CN105390223B - A kind of room temperature magnetic refrigerating alloy material and preparation method - Google Patents
A kind of room temperature magnetic refrigerating alloy material and preparation method Download PDFInfo
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- CN105390223B CN105390223B CN201510713559.3A CN201510713559A CN105390223B CN 105390223 B CN105390223 B CN 105390223B CN 201510713559 A CN201510713559 A CN 201510713559A CN 105390223 B CN105390223 B CN 105390223B
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
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- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C22/00—Alloys based on manganese
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- 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
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- 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
A kind of room temperature magnetic refrigerating alloy material of the present invention, molecular formula Mn1‑XAlXCoGe, in alloy material, the mass percent of manganese element is 33.3 ~ 34.4%, and the mass percent of aluminium element is 0.6 ~ 2.7%, and the mass percent of cobalt element is 32.8 ~ 33.3%, and the mass percent of Germanium is 30.2 ~ 32.7%.The present invention also provides the preparation methods of above-mentioned alloy material, and reactive material is added in vacuum arc furnace ignition, vacuumize less than 10‑4Pa is passed through argon gas；By sample melt back；Sample cooling is taken out, sample is put into high temperature resistant quartz glass test tube, is vacuumized, high purity argon is filled with and carries out gas washing, be put into stove formula case, sample annealing is taken out, obtains room temperature magnetic refrigerating alloy material.The present invention significantly makes the Curie temperature of alloy be down near room temperature, efficiently avoids the thermal hysteresis near phase transformation, and have larger temperature controllable wide near room temperature.
Description
Technical field
The invention belongs to field of metallurgy, the alloy magneto-caloric material being related in a kind of magnetic refrigerating field, especially a kind of room temperature
Magnetic refrigeration alloy material and preparation method.
Background technology
With a large amount of consumption of traditional energy, the pressure of environmental protection, the new energy such as development magnetic refrigeration have been compeled in eyebrow in addition
Eyelash.For traditional vapor compression refrigeration etc., magnetic freezes with efficient, low noise, floor space is small and is using
Not the advantages that not will produce any pollution in the process.Refrigeration is realized by the magnetothermal effect of magnetic material itself, will necessarily be become
The mankind solve the important channel of energy and environmental problem.But compared with other refrigeration modes, magnetic refrigeration technology also less at
Ripe, especially soon, Curie temperature and room temperature deviation are larger for the research ability ground zero of room temperature magnetic refrigerating, heat stagnation and magnetic hysteresis compared with
It is the key that restrict magnetic refrigeration development that greatly and magnetothermal effect is smaller etc..Therefore, how to make the Curie temperature tune of magnetic refrigerating material
Control reduces the heat stagnation and magnetic hysteresis of material, and it is for a long time to obtain larger magnetothermal effect near room temperature near room temperature
People endeavour to solve the problems, such as always, and a key factor of room temperature magnetic refrigerating development is exactly that Curie temperature is too high or too low,
Nearby heat stagnation magnetic hysteresis is larger for phase transformation, and near room temperature magnetothermal effect is smaller, i.e., larger magnetothermal effect is obtained near room temperature.We
Know, MnCoGe alloys are typical martensitic traoformation alloys, because its significant magnetic characteristic and magnetic heating performance are considered to be one kind
One of ideal magneto-caloric material, alloy are in hexagonal in 650K recurring structure phase transformations, the orthogonal thereto TiNiSi structures of low temperature, high temperature
Ni2In structures.It is respectively 275K and 345K in the Curie temperature of hexagonal structure and orthogonal type structure.But MnCoGe alloy structure phases
Change occurs mainly in paramagnetic state, and magnetization change is little, without apparent application value.Therefore, for how to regulate and control
The Curie temperature of MnCoGe alloys avoids the appearance and raising in the larger heat stagnation of near room temperature, magnetic hysteresis near room temperature again simultaneously
It is the key that in room temperature magnetic refrigerating material design, preparation that near room temperature magnetothermal effect, which carries out research,.
Currently, a large amount of detailed research work has been done in home and abroad to design, the preparation etc. of MnCoGe alloys, master
It wants there are three types of technological means：Interstitial atom is adulterated, the chemical composition of compound is changed, is substituted using transition group atom.Especially
Good magnetothermal effect is had been achieved in preparation to the replacement of MnCoGe alloy atoms.But since preparation method and raw material are pure
The limitations such as degree so that MnCoGe is still not satisfactory in the magnetothermal effect of near room temperature at present.This is because main research at present
The progress to work acquired by MnCoGe bases, mainly makes the structural phase transition of material be coupled with magnetic phase transition and has obtained huge magnetic thermal effect
It answers, but incident many still unresolved for room temperature magnetic refrigerating, if Curie temperature is excessively high or too low, near room temperature
Magnetothermal effect is smaller, first order phase change evident characteristic：Smaller half-peak breadth and larger heat stagnation.Prepared by generally conventional method
MnCoGe based alloys are usually first order phase change material.And the magnetic entropy of first order phase change material becomes considerable, but in refrigeration temperature controllable
Wide and magnetothermal effect utilization is often unsatisfactory.In recent years, second-order phase transistion material is special to material science research, including material
Property, new material synthesis and new diseases, produce great influence.Related research is it has been shown that carry out MnCoGe alloys
Element substitution technology, can be promoted MnCoGe alloys magnetic Refrigeration Technique competitiveness.For room temperature magnetic refrigerating, refrigeration is improved
The key of efficiency is to obtain larger magnetothermal effect near room temperature first secondly have smaller heat stagnation and larger temperature controllable
It is wide.And for general material, magnetothermal effect is all bigger, and but meet simultaneously near room temperature with larger magnetic thermal effect
Larger heat stagnation is avoided while answering again, this must just improve original technology of preparing, improve the microstructure of alloy, to subtract
Small heat stagnation and larger magnetothermal effect is obtained near room temperature.With the further investigation of MnCoGe alloys so that it is huge to prepare room temperature
The second-order phase transistion material of magnetothermal effect has become possibility, though there is the much research about MnCoGe based alloys both at home and abroad, but still
Lack research of the MnCoGe based alloys in room temperature magnetic refrigerating field to report.
Invention content
For above-mentioned technical problem in the prior art, the present invention provides a kind of room temperature magnetic refrigerating alloy material and preparations
Method, this room temperature magnetic refrigerating alloy material and preparation method solve to be existed in MnCoGe alloys in the prior art
Larger heat stagnation problem, Curie temperature be excessively high, too low, the wide smaller technical problem of temperature controllable.
The present invention provides a kind of room temperature magnetic refrigerating alloy material, molecular formula Mn1-XAlXCoGe, in the room temperature
Magnetic freezes in alloy material, and the mass percent of manganese element is 33.3~34.4%, and the mass percent of aluminium element is 0.6~
2.7%, the mass percent of cobalt element is 32.8~33.3%, and the mass percent of Germanium is 30.2~32.7%.
Further, X is 0.02~0.08.
Further, when the doping content of the Al is 0.02~0.08, Curie temperature is promoted to 301K by 271K,
Under the changes of magnetic field of 5T, maximum magnetic entropy variable is:3.21J·Kg-1K-1, 2.76JKg-1K-1, 2.4JKg-1K-1, 2.34J
Kg-1K-1, it is with respect to refrigerating capacity:242.2J·Kg-1, 109.1JKg-1, 102.2JKg-1, 101.8JKg-1, temperature controllable
It is wide：75.5K, 79K, 85K, 87K.
The present invention also provides the preparation methods of above-mentioned room temperature magnetic refrigerating alloy material, include the following steps：
1) high-purity manganese powder, aluminium powder, cobalt powder and germanium powder are weighed according to mass percent, the purity of above-mentioned substance >=
99.9%；
2) above-mentioned load weighted reactive material is added in vacuum arc furnace ignition, with mechanical pump by vacuum arc furnace ignition sample cavity
It vacuumizes and is less than 5Pa, open molecular pump and be evacuated to again less than 10-4Pa, is passed through the high purity argon of air pressure 10Pa, repeat with
On vacuumize and scrubbing operations step 1~3 time；
3) it uses the electric current of 25~35A on fire, electrode is moved to right over sample apart from 0.4~0.8cm of sample, by electric current
70~90A is adjusted to until sample melts completely, then electric current 55~65A meltings is down to 0.3~0.6 minute, waits for alloy cooling pair
It turns over, melt back 2~5 times；
4) sample cooling is taken out, sample is put into high temperature resistant quartz glass test tube, is taken out using hight atmospheric molecular pumping system
Vacuum is filled with high purity argon and carries out gas washing, repeat above step 2~4 times, sealed silica envelope is put into stove formula case to 5Pa is less than
In 800~900 DEG C anneal 5~8 days, it is to be made annealing treatment in 5~12 DEG C of cold water to take out sample and be put into temperature, obtains room temperature magnetic system
Cold alloy material.
Further, the manganese powder purity is 99.9%, and aluminium powder purity is 99.95%, and cobalt powder aluminium element purity is
99.95%, the purity of germanium powder is 99.99%.
Further, the purity of the argon gas is 99.999%.
The present invention proposes a kind of MnAlCoGe alloys of Mn doping trace of Al, at room temperature orthogonal thereto TiNiSi knots
Structure, doping of the structure by Al to Mn make to obtain wide larger temperature controllable and refrigerating capacity and alloy near room temperature
Two level magnetic phase transition occurs near room temperature, to preferably solve the problems such as Curie temperature is excessively high, too low, heat stagnation is larger.It is logical
The aluminium content in adjustment magnetic material is crossed, is capable of the crystal structure of more preferable controlled material, effectively drops the Curie temperature of alloy
Have larger temperature controllable wide near room temperature, and near room temperature.The temperature controllable of the room temperature magnetic refrigerating material is wide：
75.5K, 79K, 85K, 87K and routine MnCoGe (343K, 5.8JKg-1K-1, 227JKg-1, 60K) and alloy compares, it will be apparent that
So that alloy Curie temperature is down to room temperature and has larger temperature controllable wide near room temperature.
Compared with prior art, the present invention its technological progress is significant.The present invention is using trace of Al to MnCoGe chemical combination
Mn doping of object show that the micro Al of the Mn doping significantly makes alloy Curie temperature be down to room temperature by survey calculation
The alloy for nearby and near room temperature having larger temperature controllable wide and obtained is second-order phase transistion material, is effectively avoided
First order phase change material strips come heat stagnation problem, for MnCoGe systems alloy the development of room temperature magnetic refrigerating and apply provide it is advantageous
Foundation.
The MnAlCoGe room temperature magnetic refrigerating alloy materials of the present invention are small with heat stagnation, adjustable warm area is big, prepare simple etc. excellent
Point can provide preparation parameter for the development of room temperature magnetic refrigerating, can be applied to such as high-energy physics, cryogenic engineering precision instrument, electricity
Power industry, superconducting technology, medical instrument etc. are related to numerous key areas of national economy.
Description of the drawings
Fig. 1 Mn1-xAlxCoGe (x=0.02,0.04,0.06,0.08) Alloy At Room Temperature XRD diffraction patterns.
Fig. 2 Mn1-xAlxThe M-T that CoGe alloys are 0.02T in magnetic field schemes.
Fig. 3 Mn1-xAlxIsothermal magnetization curve of the CoGe alloys near Curie temperature.
Fig. 4 Mn1-xAlxArrott curve of the CoGe compounds near Curie temperature.
Fig. 5 Mn1-xAlxIsothermal magnetic entropy varied curve of the CoGe alloys under 2T and 5T changes of magnetic field.
Specific implementation mode
Embodiment 1
The use of the purity of raw material is 99.9%Mn, 99.95%Al, 99.9%Co, 99.99%Ge, according to mass percent
Each powder is weighed, the mass percent of manganese element is 33.3~34.4%, and the mass percent of aluminium element is 0.6~2.7%, cobalt
The mass percent of element is 32.8~33.3%, and the mass percent of Germanium is 30.2~32.7%.
Alloy uses vacuum arc furnace melting method, and each element is added in vacuum arc furnace ignition, first before alloy melting
It is first vacuumized less than 5Pa with mechanical pump, opens molecular pump and be evacuated to again less than 10-4Pa is passed through the high-purity of air pressure 10Pa
Argon gas (99.999%), repetition is above to be vacuumized with scrubbing operations step twice, on fire using the electric current of 30A or so, by electrode
It moves to right over sample apart from sample 0.5cm or so, electric current is slowly adjusted to 80A or so until sample melts completely, then will be electric
Stream is down to 60A melting half a minute, waits for that sample bottom is turned to top by alloy cooling, melt back four times is to ensure that sample is uniform
Degree.Sample is put into high-purity high temperature resistant quartz glass test tube after taking out cooling, is evacuated to and is less than using hight atmospheric molecular pumping system
5Pa is filled with high purity argon (99.999%) and carries out gas washing, repeats above step three times, sealed silica envelope is put into stove formula case
850 DEG C are annealed 7 days to ensure good crystallinity, are taken out sample and are put into rapidly in the cold water that temperature is 10 DEG C or so at annealing
Manage
The present invention is prepared for Mn by vacuum arc furnace melting method1-xAlxCoGe alloys, x-ray diffraction experiment show institute
The good main orthogonal thereto TiNiSi structures at room temperature of the alloy crystallinity of preparation.Physical measurement (PPMS-9T) the result shows that, Al
Incorporation reduce the Curie temperature of alloy, make alloy have larger temperature controllable wide larger to obtain near room temperature
Refrigerating capacity, alloy mutually becomes second-order phase transistion near Curie temperature.
Mn1-xAlxCoGe (x=0.02,0.04,0.06,0.08) Alloy At Room Temperature XRD diffraction patterns are as shown in Figure 1, all samples
Product crystallinity is good, at room temperature the main orthogonal thereto TiNiSi structures of all samples, while having a small amount of hexagonal Ni2In structures.
Fig. 2 is magnetic variationization M-T (FC-ZFC) figure off field of alloy in 0.02T, and illustration is that the Al content of alloy is 0.08
When, the Curie temperature of alloy, alloy occurs near Curie temperature by the ferromagnetic magnetic phase transition to paramagnetic, and Curie temperature is schemed by M-T
Slope variation maximum value acquires, and 301K is risen to by 271K with the increase Curie temperature of Al doping contents.
Fig. 3 provides the isothermal magnetization curve M-H of alloy near Curie temperature under the changes of magnetic field of 0-7T, can by M-H figures
Know, it is larger in the magnetization change of near Curie temperature alloy, it is consistent with M-T analyses.
Fig. 4 is Arrott curve of the alloy near Curie temperature, further to analyze the magnetic property of alloy, from
It can be seen that all sample near Curie temperature slope of a curve is that positive value shows that all samples exist in Arrott curves
Two level magnetic phase transition occurs near Curie temperature, illustrates that all samples only have smaller heat stagnation near transformation temperature, effectively
The first order phase change larger problem of heat stagnation nearby is avoided, the utilization ratio of the energy is improved.
Fig. 5 is isothermal magnetic entropy varied curve of the series alloy under 2T and 5T changes of magnetic field, second-order phase transistion magnetic refrigerating material
The change of isothermal magnetic entropy can be obtained by Maxwell equations：
The numerical value in (1) in equation can be write as following formula with trapezoidal rule
M in formulai+1And MiRespectively Ti+1And TiWhen the intensity of magnetization.Then, we combine the experimental result of Fig. 3, and utilize
(2) formula calculates the isothermal magnetic entropy that the sample is shown under different magnetic field and becomes.The result shows that：Under the changes of magnetic field of 2T,
Maximum isothermal magnetic entropy becomes:1.75J·Kg-1K-1, 1.48JKg-1K-1, 1.28JKg-1K-1, 1.23JKg-1K-1, in 5T
Changes of magnetic field under, maximum isothermal magnetic entropy becomes:3.21J·Kg-1K-1, 2.76JKg-1K-1, 2.4JKg-1K-1, 2.34J
Kg-1K-1。
In addition, another important parameter of evaluation magnetothermal effect is the opposite refrigerating capacity (RCP) of magneto-caloric material, RCP can be expressed
For：
According to above formula, we calculate Mn1-xAlxCoGe (x=0.02,0.04,0.06,0.08) alloy changes in magnetic field
Refrigerating capacity is respectively 242.2JKg under the conditions of 5T-1, 109.1JKg-1, 102.2JKg-1, 101.8JKg-1, temperature controllable
It is wide：75.5K, 79K, 85K, 87K.As it can be seen that by adjusting the content of the Al in MnCoGe magnetic materials, conjunction can be preferably controlled
The crystal structure of gold effectively makes the Curie temperature of alloy material be down near room temperature and have near room temperature larger adjustable
Warm wide and larger refrigerating capacity.With conventional MnCoGe (227JKg-1, 60K) and alloy compares, it will be apparent that improve magnetic material
Curie temperature and magnetothermal effect.And obtained alloy material is second-order phase transistion material, effectively avoids heat stagnation problem.
Claims (5)
1. a kind of room temperature magnetic refrigerating alloy material, it is characterised in that：Its molecular formula is Mn1-XAlXCoGe, in the room temperature magnetic system
X is 0.02 ~ 0.08 in cold alloy material.
2. room temperature magnetic refrigerating alloy material according to claim 1, it is characterised in that：As x=0.02 0.04 0.06
When 0.08, with the increase of Al doping contents, Curie temperature is promoted to 301K by 271K, under the changes of magnetic field of 5T, maximum magnetic flux
Entropy Changes is:3.21 J·kg-1K-1, 2.76 Jkg-1K-1, 2.4 Jkg-1K-1, 2.34 Jkg-1K-1, opposite refrigerating capacity
For: 242.2 J·kg-1, 109.1 Jkg-1, 102.2 Jkg-1, 101.8 Jkg-1, temperature controllable is wide：75.5K, 79K,
85K, 87K.
3. the preparation method of room temperature magnetic refrigerating alloy material described in claim 1, it is characterised in that include the following steps：
1）High-purity manganese powder, aluminium powder, cobalt powder and germanium powder are weighed according to mass percent, the purity of above-mentioned substance is >=99.9%；
2）Above-mentioned load weighted reactive material is added in vacuum arc furnace ignition, is less than vacuum arc stove evacuation with mechanical pump
5Pa opens molecular pump and is evacuated to again less than 10-4Pa, is passed through the high purity argon of air pressure 10Pa, repeat it is above vacuumize and
Scrubbing operations step 1 ~ 3 time；
3）It is on fire using the electric current of 25 ~ 35A, electrode is moved to right over sample apart from 0.4 ~ 0.8cm of sample, electric current is adjusted to 70
~ 90A melts completely up to sample, then electric current is down to 55 ~ 65A meltings 0.3 ~ 0.6 minute, waits for that bottom is turned to top by alloy cooling
Portion, melt back 2 ~ 5 times；
4）Sample cooling is taken out, sample is put into high temperature resistant quartz glass test tube, is vacuumized using hight atmospheric molecular pumping system
To 5Pa is less than, it is filled with high purity argon and carries out gas washing, repeat above step 2 ~ 4 times, sealed silica envelope is put into 800 in stove formula case
~ 900 DEG C are annealed 5 ~ 8 days, are taken out sample and are put into temperature to be made annealing treatment in 5 ~ 12 DEG C of cold water, obtain room temperature magnetic refrigerating alloy material
Material.
4. the preparation method of room temperature magnetic refrigerating alloy material according to claim 3, it is characterised in that：The manganese powder
Purity is 99.9%, and the purity of aluminium powder is 99.95%, and the purity of cobalt powder is 99.9%, and the purity of germanium powder is 99.99%.
5. the preparation method of room temperature magnetic refrigerating alloy material according to claim 3, it is characterised in that：The argon gas
Purity is 99.999%.
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| CN107760962B (en) * | 2017-10-17 | 2020-05-08 | 上海电力学院 | Magnetic refrigeration alloy material and preparation method thereof |
| CN112430757A (en) * | 2020-10-19 | 2021-03-02 | 北京工业大学 | MnCoGe-based magnetic alloy capable of being used as magnetic refrigeration material |
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| CN1584082A (en) * | 2004-06-09 | 2005-02-23 | 北京科技大学 | Compounds with large magnetic entropy changes and their preparation |
| CN1750181A (en) * | 2005-10-20 | 2006-03-22 | 中国科学院物理研究所 | Semimetal magnetic material with high spinning polarizability |
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| CN103710605B (en) * | 2012-09-28 | 2016-06-29 | 中国科学院物理研究所 | A kind of ferromagnetic Martensitic Transformation Materials of MnCoGe base with big Entropy Changes and preparation method and purposes |
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| CN1584082A (en) * | 2004-06-09 | 2005-02-23 | 北京科技大学 | Compounds with large magnetic entropy changes and their preparation |
| CN1750181A (en) * | 2005-10-20 | 2006-03-22 | 中国科学院物理研究所 | Semimetal magnetic material with high spinning polarizability |
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