CN108467928A - A method of improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths - Google Patents
A method of improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths Download PDFInfo
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- CN108467928A CN108467928A CN201810175950.6A CN201810175950A CN108467928A CN 108467928 A CN108467928 A CN 108467928A CN 201810175950 A CN201810175950 A CN 201810175950A CN 108467928 A CN108467928 A CN 108467928A
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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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/008—Heat treatment of ferrous alloys containing Si
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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
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/007—Heat treatment of ferrous alloys containing Co
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/012—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials adapted for magnetic entropy change by magnetocaloric effect, e.g. used as magnetic refrigerating material
- H01F1/015—Metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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Abstract
The present invention relates to technical field of magnetic.The invention discloses a kind of methods improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths, it includes heat treatment, furnace cooling, air-cooled and be flushed with hydrogen, LaFeSi alloy magnetic refrigeration materials are carried out at 1000~1300 DEG C to high-temperature heat treatment 1~24 hour, then in turn through furnace cooling and air-cooled it is cooled to room temperature, it finally carries out being flushed with hydrogen operation, obtains the LaFeSi alloy magnetic refrigeration materials with wider magnetic entropy varied curve halfwidth.LaFeSi alloy magnetic refrigeration materials have broader magnetic entropy varied curve halfwidth, reduce the magnetic refrigerating material type of use in practical applications, can substantially reduce cost under the premise of keeping magnetic entropy to become larger after the method processing in the present invention.
Description
Technical field
The present invention relates to technical field of magnetic, more particularly, to a kind of raising LaFeSi alloy magnetic refrigeration material magnetic
The method of Entropy Changes curve halfwidth.
Background technology
The technology that magnetic refrigeration is the magnetothermal effect using magnetic material during adding magnetic field and demagnetizing field to freeze.
Compared to traditional compressor cooling, there are the advantages such as small, theoretical efficiency is high, green non-pollution, be very potential
Substitute the technology of compressor cooling.
The core of magnetic Refrigeration Technique is magnetic field and magnetic refrigerating material.General magnetic field is higher, the refrigerating capacity of magnetic refrigerating material
It is higher, but the increase higher of cost, so the research staff of magnetic refrigerating material, which is being dedicated to obtaining always, has big magnetic under low field
The magnetic refrigerating material that Entropy Changes and adiabatic temperature become.
After decades of development, current magnetic refrigerating material system mainly has LaFeSi systems, GdSiGe systems, NiMnGa systems
Deng, the advantages that wherein LaFeSi systems magnetic refrigerating material is because of its nontoxic, of low cost, easy preparation as most there is the magnetic system of application prospect
Cold material.For the research staff of magnetic refrigerating material, the target of pursuit is that have big magnetic entropy to become, to obtain height
Refrigerating capacity, have higher refrigerating efficiency.However a problem is but had ignored simultaneously, it is exactly that magnetic entropy becomes and thermal insulation Wen Bianyue
Height, halfwidth is narrower, and the type of the identical required magnetic refrigerating material of refrigeration temperature area is more, and corresponding cost is also got over
It is high.Only with the material of a Curie temperature to freeze it is inadequate generally inside required refrigeration temperature area, generally requires Curie
Temperature interval is that several or even ten several material mating uses in several years can be only achieved better effect.LaFeSi systems magnetic refrigeration material
In near Curie temperature first order phase change occurs for material, and to have big magnetothermal effect, and Phase Transformation Characteristic is that magnetic entropy varied curve exists
Near Curie temperature has narrow and high peak, and usually peak value is higher, and the halfwidth at peak is with regard to smaller, and peak value is lower, peak
Halfwidth it is bigger.In the case where magnetic entropy varied curve halfwidth is smaller, generally require to be divided into the several of several years between Curie temperature
Kind even ten several material mating uses can be only achieved better effect.Since LaFeSi ternary alloy three-partalloys its Curie temperature is in 200K
Left and right, is not used to room temperature magnetic refrigerating, obtains LaFeSiH alloys often through hydrogenation treatment, make its Curie temperature in room temperature
Near, and the feature of first order phase change is kept, still there is big magnetic entropy to become.
Magnetic refrigerating material preparation process is often alloy melting at present, and master alloy heat treatment is used after heat treatment and is quenched to
It is cooled down in ice water or liquid nitrogen, being broken into powder to be retained in the NaZn13 phases of high temperature formation, after cooling is flushed with hydrogen.
The prior art becomes to obtain higher magnetic entropy, often using quenching technical, i.e., the material after heat treatment
It is put into ice water or liquid nitrogen and is cooled down, ice water cooling cost low velocity is fast, but is easy water inlet after material breaks, rotten by oxidation
Erosion reduces yield rate；Liquid nitrogen cooling will not be aoxidized material breaks, and cooling velocity is faster, but cost is very high.Pass through
The NaZn of material is kept after ice water or liquid nitrogen chilling13Phase, to become with very high magnetic entropy, but often magnetic entropy become halfwidth compared with
It is low, only have 4~5K or so such as under the magnetic fields 1T, the magnetic refrigerating material cooperation of more a variety of different Curie temperature is needed to make in the case of this
With can be only achieved preferable effect, corresponding cost is higher.
Invention content
To solve the above problems, the present invention provides a kind of obtain to improve LaFeSi alloys under the premise of magnetic entropy becomes larger
The method of magnetic refrigerating material magnetic entropy varied curve halfwidth.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A method of LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths are improved, are included the following steps：
A) it is heat-treated：LaFeSi alloy magnetic refrigeration materials are subjected to high-temperature heat treatment, heat treatment time at 1000~1300 DEG C
It is 1~24 hour；
B) furnace cooling：Heating is closed after heat treatment, it is 0~60 minute cooling in stove；
C) air-cooled：Calandria in stove is taken out after furnace cooling, and to the LaFeSi alloy magnetic refrigeration materials in furnace body and furnace body
It carries out air-cooled, it is made to be cooled to room temperature in 10~300 minutes.
Key point in the present invention, one are temperature and the processing time of high-temperature heat treatment, 1000~1300 DEG C of place
Manage temperature and 1~24 hour processing time, be for the magnetic refrigerating material in LaFeSi alloy magnetic refrigeration material systems specially
Selection, the magnetic entropy too high or too low for temperature that can all influence LaFeSi alloy magnetic refrigeration materials becomes so that magnetic refrigerating material does not obtain
Magnetic entropy change can be also lost while obtaining wider halfwidth, for magnetic refrigeration material different in LaFeSi alloy magnetic refrigeration material systems
Material, 1000~1300 DEG C for the treatment of temperatures and selected within the scope of 1~24 hour processing time suitable heat treatment temperature and
It processing time, can be under the premise of keeping higher magnetic entropy to become so that magnetic refrigerating material has broader halfwidth；The present invention
Another key point be heat-treated after cooling down rate, although the quickly cooling side of direct ice water/liquid nitrogen in the prior art
Method can obtain higher magnetic entropy and become, but this quickly cooling technique causes adverse effect to the integrality of magnetic refrigerating material, occur
The problems such as broken, and then the more serious problem such as cause oxidation corrosion, and the magnetic entropy of magnetic refrigerating material that similar technique obtains
It is not wide to become halfwidth, only there was only 4~5K under the magnetic fields 1T, first furnace cooling is selected in the present invention, and air-cooled method cools down again,
One initial stage rate of temperature fall is relatively low, can ensure the integrality of magnetic refrigerating material, reduces spoilage, after cooling down in the early stage, uses
It is still relatively mild air-cooled, in the case of the NaZn13 phases that can ensure holding material, increase magnetic entropy and become halfwidth, obtains more preferable
Performance.
It is flushed with hydrogen preferably, it further includes step d)：LaFeSi alloy magnetic refrigeration materials after cooling are crushed, and
Processing 5 hours is flushed with hydrogen in 0.5MPa pressure hydrogen atmosphere.
Preferably, the ingredient of LaFeSi alloy magnetic materials is La1-xCexFe13-a-b-c-dMnaCrbCocSid。
Preferably, La1-xCexFe13-a-b-c-dMnaCrbCocSidIn, ranging from the 0 of x<Ranging from the 1.0 of x≤0.5, d
≤d≤1.5；Ranging from 0≤c≤0.5 of ranging from 0≤b≤0.5 of ranging from 0≤a≤0.5 of a, b, c, and a+b+c
Ranging from 0.003≤a+b+c≤0.5.
Preferably, the air-cooled processing in step c is handled using fan or air blower.
Preferably, in step d, LaFeSi alloy magnetic refrigeration materials after cooling are crushed to grain diameter and are less than 1mm.
Therefore, the invention has the advantages that：The LaFeSi alloy magnetic refrigeration materials after the method processing in the present invention
Material has broader magnetic entropy varied curve halfwidth under the premise of keeping magnetic entropy to become larger, and reduction in practical applications uses
Magnetic refrigerating material type can substantially reduce cost.
Description of the drawings
Fig. 1 is that magnetic refrigerating material halfwidth (indicates) schematic diagram with δ FWHM；
Fig. 2 is La in embodiment 61-xCexFe13-a-b-c-dMnaCrbCocSidThe XRD diffracting spectrums of alloy.
Specific implementation mode
Technical scheme of the present invention is further described With reference to embodiment.
Obviously, the described embodiments are merely a part of the embodiments of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, all other reality obtained by those of ordinary skill in the art without making creative efforts
Example is applied, shall fall within the protection scope of the present invention.
Embodiment 1
1. a kind of method improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths, it is characterised in that including following step
Suddenly：
A) it is heat-treated：LaFeSi alloy magnetic refrigeration materials are subjected to high-temperature heat treatment, heat treatment time at 1000~1300 DEG C
It is 1~24 hour；
B) furnace cooling：Heating is closed after heat treatment, it is 0~60 minute cooling in stove；
C) air-cooled：Calandria in stove is taken out after furnace cooling, and to the LaFeSi alloy magnetic refrigeration materials in furnace body and furnace body
Air-cooled processing is carried out using fan or air blower, it is made to be cooled to room temperature in 10~300 minutes；
D) it is flushed with hydrogen：LaFeSi alloy magnetic refrigeration materials after cooling are crushed to grain diameter and are less than 1mm, and 0.4~
It is flushed with hydrogen processing 4~6 hours in 0.6MPa pressure hydrogen atmosphere.
Embodiment 2
1. a kind of method improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths, it is characterised in that including following step
Suddenly：
A) it is heat-treated：LaFeSi alloy magnetic refrigeration materials are subjected to high-temperature heat treatment, heat treatment time at 1000~1300 DEG C
It is 1~24 hour；
B) furnace cooling：Heating is closed after heat treatment, it is 0~60 minute cooling in stove；
C) air-cooled：Calandria in stove is taken out after furnace cooling, and to the LaFeSi alloy magnetic refrigeration materials in furnace body and furnace body
Air-cooled processing is carried out using fan or air blower, it is made to be cooled to room temperature in 10~300 minutes；
D) it is flushed with hydrogen：LaFeSi alloy magnetic refrigeration materials after cooling are crushed to grain diameter and are less than 1mm, and 0.4~
It is flushed with hydrogen processing 4~6 hours in 0.6MPa pressure hydrogen atmosphere.
Embodiment 3
1. a kind of method improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths, it is characterised in that including following step
Suddenly：
A) it is heat-treated：LaFeSi alloy magnetic refrigeration materials are subjected to high-temperature heat treatment, heat treatment time at 1000~1300 DEG C
It is 1~24 hour；
B) furnace cooling：Heating is closed after heat treatment, it is 0~60 minute cooling in stove；
C) air-cooled：Calandria in stove is taken out after furnace cooling, and to the LaFeSi alloy magnetic refrigeration materials in furnace body and furnace body
Air-cooled processing is carried out using fan or air blower, it is made to be cooled to room temperature in 10~300 minutes；
D) it is flushed with hydrogen：LaFeSi alloy magnetic refrigeration materials after cooling are crushed to grain diameter and are less than 1mm, and 0.4~
It is flushed with hydrogen processing 4~6 hours in 0.6MPa pressure hydrogen atmosphere.
Embodiment 4
1. a kind of method improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths, it is characterised in that including following step
Suddenly：
A) it is heat-treated：LaFeSi alloy magnetic refrigeration materials are subjected to high-temperature heat treatment, heat treatment time at 1000~1300 DEG C
It is 1~24 hour；
B) furnace cooling：Heating is closed after heat treatment, it is 0~60 minute cooling in stove；
C) air-cooled：Calandria in stove is taken out after furnace cooling, and to the LaFeSi alloy magnetic refrigeration materials in furnace body and furnace body
Air-cooled processing is carried out using fan or air blower, it is made to be cooled to room temperature in 10~300 minutes；
D) it is flushed with hydrogen：LaFeSi alloy magnetic refrigeration materials after cooling are crushed to grain diameter and are less than 1mm, and 0.4~
It is flushed with hydrogen processing 4~6 hours in 0.6MPa pressure hydrogen atmosphere.
Embodiment 5
1. a kind of method improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths, it is characterised in that including following step
Suddenly：
A) it is heat-treated：LaFeSi alloy magnetic refrigeration materials are subjected to high-temperature heat treatment, heat treatment time at 1000~1300 DEG C
It is 1~24 hour；
B) furnace cooling：Heating is closed after heat treatment, it is 0~60 minute cooling in stove；
C) air-cooled：Calandria in stove is taken out after furnace cooling, and to the LaFeSi alloy magnetic refrigeration materials in furnace body and furnace body
Air-cooled processing is carried out using fan or air blower, it is made to be cooled to room temperature in 10~300 minutes；
D) it is flushed with hydrogen：LaFeSi alloy magnetic refrigeration materials after cooling are crushed to grain diameter and are less than 1mm, and 0.4~
It is flushed with hydrogen processing 4~6 hours in 0.6MPa pressure hydrogen atmosphere.
Embodiment 6
1. a kind of method improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths, it is characterised in that including following step
Suddenly：
A) it is heat-treated：LaFeSi alloy magnetic refrigeration materials are subjected to high-temperature heat treatment, heat treatment time at 1000~1300 DEG C
It is 1~24 hour；
B) furnace cooling：Heating is closed after heat treatment, it is 0~60 minute cooling in stove；
C) air-cooled：Calandria in stove is taken out after furnace cooling, and to the LaFeSi alloy magnetic refrigeration materials in furnace body and furnace body
Air-cooled processing is carried out using fan or air blower, it is made to be cooled to room temperature in 10~300 minutes；
D) it is flushed with hydrogen：LaFeSi alloy magnetic refrigeration materials after cooling are crushed to grain diameter and are less than 1mm, and 0.4~
It is flushed with hydrogen processing 4~6 hours in 0.6MPa pressure hydrogen atmosphere.
The La used in above-described embodiment 1~61-xCexFe13-a-b-c-dMnaCrbCocSidAlloy magnetic material it is specific at
Divide as shown in following table.
Performance characterization and result：
It will be flushed with hydrogen LaFeSi alloy magnetic refrigeration materials made from above-described embodiment 1~6 and utilize VSM equimagnetic performance measurement devices, survey
The M-H curves under the magnetic fields material 1T are tried, calculating the magnetic entropy under the magnetic fields material 1T by Maxwell relation becomes, and calculates
Go out the halfwidth of magnetic entropy varied curve at this time.
The Curie temperature of LaFeSi alloy magnetic refrigeration materials is flushed with hydrogen made from above-described embodiment 1~6, magnetic entropy becomes and magnetic entropy becomes
The halfwidth equimagnetic results of property such as following table of curve.
| Curie temperature/K | Magnetic entropy change/Jkg-1K-1 | Halfwidth/K | |
| Embodiment 1 | 283 | 9.2 | 7.1 |
| Embodiment 2 | 289 | 9.8 | 6.9 |
| Embodiment 3 | 295 | 6.1 | 12 |
| Embodiment 4 | 287 | 10.8 | 6.8 |
| Embodiment 5 | 295 | 6.8 | 8 |
| Embodiment 6 | 291 | 10 | 8 |
By above-mentioned performance characterization result it is found that LaFeSi alloy magnetic refrigeration materials through in the present invention method processing after magnetic
The halfwidth of Entropy Changes curve is increased, and 7K or more is all reached, and most pronounced effects have reached 12K, compared with the prior art in
The halfwidth of the magnetic entropy varied curve of LaFeSi alloy magnetic refrigeration materials 5K or so has great growth, at least increases 40%,
Magnetic entropy becomes and approaches in the prior art simultaneously；It can be seen that the present invention in processing method can under the premise of keeping great magnetic entropy variation,
Improve the halfwidth of magnetic refrigerating material.
It should be understood that those skilled in the art, can be improved or be become according to the above description
It changes, and all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (6)
1. a kind of method improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths, it is characterised in that including following step
Suddenly：
A) it is heat-treated：LaFeSi alloy magnetic refrigeration materials are subjected to high-temperature heat treatment, heat treatment time at 1000~1300 DEG C
It is 1~24 hour；
B) furnace cooling：Heating is closed after heat treatment, it is 0~60 minute cooling in stove；
C) air-cooled：Calandria in stove is taken out after furnace cooling, and to the LaFeSi alloy magnetic refrigeration materials in furnace body and furnace body
It carries out air-cooled, it is made to be cooled to room temperature in 10~300 minutes.
2. a kind of method improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths according to claim 1,
Characterized by further comprising following steps：
D) it is flushed with hydrogen：LaFeSi alloy magnetic refrigeration materials after cooling are crushed, and place is flushed with hydrogen in 0.5MPa pressure hydrogen atmosphere
Reason 5 hours.
3. a kind of method improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths according to claim 1,
It is characterized in that：
The ingredient of the LaFeSi alloys magnetic material is La1-xCexFe13-a-b-c-dMnaCrbCocSid。
4. a kind of method improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths according to claim 3,
It is characterized in that：
The La1-xCexFe13-a-b-c-dMnaCrbCocSidIn, ranging from the 0 of x<Ranging from 1.0≤d of x≤0.5, d≤
1.5；Ranging from 0≤c≤0.5 of ranging from 0≤b≤0.5 of ranging from 0≤a≤0.5 of a, b, c, and the range of a+b+c
For 0.003≤a+b+c≤0.5.
5. a kind of side for improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths according to claim 1 or 2
Method, it is characterised in that：
Air-cooled processing in the step c is handled using fan or air blower.
6. a kind of side for improving LaFeSi alloy magnetic refrigeration material magnetic entropy varied curve halfwidths according to claim 1 or 2
Method, it is characterised in that：
In the step d, LaFeSi alloy magnetic refrigeration materials after cooling are crushed to grain diameter and are less than 1mm.
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| CN112885549A (en) * | 2021-01-08 | 2021-06-01 | 哈尔滨工业大学 | Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system |
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