CN105714173B - A kind of manganese cobalt germanium-base alloy magnetic refrigerating material and its preparation - Google Patents
A kind of manganese cobalt germanium-base alloy magnetic refrigerating material and its preparation Download PDFInfo
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- CN105714173B CN105714173B CN201610268488.5A CN201610268488A CN105714173B CN 105714173 B CN105714173 B CN 105714173B CN 201610268488 A CN201610268488 A CN 201610268488A CN 105714173 B CN105714173 B CN 105714173B
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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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- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- 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
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
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Abstract
The present invention relates to a kind of manganese cobalt germanium-base alloy magnetic refrigerating material and its preparation, the general molecular formula of described magnetic refrigerating material is MnCoGe1‑xCux, wherein, x span is 0.005~0.05；It is prepared from by following steps：(1) according to mol ratio 1：1：(1‑x)：X weighs manganese, cobalt, germanium and copper product, and heating is melted and is well mixed under inert gas shielding, obtains biased sample；(2) biased sample is taken out, annealing obtains purpose product.Compared with prior art, Curie temperature and magnetothermal effect of the present invention with magnetic refrigerating material are good, and magnetic refrigerating material is second-order phase transistion material, effectively avoid coming the heat stagnation problem that first order phase change material strips are come, the advantages of preparing simple and easy to apply.
Description
Technical field
The present invention relates to the alloy magnetic refrigeration material in a kind of magnetic refrigerating field, more particularly, to a kind of manganese cobalt germanium copper alloy
Magnetic refrigerating material and its preparation.
Background technology
Nearly room temperature magnetic refrigerating development is at a low ebb at present, and it is that its heat stagnation, magnetic hysteresis are larger to trace it to its cause, and temperature controllable is wide and refrigeration
Amount is smaller, and cost is too high to be caused；And with the pressure of a large amount of consumption of traditional energy, in addition environmental protection, development magnetic refrigeration etc.
New energy is extremely urgent.For traditional vapor compression refrigeration etc., magnetic refrigeration is with efficiency high, noise is low, take up an area
Area is small and the features such as will not producing any pollution in use.System is realized by the magnetothermal effect of magnetic material in itself
It is cold, the important channel that the mankind solve the energy and environmental problem will necessarily be turned into.But, compared with other refrigeration modes, magnetic refrigeration
Technology it is also not overripened, particularly the research ability ground zero of room temperature magnetic refrigerating soon, larger heat stagnation and magnetic hysteresis, and compared with
Small magnetothermal effect is the key for restricting magnetic refrigeration development.Therefore, how to reduce heat stagnation and magnetic hysteresis, nearly near room temperature obtain compared with
Big magnetothermal effect is the problem of people endeavour to solve always for a long time, and a key factor of room temperature magnetic refrigerating development is just
It is smaller in nearly near room temperature magnetothermal effect, i.e., larger magnetothermal effect is obtained near room temperature.It is known that MnCoGe alloys
Typical martensitic traoformation alloy, because its significant magnetic characteristic and magnetic heating performance be considered to be a kind of preferable magneto-caloric material it
One, the MnCoGe alloys just divided are a simple ferromagnets, and at room temperature with orthogonal TiNiSi structures, Curie temperature is about
345K, in about 650K, MnCoGe alloys can occur one from orthogonal TiNiSi to hexagonal Ni2In structural phase transition.But MnCoGe
Alloy structure phase transformation occurs mainly in paramagnetic state, and magnetization change is little, without obvious application value.Therefore, for such as
The structural phase transition of what reduction MnCoGe alloy and the nearly room temperature magnetothermal effect of raising, which carry out research, to be nearly room temperature magnetic refrigerating design, prepares
In key.
At present, substantial amounts of detailed research work has been done in home and abroad to design, preparation of MnCoGe alloys etc., and it is led
Technological means is wanted there are three kinds：Adulterate interstitial atom, changes the chemical composition of compound, is substituted using transition group atom.Particularly
Replacement to MnCoGe alloy atoms has been achieved for good magnetothermal effect in preparation.But because preparation method and raw material are pure
The limitation such as degree so that current MnCoGe is still not ideal in the magnetothermal effect of nearly near room temperature.Because, it is main at present to grind
Study carefully the replacement that work concentrates on Mn and Co atoms, although these are operated in nearly near room temperature and have been obtained for huge magnetic thermal effect
Should, but incident first order phase change evident characteristic：Less half-peak breadth and larger heat stagnation, still without solution.It is generally conventional
Method prepare MnCoGe based alloys be usually first order phase change material.And first order phase change material is wide warm with magnetic in refrigeration temperature controllable
The utilization of effect is often unsatisfactory, such as Mn1-xCuxCoGe, in x=0.085, under 5T changes of magnetic field, the isothermal magnetic of alloy
Entropy Changes can reach 53.3JKg-1K-1, but there is larger heat stagnation during alloy phase change and less temperature controllable is wide.In recent years,
Second-order phase transistion material generates important shadow to material science research, including the synthesis of material property, new material and new diseases
Ring.Relevant research is it has been shown that to MnCoGe alloys progress element substitution technology, can lift MnCoGe alloys in magnetic refrigeration skill
The competitiveness of art.For room temperature magnetic refrigerating, the key for improving refrigerating efficiency is to obtain larger magnetic heat in nearly room temperature first
Effect, secondly has smaller heat stagnation and larger temperature controllable wide.And for general material, magnetothermal effect all than larger,
And but meet simultaneously larger heat stagnation is avoided while the larger magnetothermal effect of nearly room temperature, this must just improve original preparation
Technology, improves the microstructure of alloy, so as to reduce heat stagnation and obtain larger magnetothermal effect.With going deep into for MnCoGe alloys
Research so that the second-order phase transistion for preparing nearly room temperature giant magnetio-caloric effects is possibly realized, though have many on the conjunction of MnCoGe bases both at home and abroad
The research of gold, but still lack the research to the Ge doping of MnCoGe bases.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of manganese cobalt germanium-base alloy
Magnetic refrigerating material and its preparation.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of manganese cobalt germanium-base alloy magnetic refrigerating material, its general molecular formula is MnCoGe1-xCux, wherein, x span is
0.005~0.05.
X span is 0.01~0.04.
The preparation method of manganese cobalt germanium-base alloy magnetic refrigerating material, comprises the following steps：
(1) manganese, cobalt, germanium and copper product are weighed, heating is melted and is well mixed under inert gas shielding, obtains aggregate sample
Product；
(2) biased sample is taken out, annealing obtains purpose product.
The air pressure of inert gas is 5~15Pa in step (1).
The processing step of annealing is in step (2)：First under inert gas shielding, in annealing 5 at 800~900 DEG C
~10 days, then annealing in 10~30 DEG C of water is placed in, processing time is about 2min or so.
Described inert gas is argon gas.
The present invention is finally made by employing micro Cu in MnCoGe architectures to the Ge doping of MnCoGe compounds
Obtain MnCoGe1-xCuxAlloy magnetic refrigeration material.Find afterwards after testing, when it is 0.01~0.04 that Cu replaces content x to Ge, Curie
Temperature (TC) 363K is risen to by 353K, under 5T changes of magnetic field, maximum magnetic entropy variable is：18.3JKg-1K-1, 12.9JKg-1K-1, 15.3JKg-1K-1, 6.8JKg-1K-1, it is with respect to refrigerating capacity：292.5JKg-1, 206.9JKg-1, 260.5JKg-1, 242.4JKg-1；With conventional MnCoGe (343K, 5.8JKg-1K-1, 227JKg-1) alloy compares, it will be apparent that improve Curie's temperature of magnetic material
Degree and magnetothermal effect.
Compared with prior art, the present invention has advantages below：
(1) present invention is by the Ge positions doping micro Cu in MnCoGe architectures, and then significantly improves magnetic material
Curie temperature and magnetothermal effect, and obtained alloy is second-order phase transistion material, effectively avoids first order phase change material strips
The heat stagnation problem come.
(2) preparation method is simple, it is easy to accomplish, cheap, application prospect extensively, can be applied to be related to refrigeration and low temperature
Numerous key areas of the national economy of technology, such as high-energy physics, cryogenic engineering, Aero-Space, precision instrument, petrochemical industry,
Power industry, superconducting technology, medicine equipment etc..
Brief description of the drawings
Fig. 1 is magnetic refrigerating material MnCoGe of the invention1-xCux(x=0.01,0.02,0.03,0.04) room temperature XRD spreads out
Penetrate figure；
Fig. 2 is magnetic refrigerating material MnCoGe of the invention1-xCuxSeries alloy M-T in outfield 0.02T schemes；
Fig. 3 is magnetic refrigerating material MnCoGe of the invention1-xCuxSeries alloy is bent in the isothermal magnetization of near Curie temperature
Line；
Fig. 4 is magnetic refrigerating material MnCoGe of the invention1-xCuxArrott curve of the series alloy in vicinity of Curie temperatures；
Fig. 5 is magnetic refrigerating material MnCoGe of the invention1-xCuxSeries alloy respectively under 2T and 5T changes of magnetic field etc.
Warm magnetic entropy varied curve；
Fig. 6 is magnetic refrigerating material MnCoGe of the invention1-xCuxThe maximum magnetic flux of series alloy respectively under 5T changes of magnetic field
Entropy Changes and H2/3Curve.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
According to mol ratio 1:1:0.99:0.01 weighs purity for 99.9%Mn, 99.9%Co, 99.99%Ge, 99.9%
Cu, is placed in vacuum arc furnace melting, specifically before alloy melting, is evacuated to first with mechanical pump less than 5Pa, opens molecular pump
It is evacuated to again less than 10-4Pa, is passed through air pressure 10Pa high purity argon (99.999%), repeats above operating procedure two
Secondary, on fire with 30A electric currents, the distance of electrode and sample is 0.5cm or so, slowly by current-modulation 80A until sample melts completely
Change, then electric current is down to 60A melting half a minute, treat alloy cooling to turning over, melt back four times is to ensure that sample is well mixed.Take
Go out sample after cooling and be put into high-purity high temperature resistant quartz glass test tube, be evacuated to less than 5Pa, filled using hight atmospheric molecular pumping system
Enter high purity argon (99.999%) and carry out gas washing, repeat above step three times, sealed silica envelope is put into stove formula case 850 DEG C
Annealing takes out sample annealing 2min or so in temperature is 15 DEG C of cold water, that is, obtains mesh for 7 days to ensure good crystallinity
Product MnCoGe1-xCuxAlloy.
Embodiment 2
Except the ratio between mole addition between Mn, Co, Ge and Cu is 1:1:0.98:Outside 0.02, remaining all same.
Embodiment 3
Except the ratio between mole addition between Mn, Co, Ge and Cu is 1:1:0.97:Outside 0.03, remaining all same.
Embodiment 4
Except the ratio between mole addition between Mn, Co, Ge and Cu is 1:1:0.96:Outside 0.04, remaining all same.
To MnCoGe made from above-described embodiment 1-41-xCuxAlloy detected, MnCoGe1-xCux(x=0.01,0.02,
0.03,0.04) Alloy At Room Temperature XRD diffraction patterns are as shown in figure 1, all samples crystallinity is good, and all samples are main at room temperature
Orthogonal thereto TiNiSi structures, while there is a small amount of hexagonal Ni2In structures.
Fig. 2 is outer M-T (FC-ZFC) figure off field of alloy in 0.02T, and illustration is the Curie temperature and temperature of alloy
Relation, alloy occurs by the ferromagnetic magnetic phase transition to paramagnetic near Curie temperature, and Curie temperature is by M-T figure slope variation maximums
Try to achieve, it is known that, as the increase Curie temperature of Cu doping contents by 353K rises to 363K.
Fig. 3 is the isothermal magnetization curve M-H of obtained alloy near Curie temperature under 0~7T magnetic fields, is schemed from M-H
Near Curie temperature magnetization change is larger, consistent with M-T analyses.
Fig. 4 is Arrott curve of the obtained alloy near Curie temperature, it can be seen that all from Arrott curves
Sample near Curie temperature slope of a curve be on the occasion of this shows that all samples occur two grades near Curie temperature
Magnetic phase transition, illustrates that all samples only have less heat stagnation near transformation temperature, effectively avoids first order phase change heat stagnation nearby
Larger the problem of, improve the utilization ratio of the energy.
Fig. 5 is the isothermal magnetic entropy varied curve under obtained alloy material 2T and 5T changes of magnetic field, second-order phase transistion magnetic refrigeration material
The isothermal magnetic entropy of material, which becomes, to be obtained by Maxwell equations：
The numerical value in (1) in equation can be write as following formula with trapezoidal rule
In formula, H is magnetic field intensity；T is measurement temperature；Mi+1And MiRespectively Ti+1And TiWhen the intensity of magnetization.Then, I
Combine Fig. 3 experimental result, and utilize (2) formula to calculate the isothermal magnetic entropy that the sample shown under different magnetic field to become.
As a result show：Under 2T changes of magnetic field, maximum isothermal magnetic entropy is changed into：7.05JKg-1K-1(x=0.01), 4.96JKg-1K-1(x
=0.02), 5.84JKg-1K-1(x=0.03), 2.87JKg-1K-1(x=0.04), under 5T changes of magnetic field, maximum isothermal magnetic
Entropy Changes is：18.3JKg-1K-1(x=0.01), 12.9JKg-1K-1(x=0.02), 15.3JKg-1K-1(x=0.03), 6.8JKg- 1K-1(x=0.04).
In addition, another important parameter for evaluating magnetothermal effect is the relative refrigerating capacity (RCP) of magneto-caloric material, RCP can be expressed
For
Become corresponding half-peak breadth for maximum isothermal magnetic entropy, we calculate MnCoGe according to above formula1-xCuxClose
Gold magnetic field change under the conditions of RCP be respectively 2T when：113.8JKg-1(x=0.01), 79.4JKg-1(x=0.02),
99.2JKg-1(x=0.03), 97.7JKg-1(x=0.04)；During 5T：292.5JKg-1(x=0.01), 206.9JKg-1(x=
0.02), 260.5JKg-1(x=0.03), 242.4JKg-1(x=0.04).It can be seen that, by adjusting containing for the copper in magnetic material
Amount, can better control over the crystal structure of material, effectively raise Curie temperature and the magnetothermal effect of magnetic material.With it is normal
Advise MnCoGe (343K, 5.8JKg-1K-1, 227JKg-1) alloy compares, it will be apparent that improve the Curie temperature and magnetic of magnetic material
Fuel factor.And obtained alloy material is second-order phase transistion material, effectively avoids heat stagnation problem.
Fig. 6 is the maximum magnetic entropy variable and H of different-alloy respectively under 5T changes of magnetic field2/3Curve, recent studies have shown that
In the case of second-order phase transistion, the maximum magnetic entropy variable of alloy and and H2/3Certain linear relationship, such as theory based on mean field is presented：
Every mole of q magnetic ion number in formula, R is gas constant, g Lande factors, the total angular-momentum quantum numbers of J, kBFor Boltzmann
Constant, as shown in Figure 6 | Δ SM| with H2/3It is linear, indicate the feature of second-order phase transistion.With Arrott map analysis result one
Cause.
Embodiment 5
According to mol ratio 1:1:0.995:0.005 weighs purity for 99.9%Mn, 99.9%Co, 99.99%Ge, 99.9%
Cu, is placed in vacuum arc furnace melting, specifically before alloy melting, is evacuated to first with mechanical pump less than 5Pa, opens molecular pump
It is evacuated to again less than 10-4Pa, is passed through air pressure 5Pa high purity argon (99.999%), repeats above operating procedure twice,
On fire with 30A electric currents, the distance of electrode and sample is 0.5cm or so, slowly by current-modulation 80A until sample melts completely,
Electric current is down to 60A melting half a minute again, alloy cooling is treated to turning over, melt back four times is to ensure that sample is well mixed.Take out
Sample is put into high-purity high temperature resistant quartz glass test tube after cooling, is evacuated to less than 5Pa, is filled with using hight atmospheric molecular pumping system
High purity argon (99.999%) carries out gas washing, repeats above step three times, sealed silica envelope, is put into stove formula case 800 DEG C and moves back
Fire takes out sample annealing 2min or so in temperature is 30 DEG C of cold water, that is, obtains mesh for 10 days to ensure good crystallinity
Product MnCoGe1-xCuxAlloy.
Embodiment 6
According to mol ratio 1:1:0.95:0.05 weighs purity for 99.9%Mn, 99.9%Co, 99.99%Ge, 99.9%
Cu, is placed in vacuum arc furnace melting, specifically before alloy melting, is evacuated to first with mechanical pump less than 5Pa, opens molecular pump
It is evacuated to again less than 10-4Pa, is passed through air pressure 15Pa high purity argon (99.999%), repeats above operating procedure two
Secondary, on fire with 30A electric currents, the distance of electrode and sample is 0.5cm or so, slowly by current-modulation 80A until sample melts completely
Change, then electric current is down to 60A melting half a minute, treat alloy cooling to turning over, melt back four times is to ensure that sample is well mixed.Take
Go out sample after cooling and be put into high-purity high temperature resistant quartz glass test tube, be evacuated to less than 5Pa, filled using hight atmospheric molecular pumping system
Enter high purity argon (99.999%) and carry out gas washing, repeat above step three times, sealed silica envelope is put into stove formula case 900 DEG C
Annealing takes out sample annealing 2min or so in temperature is 10 DEG C of cold water, that is, obtains mesh for 5 days to ensure good crystallinity
Product MnCoGe1-xCuxAlloy.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using invention.
Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without passing through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel are according to the announcement of the present invention, and not departing from improvement and modification that scope made all should be the present invention's
Within protection domain.
Claims (6)
1. a kind of manganese cobalt germanium-base alloy magnetic refrigerating material, it is characterised in that its general molecular formula is MnCoGe1-xCux, wherein, x's takes
It is 0.005~0.05 to be worth scope.
2. a kind of manganese cobalt germanium-base alloy magnetic refrigerating material according to claim 1, it is characterised in that x span is
0.01~0.04.
3. the preparation method of manganese cobalt germanium-base alloy magnetic refrigerating material as claimed in claim 1 or 2, it is characterised in that including with
Lower step：
(1) in molar ratio 1：1：(1-x)：X weighs manganese, cobalt, germanium and copper product, and heating is melted and mixed under inert gas shielding
It is even, obtain biased sample；
(2) biased sample is taken out, annealing obtains purpose product.
4. a kind of preparation method of manganese cobalt germanium-base alloy magnetic refrigerating material according to claim 3, it is characterised in that step
(1) air pressure of inert gas is 5~15Pa in.
5. a kind of preparation method of manganese cobalt germanium-base alloy magnetic refrigerating material according to claim 3, it is characterised in that step
(2) processing step of annealing is in：First under inert gas shielding, in annealing 5~10 days at 800~900 DEG C, then it is placed in
Made annealing treatment in 10~30 DEG C of water.
6. the preparation method of a kind of manganese cobalt germanium-base alloy magnetic refrigerating material according to claim 3, it is characterised in that described
Inert gas be argon gas.
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| CN106917029B (en) * | 2017-04-13 | 2018-08-21 | 佛山市程显科技有限公司 | A kind of ferromagnetic martensitic traoformation MM ' X-Y metal composite functional materials and preparation method thereof |
| CN107267839B (en) * | 2017-07-31 | 2018-08-07 | 上海电力学院 | A kind of room temperature magnetic refrigerating alloy magneto-caloric material and the preparation method and application thereof |
| CN107910150A (en) * | 2017-10-17 | 2018-04-13 | 上海电力学院 | A kind of alloy magnetic refrigeration working medium and preparation method thereof |
| CN107760962B (en) * | 2017-10-17 | 2020-05-08 | 上海电力学院 | Magnetic refrigeration alloy material and preparation method thereof |
| CN109266951B (en) * | 2018-09-25 | 2020-05-22 | 北京航空航天大学 | LaFeSiCu magnetic refrigeration alloy and preparation method thereof |
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| CN103710605A (en) * | 2012-09-28 | 2014-04-09 | 中国科学院物理研究所 | MnCoGe based martensite phase change material with large entropy change, and preparation method and application thereof |
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