CN108286004A - A kind of rare earth-nickel-aluminum material, preparation method and applications - Google Patents
A kind of rare earth-nickel-aluminum material, preparation method and applications Download PDFInfo
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- CN108286004A CN108286004A CN201711467029.0A CN201711467029A CN108286004A CN 108286004 A CN108286004 A CN 108286004A CN 201711467029 A CN201711467029 A CN 201711467029A CN 108286004 A CN108286004 A CN 108286004A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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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
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Abstract
The invention discloses a kind of rare earth nickel aluminum material, preparation method and applications.By chemical formula R14Ni3Al3‑xAtomic percent weigh each raw material respectively, be uniformly mixed, wherein R is rare earth Gd, one kind in Tb, Dy, Ho, Er, Tm or Yb, 0≤x≤0.3；It is smelting, cooling, obtain cast alloy；It is quickly cooled down after vacuum annealing process, obtains a kind of rare earth nickel aluminum material, it is Lu14Co3In3Type tetragonal structure, space group areP42/nmc.Rare earth nickel aluminum material provided by the invention is presented in the temperature range of 20K~80K compared with great magnetic entropy variation, has a larger magnetic refrigeration capacity, good thermal and magnetic reversible nature, and cheap, is very ideal middle warm area magnetic cooling material.
Description
Technical field
The present invention relates to a kind of rare earth-nickel-aluminum material, preparation method and applications, belong to technical field of magnetic materials.
Background technology
Traditional gas Compressing Refrigeration is widely used in Refrigeration ＆ Cryogenic Technique field, but there are refrigerating efficiencies low, energy
Consumption is big, destroys the shortcomings of atmospheric environment.Mangneto refrigeration technique refers to a kind of New Refrigerating technology using magnetic material as refrigeration working medium,
Its refrigeration principle is the magnetothermal effect by means of magnetic cooling material.Under isothermal conditions, when magnetic field intensity increases（Magnetization）Shi Ci
The magnetic moment of material of cooling tends to ordered arrangement, and magnetic entropy reduces, outwardly heat extraction；When the intensity of magnetization weakens（Demagnetization）When magnetic moment tend to
Disorderly arranged, magnetic entropy increases, and magnetic cooling medium absorbs heat from the external world, to achieve the purpose that refrigeration.It compresses and freezes with traditional gas
Technology is compared, and mangneto refrigeration technique has the significant advantages such as energy-efficient, environmentally protective, reliable and stable, is considered high new green system
Refrigeration technique.Wherein, it is magnetic cooling technical application and commercialized core place to find high-performance magnetism material of cooling.
In general, the parameter for weighing magnetic cooling material magnetic heating performance is mainly magnetic entropy change and magnetic refrigeration capacity（That is RC refers to one
Transferable heat in a refrigeration cycle）.It is divided by operation temperature area, magnetic cooling material can be divided into low temperature（20K or less）, medium temperature
（20K~77K）, high temperature（77K~270K）And room temperature（270K~330K）Magnetic cooling material.Wherein, middle warm area be liquefaction nitrogen,
The important warm area of hydrogen, natural gas.Currently, the research in the warm area is concentrated mainly on heavy rare earth Pr, Nd, Er, Tm, DyxEr1-x
Metal and RAl2、RNi2In equal rare earth intermetallic compounds.But the magnetic heating performance of above-mentioned magnetic cooling material is relatively low, transition temperature area
It is narrow, so that its business application is restricted.Therefore, it finds under middle warm area with reversible great magnetic entropy variation and high magnetic refrigeration capacity
Magnetic material is the key that promote the application of medium temperature mangneto refrigeration technique.
Invention content
The present invention provides a kind of with reversible great magnetic entropy variation, price for deficiency existing for existing medium temperature magnetic cooling material
It is cheap, be suitable for middle warm area（20K~80K）The rare earth of refrigeration-nickel-aluminum material, preparation method and applications.
Realize that the technical solution of the object of the invention is to provide a kind of rare earth-nickel-aluminum material, its general formula is R14Ni3Al3-x,
Wherein, R is one kind in rare earth Gd, Tb, Dy, Ho, Er, Tm or Yb, 0≤x≤0.3.
Rare earth of the present invention-nickel-aluminum material, it is Lu14Co3In3Type tetragonal structure, space group areP42/nmc。
Technical solution of the present invention further includes a kind of preparation method of rare earth-nickel-aluminum material, and steps are as follows：
（1）By chemical formula R14Ni3Al3-xAtomic percent weigh each raw material respectively, be uniformly mixed, wherein R is rare earth element
One kind in Gd, Tb, Dy, Ho, Er, Tm or Yb, 0≤x≤0.3；
（2）By step（1）The raw material being mixed to get is placed in electric arc furnaces or induction heater, after furnace chamber vacuumizes, then with high-purity
Argon cleans, smelting, cooling, obtains cast alloy；
（3）By step（2）Obtained cast alloy carries out vacuum annealing process；Or first by step（2）Obtained cast alloy exists
It gets rid of induction melting fast quenching in band machine and obtains amorphous thin ribbon, then carry out vacuum annealing process；
（4）Alloy after vacuum annealing process is quenched and is quickly cooled down in liquid nitrogen or ice water, a kind of rare earth-nickel-aluminum material is obtained.
The step of above-mentioned technical proposal（1）In, since rare earth element is oxidizable, and compensate its waving in preparation process
Hair and scaling loss, rare earth element raw material R is excessively added 1~5% by atomic percent, to obtain monophase materials.
Step（2）In, the vacuum degree that furnace chamber vacuumizes is equal to or less than 5 × 10-2Pa；The temperature of melting be 1200 DEG C~
2000 DEG C, the time of melting is 20 seconds~100 seconds.
Step（3）In, the vacuum degree of vacuum annealing process is 1 × 10-3Pa~1 × 10-5Pa, annealing temperature be 600 DEG C~
1200 DEG C, the time of annealing is 1~40 day.
Technical solution of the present invention provides a kind of application of rare earth-nickel-aluminum material, is used as the refrigeration material of middle warm area 20K~80K
Material.
Compared with prior art, the present invention has following advantageous effect：
1. rare earth prepared by the present invention-nickel-aluminum material has Lu14Co3In3Type tetragonal structure, due to ferromagnetic-paramagnetic phase
Change can be with the variation of rare earth element type, rare earth provided by the invention-nickel-aluminum material wider warm area near middle warm area（20K~
80K）It presents compared with great magnetic entropy variation, there is larger magnetic refrigeration capacity, Gd therein14Ni3Al3、Dy14Ni3Al2.7Magnetic entropy become peak value
- 7J/kgK and -8J/kgK are respectively reached under 0~2T changes of magnetic field.
2. the ferromagnetic phase transition of compound provided by the present invention is second-order phase transistion, there is good magnetic, heat reversible performance, and valence
Lattice are cheap, are ideal medium temperature magnetic cooling materials.
Description of the drawings
Fig. 1 is Gd prepared by the embodiment of the present invention14Ni3Al3And Dy14Ni3Al2.7The room temperature X-ray diffraction of crystalline compound
Spectral line；
Fig. 2 is Gd prepared by the embodiment of the present invention 114Ni3Al3Null field of the crystalline compound under the magnetic fields 100Oe cools down and with field
The thermomagnetization curve of cooling；
Fig. 3 is Gd prepared by the embodiment of the present invention 114Ni3Al3The isothermal magnetization curve of crystalline compound；
Fig. 4 is Gd prepared by the embodiment of the present invention 114Ni3Al3The Arrott curves of crystalline compound；
Fig. 5 is Gd prepared by the embodiment of the present invention 114Ni3Al3The magnetic entropy of crystalline compound becomes the relation curve with temperature；
Fig. 6 is Dy prepared by the embodiment of the present invention 214Ni3Al2.7Null field of the crystalline compound under the magnetic fields 100Oe cools down and with field
The thermomagnetization curve of cooling；
Fig. 7 is Dy prepared by the embodiment of the present invention 214Ni3Al2.7The magnetic entropy of crystalline compound becomes the relation curve with temperature.
Specific implementation mode
Technical solution of the present invention is further elaborated with specific embodiment below in conjunction with the accompanying drawings.
The raw metals such as rare earth, Ni and Al used are purchased from middle promise green wood in following embodiment, and purity is above
99.9%.Utilize the PANalytical X`Pert Pro diffractometers of Dutch Panaco（Cu K α targets）Measure prepared crystalline state chemical combination
The powder x-ray diffraction spectral line of object.It is surveyed using the multi-functional physical measurement system of the PPMS-Dynacool types of Quantum Design
The magnetism and magnetic dsc data of the prepared crystalline compound of amount.
Embodiment 1
The present embodiment prepares Gd14Ni3Al3And measure its performance.
1.Gd14Ni3Al3Preparation, specifically include following steps：
Step（1）：By Gd14Ni3Al3The atomic percent weighing of chemical formula, the commercially available rare earth gold by purity higher than 99.9%
Belong to Gd, W metal and the mixing of Al raw materials, wherein Gd is excessively added 1%（Atomic percent）；
Step（2）：By step（1）The raw material configured is put into electric arc furnaces or induction heater and vacuumizes, when vacuum degree up to 5 ×
10-2Pa~1×10-3When Pa, after the high-purity argon for being 99.999% with purity cleans 1~2 time, vacuum is evacuated to 5 × 10 again-2Pa
~1×10-3When Pa, it is filled with high-purity argon gas protection, air pressure is 1 atmospheric pressure in furnace chamber, overturns melting 2~3 times, each melting repeatedly
Time is 20 seconds, and smelting temperature is between 1200 DEG C~2000 DEG C；
Step（3）：It is cooling in copper crucible to obtain cast alloy, cast alloy is wrapped with tantalum foil, be sealed in vacuum degree be 1 ×
10-3It in the quartz ampoule of Pa, is made annealing treatment 40 days at 600 DEG C, takes out in liquid nitrogen of quickly quenching, obtain product Gd14Ni3Al3Crystalline state
Compound.
2.Gd14Ni3Al3Performance measurement
（1）X-ray diffraction spectral line
Referring to attached drawing 1, it is to measure Gd using PANalytical X`Pert Pro diffractometers14Ni3Al3X-ray powder spread out
Spectrum is penetrated, analysis shows, Gd14Ni3Al3Crystal structure is four directions Lu14Co3In3Type, space group areP42/nmc, cell parameter a=b=
0.96693 (7) nm, c=2.2435 (2) nm, V=2.0976 (2) nm3。
（2）Thermomagnetization curve
The Gd measured in PPMS-Dynacool systems14Ni3Al3Crystalline compound is pyromagnetic at magnetic field intensity H=100Oe
（M-T）Curve, as shown in Figure 2.Gd is can determine from null field cooling M-T curves14Ni3Al3The Curie temperature T of crystalline compoundCFor
60K.In addition, the thermomagnetization curve for cooling down and cooling down with field near Curie temperature null field is completely superposed, show the ferromagnetic-suitable of material
Magnetic phase transition is second-order phase transistion, has good thermal reversibility.
（3）Isothermal magnetization curve and Arrott curves
Fig. 3 is Gd14Ni3Al3Crystalline compound is near Curie temperature（The temperature range of 32K to 82K）Rise field and drop field
Isothermal magnetization curve.Magnetic lag phenomenon is not observed in figure, illustrates Gd made from the present embodiment14Ni3Al3Magnetic refrigeration capacity pair
Magnetic field is reversible.
Isothermal magnetization curve based on Fig. 3 can get Arrott curves, as shown in Figure 4.The phase transition property of compound can be by
The shape of its Arrott curve determines that Arrott slope of a curve of the usual first order phase change material near phase transition temperature be negative
Or S-shaped is presented, and positive slope is then presented in the Arrott curves of second-order phase transistion material near phase transition temperature.It can from Fig. 4
Go out, Curie temperature TCNeighbouring curve is in positive slope, shows Gd made from embodiment 114Ni3Al3Crystalline compound is in Curie's temperature
Ferromagnetic-paramagnetic near degree mutually becomes typical second-order phase transistion.Well known second-order phase transistion material to those skilled in the art
For material with good magnetic, thermal reversibility, magnetic entropy change peak is wider, is conducive to its application in magnetic refrigerator.
（4）Magnetic entropy change effect and magnetic refrigeration capacity
Based on Fig. 3's as a result, according to Maxwell relation：, can be from the temperature
It spends magnetization curve and calculates magnetic entropy change.Calculate Gd14Ni3Al3In TCNeighbouring magnetic entropy becomes to temperature (| Δ S |-T) curve, such as
Shown in Fig. 5.It can be seen that compound is in TCNearby there is big magnetic entropy to become, wherein under 0~5T changes of magnetic field,
Gd14Ni3Al3The maximum magnetic entropy variable of crystalline compound is respectively -13.7J/kgK.Due to can easily be obtained using permanent magnet NdFeB
The magnetic field of 2T is obtained, therefore the change of the magnetic entropy of the material under 0 ~ 2T changes of magnetic field receives much attention.Under 0~2T changes of magnetic field,
Gd14Ni3Al3The Entropy Changes peak value of crystalline compound reaches -7J/kgK.
Refrigerating capacity（RC）It is another important parameter for weighing material practical value.Usually, size is Entropy Changes-temperature
The magnetic entropy of curve becomes the product of peak value and halfwidth.As can be seen from Figure 6, under 0~5T changes of magnetic field, Entropy Changes peak value reaches -13.7J/
KgK, halfwidth 70K, Gd14Ni3Al3The RC of crystalline compound reaches 959J/kg；Under 0~2T changes of magnetic field, Entropy Changes peak
Value reaches -7J/kgK, and halfwidth 45K, RC reach 315J/kg.Gd14Ni3Al3It is hot that crystalline compound shows excellent magnetic
Can, and it is cheap.
Embodiment 2
The present embodiment prepares Dy14Ni3Al2.7, and measure its performance.
1.Dy14Ni3Al2.7Preparation, specifically include following steps：
Step（1）：By Dy14Ni3Al2.7Chemical formula（That is atomic ratio）Purity is higher than 99.9% commercially available Dy, Ni, Al by weighing
Raw material mixes, and wherein Ni is excessively added 5%（Atomic percent）；
Step（2）：By step（1）The raw material configured is put into electric arc furnaces or induction heater and vacuumizes, when vacuum degree up to 5 ×
10-2Pa~1×10-3When Pa, after the high-purity argon for being 99.999% with purity cleans 1~2 time, vacuum is evacuated to 5 × 10 again-2Pa
~1×10-3When Pa, be filled with high-purity argon gas protection, air pressure is 1 atmospheric pressure in furnace chamber, and smelting time is 100 seconds, smelting temperature between
Between 1200 DEG C~2000 DEG C；
Step（3）：By cast alloy coarse crushing, it is placed in and gets rid of the induction coil center in machine cavity body, utilize vacuum fast melt-quenching
Method obtains amorphous thin ribbon shaped sample.It is 1 × 10 that thin ribbon shaped sample, which is sealed in vacuum degree,-3In the quartz ampoule of Pa, at 600 DEG C
Annealing 1 day is taken out in ice water of quickly quenching, obtains product crystalline compound.It is cooling in copper crucible to obtain cast alloy,
Cast alloy is wrapped with tantalum foil, it is 1 × 10 to be sealed in vacuum degree-5In the quartz ampoule of Pa, makes annealing treatment 1 day, take at 1200 DEG C
Go out in ice water of quickly quenching, obtains product Dy14Ni3Al2.7Crystalline compound.
2.Dy14Ni3Al2.7Performance measurement
（1）X-ray diffraction spectral line
Gained Dy is measured using PANalytical X`Pert Pro diffractometers14Ni3Al2.7The room temperature X-ray of crystalline compound is spread out
Spectral line is penetrated, as shown in Figure 1.The result shows that the structure of product is four directions Lu14Co3In3Type, space group areP42/nmc, structure cell ginseng
Number a=b=0.95044 (8) nm, c=2.2795 (2) nm, V=2.0596 (2) nm3。
（2）Thermomagnetization curve
The Dy measured in magnetic measurement systems14Ni3Al2.7Crystalline compound is pyromagnetic at magnetic field intensity H=100Oe（M-T）
Curve, as shown in Figure 6.Dy is can determine from null field cooling M-T curves14Ni3Al2.7The Curie temperature T of crystalline compoundCFor
25K.In addition, the thermomagnetization curve for cooling down and cooling down with field near Curie temperature null field is completely superposed, show the ferromagnetic-suitable of material
Magnetic phase transition is second-order phase transistion, has good thermal reversibility.
（3）Magnetic entropy change effect and magnetic refrigeration capacity
Calculate Dy14Ni3Al2.7In TCNeighbouring magnetic entropy becomes to temperature (| Δ S |-T) curve, as shown in Figure 7.From figure
It is found that compound is in TCNearby there is big magnetic entropy to become, wherein under 0~5T changes of magnetic field, Dy14Ni3Al2.7Crystalline compound
Maximum magnetic entropy variable be respectively -15.7J/kgK.Under 0~2T changes of magnetic field, Dy14Ni3Al2.7The Entropy Changes peak of crystalline compound
Value reaches -8J/kgK, and the RC of halfwidth 52K, crystalline compound reach 416J/kg.
Above-described embodiment only lists the case where R is Gd and Dy, but according to the present invention, R can also be Tb, Ho, Er, Tm and
Any one in the rare earth elements such as Yb, these materials can equally obtain same as the previously described embodiments or comparable effect.
Claims (7)
1. a kind of rare earth-nickel-aluminum material, it is characterised in that：Its general formula is R14Ni3Al3-x, wherein R be rare earth Gd,
One kind in Tb, Dy, Ho, Er, Tm or Yb, 0≤x≤0.3.
2. a kind of rare earth-nickel-aluminum material according to claim 1, it is characterised in that：It is Lu14Co3In3Type tetragonal crystal
Structure, space group areP42/nmc。
3. a kind of preparation method of rare earth-nickel-aluminum material, it is characterised in that include the following steps：
（1）By chemical formula R14Ni3Al3-xAtomic percent weigh each raw material respectively, be uniformly mixed, wherein R is rare earth element
One kind in Gd, Tb, Dy, Ho, Er, Tm or Yb, 0≤x≤0.3；
（2）By step（1）The raw material being mixed to get is placed in electric arc furnaces or induction heater, after furnace chamber vacuumizes, then with high-purity
Argon cleans, smelting, cooling, obtains cast alloy；
（3）By step（2）Obtained cast alloy carries out vacuum annealing process；Or first by step（2）Obtained cast alloy exists
It gets rid of induction melting fast quenching in band machine and obtains amorphous thin ribbon, then carry out vacuum annealing process；
（4）Alloy after vacuum annealing process is quenched and is quickly cooled down in liquid nitrogen or ice water, a kind of rare earth-nickel-aluminum material is obtained.
4. a kind of preparation method of rare earth-nickel-aluminum material according to claim 3, it is characterised in that：Step（1）In it is dilute
Earth elements raw material R is excessively added 1~5% by atomic percent.
5. a kind of preparation method of rare earth-nickel-aluminum material according to claim 3, it is characterised in that：Step（2）In, stove
The vacuum degree that chamber vacuumizes is equal to or less than 5 × 10-2Pa；The temperature of melting is 1200 DEG C~2000 DEG C, and the time of melting is
20 seconds~100 seconds.
6. a kind of preparation method of rare earth-nickel-aluminum material according to claim 3, it is characterised in that：Step（3）In, very
The vacuum degree of sky annealing is 1 × 10-3Pa~1 × 10-5Pa, annealing temperature be 600 DEG C~1200 DEG C, annealing when
Between be 1~40 day.
7. a kind of application of rare earth-nickel-aluminum material, it is characterised in that be used as the refrigerating material of middle warm area 20K~80K.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115786825A (en) * | 2022-11-24 | 2023-03-14 | 西安交通大学 | Process for preparing amorphous alloy capable of resisting high-low temperature circulating environment |
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| JPH0696916A (en) * | 1991-03-14 | 1994-04-08 | Takeshi Masumoto | Material for magnetic refrigerating work and its manufacture |
| CN102453466A (en) * | 2010-10-14 | 2012-05-16 | 中国科学院物理研究所 | Rare earth-copper-aluminum material for magnetic refrigeration and preparation method thereof |
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| YU.B. TYVANCHUK ET AL.: "The Dy-Ni-In system at 870 K: Isothermal section, solid solutions, crystal structures", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115786825A (en) * | 2022-11-24 | 2023-03-14 | 西安交通大学 | Process for preparing amorphous alloy capable of resisting high-low temperature circulating environment |
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