtain alloy ingots, wherein the high-purity inert gas comprises but is not limited to He and/or Ar gas, and preferably, vacuumizing to the vacuum degree of 5 × 10-3Pa or less.
In one implementation manner, in the step (2), the smelted alloy ingot is placed in a quartz tube with an opening at the lower end, the alloy ingot is melted under the protection of high-purity inert gas, and the alloy melt is blown into a wedge-shaped copper mold by using the high-purity inert gas to be solidified, so that the wedge-shaped alloy ingot is obtained. The high purity inert gas includes, but is not limited to, He and/or Ar gas. Preferably, the temperature of the molten alloy ingot is 1400 ℃ to 1600 ℃, and the blowing and casting pressure is 0.03 MPa to 0.06 MPa.
Preferably, in the step (3), annealing is performed under the protection of high-purity inert gas.
Preferably, in the step (3), the annealing temperature is 1000-.
Compared with the prior art, the invention adopts the wedge-shaped copper mold in the melt casting process when preparing the LaFeSi-based magnetic refrigeration material, and has the following beneficial effects:
(1) since the width of the cross section of the wedge-shaped copper mold varies in a gradient manner in the height direction, when the melt is poured into the wedge-shaped copper mold, the cooling rate of the melt varies in a gradient manner in the height direction, and the higher the cooling rate of the melt is at the height where the width of the cross section is smaller, for example, in the wedge-shaped copper mold, the cooling rate of the alloy melt located at the tip of the copper mold (i.e., the smallest width of the cross section) is 2500 + 4500K/s, and the cooling rate of the alloy melt located at the bottom of the copper mold (i.e., the largest width of the cross section) is 50-250K/s. Therefore, the invention effectively realizes that different cooling rates are provided at different heights in the same sample, and a series of solidified alloy structures are obtained at different cooling rates, namely, the sizes of primary iron-rich phase dendrites in the same sample are changed in a gradient manner along the height direction of the copper mold, and the distances between primary iron-rich phase dendrites are finer at the height with the smaller cross section width, so that the gradient of the magnetocaloric effect is further realized, namely, the magnetocaloric effect of the material is better at the height with the smaller cross section width.
(2) The LaFeSi-based magnetic refrigeration material prepared by the preparation method has gradient solidification structure and gradient magnetocaloric effect, therefore, the microstructure obtained by different cooling rates in the same sample prepared by high flux characterization of a scanning electron microscope can be utilized, and the corresponding relation between the microstructure and the magnetocaloric effect of the LaFeSi-based magnetic refrigeration material and the section width of a copper mold can be obtained by combining the magnetocaloric performance test, can be used for rapidly screening alloy tissue structures, optimal sample preparation parameters and the like, and also can be used in actual preparation, according to the organization structure characteristics and the performance of the actually required LaFeSi-based magnetic refrigeration material, comparing the corresponding relation to obtain the section width of the copper mold, which is called as reference section width, so that in the actual preparation process, and keeping other preparation conditions unchanged, and realizing the preparation of the actually required LaFeSi-based magnetic refrigeration material only by controlling the section width of the actually used copper die to be the reference section width.
Drawings
FIG. 1 is a schematic view showing the structure of a wedge-shaped copper mold in example 1 of the present invention;
FIG. 2 shows LaFe obtained in example 1 of the present invention11.6Si1.4Scanning electron microscope photographs of different parts of the wedge-shaped alloy sample;
FIG. 3 shows LaFe obtained in example 1 of the present invention11.6Si1.4The dendrite spacing values of the primary iron-rich phase at different parts of the wedge-shaped alloy sample;
FIG. 4 shows LaFe obtained in example 1 of the present invention11.6Si1.4The change curves of the magnetic entropy change at the top end and the tip end of the sample along with the temperature;
FIG. 5 shows La obtained in example 2 of the present invention1.7Fe11.6Si1.4Scanning electron microscope photographs of different parts of the wedge-shaped alloy sample;
FIG. 6 shows La obtained in example 2 of the present invention1.7Fe11.6Si1.4The dendrite spacing values of the primary iron-rich phase at different parts of the wedge-shaped alloy sample;
FIG. 7 shows La obtained in example 2 of the present invention1.7Fe11.6Si1.4The change of magnetic entropy at the tip and point of the sample with temperature.
Detailed Description
The invention will be described in further detail below with reference to the embodiments of the drawing, which are intended to facilitate the understanding of the invention and are not intended to limit the invention in any way.
The reference numbers in figure 1 are: 1-an alloy melt; 2-copper mold.
In the following examples:
the electric arc furnace is a WK series non-consumable vacuum electric arc furnace of Beijing physical science and photoelectric technology Limited company; the induction melting furnace is a small induction melting furnace of VF-HMF100 produced in Japan;
the model of the scanning electron microscope is FEI Quanta FEG 250; the used dendrite size measurement software is Photoshop software developed by Adobe corporation, USA;
the Quantum magnetometers used are MPMS SQUID VSM manufactured by Quantum Design in the United states.
It is obvious that other devices or software with the same functionality known in the art may be used by those skilled in the art.
In the following examples, the raw materials used were 99.9% pure La, 99.99% pure Fe and 99.999% pure Si, all of which are commercially available.
Example 1:
in this embodiment, the molecular formula of the LaFeSi-based magnetic refrigeration alloy material is LaFe11.6Si1.4。
The high-flux preparation method of the LaFeSi-based magnetic refrigeration material comprises the following steps:
step 1: according to the formula LaFe11.6Si1.4Mixing raw materials of La, Fe and Si, and specifically: converting the alloy atomic percentage into mass percentage, and weighing La, Fe and Si according to the proportion respectively, wherein the purity of each raw material is more than 99%;
and 4, step 4: the LaFe obtained in the step 3 is added11.6Si1.4Annealing the wedge-shaped alloy ingot under the protection of inert gas, wherein the annealing temperature is 1000-1200 ℃, the annealing time is 5-30 minutes, and quenching is carried out in liquid nitrogen or water to obtain the alloy ingot with NaZn13A magnetic refrigeration material of the structure.
The wedge-shaped alloy ingot prepared in the step 3 is tested as follows:
(1) measuring the wedge-shaped LaFe prepared in the step 3 by using a scanning electron microscope11.6Si1.4The alloy ingot has different part structures. In this embodiment, a scanning electron microscope of FEI Quanta FEG 250 type is selected, a back-scattered electron imaging mode is adopted, the electron gun voltage is 20KV, and the magnification is 400 times. The test results are shown in FIG. 2, which is a scanning electron microscope photograph of samples taken from the bottom up at the positions 0mm, 8mm, 16mm, 24mm and 32mm away from the wedge-shaped sample tip, respectively, and show that the iron-rich phase is gradually refined from the wedge-shaped tip to the wedge-shaped tip, indicating that the sample has a continuous gradient change structure.
(2) And measuring the primary iron-rich dendritic crystal spacing from the wedge-shaped top end to different parts of the wedge-shaped tip by using Photoshop software. The test results are shown in FIG. 3, which shows that the primary iron-rich dendrite spacing from the wedge-shaped tip to the tip is refined from 5 μm to 0.3. mu.m.
The magnetic refrigeration material prepared in the step 4 is tested as follows:
(1) the magnetization curves (M-H curves) of the top end and the tip end of the magnetic refrigeration material are respectively measured by using a superconducting quantum interference vibration sample magnetometer MPMS (SQUID) VSM. According to maxwell's relationship:
calculation of magnetic entropy change Δ S from isothermal magnetization curvesMThe results are shown in FIG. 4. As can be seen from FIG. 4, the magnetic refrigeration material has a wide working temperature range and belongs to a typical two-stage phase change characteristic. Under the 1T external magnetic field, the maximum magnetic entropy changes of the top end and the tip end of the magnetic refrigeration material are respectively 4.9J/kgK and 4.6J/kgK, and the corresponding Curie temperatures are respectively 205.5K and 208.5K; under the 2T applied magnetic field, the maximum magnetic entropy changes of the top end and the tip end of the magnetic refrigeration material are respectively 8J/kgK and 7.4J/kgK, and the corresponding Curie temperatures are respectively 205.5K and 208.5K.
In conclusion, in LaFe11.6Si1.4In an alloy system, the wedge-shaped copper mold is blown and cast to realize preparation at different cooling rates in the same sample, a series of gradient solidification structures distributed along the height of the copper mold are obtained, and a simple and convenient preparation method can be provided for researching and applying samples prepared at different cooling rates.
Example 2:
in this embodiment, the molecular formula of the LaFeSi-based magnetic refrigeration alloy material is La1.7Fe11.6Si1.4。
The preparation method of the LaFeSi-based magnetic refrigeration material comprises the following steps:
step 1: according to the formula La1.7Fe11.6Si1.4Mixing raw materials of La, Fe and Si, and specifically: converting the alloy atomic percentage into mass percentage, and weighing La, Fe and Si according to the proportion respectively, wherein the purity of each raw material is more than 99%;
and step 3: crushing the alloy ingot obtained in the step 2 into small pieces of alloy, and preparing La with a gradient solidification structure by using a wedge-shaped copper die through blowing casting1.7Fe11.6Si1.4The alloy is prepared by cleaning small pieces of alloy, placing into quartz glass tube with open bottom, placing into induction coil of induction melting furnace, and vacuumizing to 5 × 10-3Introducing a proper amount of high-purity argon as a protective gas after Pa, adjusting the current until the alloy is completely melted, and injecting the melted alloy melt into a wedge-shaped copper mold by utilizing the pressure difference of 0.03-0.06MPa, wherein the height of the copper mold is about 60mm, the width of the cross section of the copper mold is linearly increased along the height direction, the width of a tip (namely the smallest width of the cross section) is 1mm, and a square gate with the inner diameter width of 6mm (namely the largest width of the cross section) is arranged at the top end, so that a wedge-shaped alloy ingot with the height of 60mm, the width of the top end of 6mm and the width of the tip;
and 4, step 4: subjecting the La obtained in step 31.7Fe11.6Si1.4Annealing the wedge-shaped alloy ingot under the protection of inert gas, wherein the annealing temperature is 1000-1200 ℃, the annealing time is 5-30 minutes, and quenching is carried out in liquid nitrogen or water to obtain the alloy ingot with NaZn13A magnetic refrigeration material of the structure.
The wedge-shaped alloy ingot prepared in the step 3 is tested as follows:
(1) measurement of the wedge-shaped La prepared in the above step 3 by using a scanning electron microscope1.7Fe11.6Si1.4The alloy ingot has different part structures. In this embodiment, a scanning electron microscope of FEI Quanta FEG 250 type is selected, a back-scattered electron imaging mode is adopted, the electron gun voltage is 20KV, and the magnification is 400 times. The test results are shown in FIG. 5, which is a scanning electron microscope photograph of samples taken from the bottom up at positions 0mm, 8mm, 16mm, 24mm and 32mm away from the wedge-shaped sample tip, respectively, and show that the iron-rich phase is gradually refined from the wedge-shaped tip to the wedge-shaped tip, indicating that the sample has a continuous gradient change structure.
(2) And measuring the primary iron-rich dendritic crystal spacing from the wedge-shaped top end to different parts of the wedge-shaped tip by using Photoshop software. The test results are shown in FIG. 6, which shows that the primary iron-rich dendrite spacing from the wedge-shaped tip to the tip is refined from 5 μm to 0.3. mu.m.
The magnetic refrigeration material prepared in the step 4 is tested as follows:
(1) the magnetization curves (M-H curves) of the top end and the tip end of the magnetic refrigeration material are respectively measured by using a superconducting quantum interference vibration sample magnetometer MPMS (SQUID) VSM. According to maxwell's relationship:
calculation of magnetic entropy change Δ S from isothermal magnetization curvesMThe results are shown in FIG. 7. As can be seen from fig. 7, the magnetocaloric effect of the magnetic refrigeration material has a gradient, and the magnetocaloric effect of the top and the tip has a significant difference. Under the 1T external magnetic field, the maximum magnetic entropy changes of the top end and the tip end of the magnetic refrigeration material are respectively 7.6J/kgK and 9.6J/kgK, and the corresponding Curie temperatures are respectively 184.5K and 187.5K; under the 2T applied magnetic field, the maximum magnetic entropy changes of the top end and the tip end of the magnetic refrigeration material are respectively 11.0J/kgK and 14.6J/kgK, and the corresponding Curie temperatures are respectively 184.5K and 190.0K.
(3) According to the test result, obtaining the corresponding relation between the organization structure characteristics and the performance of the LaFeSi-based magnetic refrigeration material and the section width of the copper mold;
in the actual preparation, according to the organization structure characteristics and the performance of the actually required LaFeSi-based magnetic refrigeration material, the corresponding relation is contrasted to obtain the section width of the copper mold, which is called as the reference section width;
in the actual preparation process, other preparation conditions in the steps (1) to (4) are kept unchanged, and the actually used copper mold is controlled to have the reference section width, so that the actually required LaFeSi-based magnetic refrigeration material can be prepared.
The embodiments described above are intended to illustrate the technical solutions of the present invention in detail, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modification, supplement or similar substitution made within the scope of the principles of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. Method for rapidly preparing LaFeSi-based magnetic refrigeration material with required organization structure and magnetocaloric property, wherein the LaFeSi-based magnetic refrigeration material has NaZn13A structural phase, said method comprising the steps of:
(1) preparing raw materials according to the chemical formula of the LaFeSi-based magnetic refrigeration material;
(2) casting the melt to obtain an alloy ingot with uniform components;
(3) annealing the alloy ingot to obtain the alloy ingot containing NaZn13The LaFeSi-based block magnetic refrigeration material with the type structure is used as an intermediate sample; the method is characterized in that: in the step (2), a wedge-shaped copper mold is adopted, when the melt is poured into the same wedge-shaped copper mold, the cross section area of the copper mold gradually increases or gradually decreases along the height direction of the copper mold from the bottom of the copper mold, and a wedge-shaped alloy ingot is obtained;
the intermediate sample has a gradient solidified alloy structure; the intermediate sample has a gradient magnetocaloric effect;
the microstructure obtained by different cooling rates in the intermediate sample is characterized by a high flux of a scanning electron microscope, and the corresponding relation between the structural characteristics and the performance of the LaFeSi-based magnetic refrigeration material and the section width of a wedge-shaped copper mold is obtained;
according to the organization structure characteristics and the performance of the actually required LaFeSi-based magnetic refrigeration material, the corresponding relation is contrasted to obtain the section width of the copper mold, which is called as the reference section width;
and (3) in the actual preparation process, keeping other preparation conditions unchanged from the step (1) to the step (3), and controlling the section width of the actually used copper mold to be the reference section width to prepare the required LaFeSi-based magnetic refrigeration material.
2. The method for rapidly preparing the LaFeSi-based magnetic refrigeration material with the required tissue structure and the magneto-thermal property as claimed in claim 1, which is characterized in that: the LaFeThe chemical formula of the Si-based magnetic refrigeration material is La1+xFe13-ySiyWherein x is more than 0 and less than or equal to 1, and y is more than or equal to 1.0 and less than or equal to 1.8.
3. The method for rapidly preparing the LaFeSi-based magnetic refrigeration material with the required tissue structure and the magneto-thermal property as claimed in claim 1, which is characterized in that: in the step (2), melt casting is carried out under the protection of high-purity inert gas.
4. The method for rapidly preparing the LaFeSi-based magnetic refrigeration material with the required tissue structure and the magneto-thermal property as claimed in claim 3, which is characterized in that: and blowing and casting the melt by using high-purity inert gas to obtain the wedge-shaped alloy ingot.
5. The method for rapidly preparing the LaFeSi-based magnetic refrigeration material with the required tissue structure and the magneto-thermal property as claimed in claim 1, which is characterized in that: and (2) putting the raw materials into an electric arc or induction smelting furnace, vacuumizing, cleaning with high-purity inert gas, and performing melt casting under the protection of the high-purity inert gas to obtain an alloy ingot.
6. The method for rapidly preparing the LaFeSi-based magnetic refrigeration material with the required tissue structure and the magneto-thermal property as claimed in claim 1, which is characterized in that: and (2) placing the alloy ingot in a quartz tube with an opening at the lower end, melting under the protection of high-purity inert gas, and blowing and casting the alloy melt into a wedge-shaped copper mold by using the high-purity inert gas for solidification.
7. The method for rapidly preparing the LaFeSi-based magnetic refrigeration material with the required tissue structure and the magneto-thermal property as claimed in claim 6, which is characterized in that: the melting temperature is 1400-1600 ℃, and the blowing and casting pressure is 0.03-0.06 MPa.
8. The method for rapidly preparing the LaFeSi-based magnetic refrigeration material with the required tissue structure and the magneto-thermal property as claimed in claim 1, which is characterized in that: and (4) annealing under the protection of high-purity inert gas in the step (3).
9. The method for rapidly preparing the LaFeSi-based magnetic refrigeration material with the required tissue structure and the magneto-thermal property as claimed in claim 1, which is characterized in that: in the step (3), the annealing temperature is 1000-1200 ℃, and the annealing time is 5-30 minutes.
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| CN112885549B (en) * | 2021-01-08 | 2022-09-20 | 哈尔滨工业大学 | Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system |
| CN113909455A (en) * | 2021-09-24 | 2022-01-11 | 北京科技大学 | Device and method for preparing sub-rapid solidification alloy in high flux |
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