CN101105996A - A kind of high temperature low magnetic field large magnetic entropy material compound and preparation method thereof - Google Patents
A kind of high temperature low magnetic field large magnetic entropy material compound and preparation method thereof Download PDFInfo
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- CN101105996A CN101105996A CNA2007100993777A CN200710099377A CN101105996A CN 101105996 A CN101105996 A CN 101105996A CN A2007100993777 A CNA2007100993777 A CN A2007100993777A CN 200710099377 A CN200710099377 A CN 200710099377A CN 101105996 A CN101105996 A CN 101105996A
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- 230000005291 magnetic effect Effects 0.000 title claims abstract description 87
- 239000000463 material Substances 0.000 title claims abstract description 37
- 150000001875 compounds Chemical class 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003723 Smelting Methods 0.000 claims abstract description 11
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000005457 ice water Substances 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 229910052779 Neodymium Inorganic materials 0.000 claims description 5
- 230000007704 transition Effects 0.000 claims description 5
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 241001062472 Stokellia anisodon Species 0.000 claims 1
- 238000010891 electric arc Methods 0.000 claims 1
- 238000005057 refrigeration Methods 0.000 abstract description 12
- 238000004378 air conditioning Methods 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 4
- 230000005290 antiferromagnetic effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000137 annealing Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 230000005415 magnetization Effects 0.000 description 4
- 230000005293 ferrimagnetic effect Effects 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 241000238366 Cephalopoda Species 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
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Abstract
一种高温低磁场大磁熵材料化合物及其制备方法，属于磁制冷材料技术领域。化合物的化学组成为La(FeyCo1－y)13－xAlx，1.50≥x≥1.2，y的取值从0.075到0.15。该材料的M2随μ0H/M变化的曲线在居里温度是线性的，并且居里温度大于305K，在磁场变化为2T下，最大磁熵变化值的绝对值大于3J/kg.K。制备方法为：将La、Fe、Co、Al原材料按化学组分进行配比，放入熔炼炉中，抽真空至4×10－3Pa以上，通入氩气，熔炼冷却后得到成份均匀的化合物。将熔炼获得的化合物在900～1100℃下均匀化处理120～360小时，然后放入冰水中。其优点在于：制备工艺相对简单，低磁场高温下磁熵变大，可以和Gd组成复合材料应用于磁制冷空调中。
A high-temperature, low-magnetic-field, high-magnetism-entropy material compound and a preparation method thereof belong to the technical field of magnetic refrigeration materials. The chemical composition of the compound is La(Fe y Co 1-y ) 13-x Al x , 1.50≥x≥1.2, and the value of y is from 0.075 to 0.15. The curve of the change of M2 of the material with μ 0 H/M is linear at the Curie temperature, and the Curie temperature is greater than 305K, and the absolute value of the maximum magnetic entropy change value is greater than 3J/kg.K when the magnetic field changes to 2T . The preparation method is as follows: mix La, Fe, Co, Al raw materials according to their chemical composition, put them into a smelting furnace, evacuate to above 4× 10-3 Pa, pass in argon, melt and cool to obtain a uniform composition compound. The compound obtained by smelting is homogenized at 900-1100° C. for 120-360 hours, and then put into ice water. Its advantages are: the preparation process is relatively simple, the magnetic entropy becomes larger under low magnetic field and high temperature, and it can form a composite material with Gd and be used in magnetic refrigeration and air conditioning.
Description
Technical field
The invention belongs to technical field of magnetic, a kind of high temperature low magnetic field large magnetic material and preparation method thereof particularly is provided.
Background technology
In recent years, because the magnetic Refrigeration Technique is considered to one of a kind of environmental protection, energy-efficient new Refrigeration Technique of future generation, has the magnetic refrigerating material exploratory development that huge magnetic entropy becomes and caused people's very big concern.To the application of magnetic Refrigeration Technique in air-conditioning, carried out detailed research especially.If but the magnetic Refrigeration Technique will be used for air conditioner refrigerating, need Curie temperature at room temperature and the big magnetic entropy material that is higher than room temperature.The material that the Curie temperature of now having reported is higher than the huge magnetic entropy change of having of room temperature has MnFeP
1-xAs
xBased compound, when x=0.55, Tc=305K, the magnetic entropy changing value Δ S when outside magnetic field changes 2T is 14Jkg
-1K
-1(US7069729B2), MnAs
1-xSb
xBased compound when temperature is higher than room temperature, has big magnetic entropy changing value (US6826915B2), and adding H in addition can be with La (Fe as interstitial atom
1-xSi
x)
13The Curie temperature of compound is brought up to the above and magnetic entropy changing value Δ S constant substantially (US7063754B2) of room temperature, for example at La (Fe
0.88Si
0.12)
13H
yIn when y=1.5, Tc=323K, the magnetic entropy changing value Δ S when outside magnetic field changes 2T is-19Jkg
-1K
-1Also has the Ni of report recently
55.5Mn
20Ga
24.5Alloy, Tc are greatly about 315K, and the magnetic entropy changing value Δ S when outside magnetic field changes 2T is for being about-15Jkg
-1K
-1(ZL200410009188.2) or the like.But, can not prepare in a large number now because the preparation process of above-mentioned material is all comparatively complicated.And, therefore be necessary to explore the magnetic refrigerating material that more Curie temperature is higher than room temperature because they are to belong to first order phase change, and heat stagnation that has and magnetic hysteresis are still waiting to overcome.
Cube NaZn
13La (the Fe of type
1-yCo
y)
13-xAl
xAlloy has high Curie temperature.It is reported La (Fe
1-xCo
x)
11.44Al
1.56When x=0.4, Tc=320K has magnetic entropy and becomes Δ S=-4.56Jkg under 5T
-1K
-1Bibliographical information La (Fe is also arranged
0.92Co
0.08)
11.83Al
1.17Curie temperature be 303K, and great magnetic entropy variation Δ S=-4.5Jkg is arranged when 2T
-1K
-1But, in this article,, need under 1273K, anneal 50 days in order to obtain uniform 1:13 phase.Therefore there is complex process, is not easy mass-produced problem.In addition, use as air-conditioning, also need Curie temperature to be higher than the material that big magnetic entropy is arranged of room temperature in order to make the magnetic refrigeration.Particularly at the material that under downfield, shows big magnetic entropy more than the room temperature.In order to solve this problem, the present invention proposes a kind of big magnetic entropy material of downfield that can be operated in more than the room temperature.
Summary of the invention
The object of the present invention is to provide a kind of high temperature low magnetic field large magnetic material and preparation method thereof, working temperature is higher than room temperature, and has great magnetic entropy variation compound and preparation method thereof under downfield, is suitable for the magnetic Refrigeration Technique of using in the refrigeration such as air-conditioning.
The present invention relates to a kind of La (Fe of the NaZn13 of having structure
yCo
1-y)
13-xAl
xMaterial is characterized in that 1.50 〉=x 〉=1.2, and La (Fe, M)
13(Al) the compound space group is Fm3c for M=Co, Si, and their magnetic performance is very responsive to the content of M.LaFe
11.37Al
1.63Two magnetic phase transitions of compound, one is first order phase change, another is a second-order phase transistion, along with the rising of temperature at first occurs occurring the second-order phase transistion of antiferromagnetic state to the paramagnetic attitude afterwards by the primary magnetic phase change of ferrimagnetic state to antiferromagnetic state.When material was in antiferromagnetic zone, downfield promptly can cause the change magnetic transition of antiferromagnetic state to ferrimagnetic state, shows LaFe
11.44Si
1.63And LaFe
11.37Al
1.63Magnetic free energy difference in the compound between ferrimagnetic state and the antiferromagnetic state is very little.In order to make material be in stable ferromagnetism phase, in the present invention, the content of Al is reduced to below 1.50 preferably about 1.3.If but the content of Al is reduced to 1.2 when following, form single 1:13 and will pass through long term annealing mutually, is unfavorable for suitability for industrialized production.In addition, its Curie temperature can descend, and is unfavorable for using as the magnetic refrigerating material more than the room temperature.
In addition, the feature of material of the present invention has secondary magnetic phase transition, M
2With μ
0The curve that H/M changes is linear near Curie temperature.Material does not have heat stagnation and magnetic hysteresis like this, and can stablize at the externally-applied magnetic field magnetic.
And the Curie temperature of material of the present invention is greater than 305K, less than 360K.This series material can use as composite material simultaneously with the Gd of Curie temperature at 295K like this, makes between refrigeration area in room temperature to more than the room temperature.Air conditioner refrigerating scope just.
Another feature of material of the present invention is that La can be by rare earth element Pr, and Nd replaces, and the replacement amount is from 3% to 20% of atomic ratio.Pr, the replacement of Nd can be finely tuned Curie temperature and magnetic entropy and be changed.
Other features of material of the present invention are values from 0.075 to 0.15 of y.Because La (Fe
xAl
1-x)
13The Curie temperature of compound is on the low side, improve its Curie temperature so add Co, but Co should not add, and Curie temperature is elevated to more than the air-conditioning work temperature.And the increase of the content of Co, also can reduce the maximum magnetic entropy variable value.
Other features of material of the present invention are that Al can be by Si, Ge, and Sn replaces, and the replacement amount is within atomic ratio 10%.Use Si, Ge, Sn replaces Al also can finely tune Curie temperature, can also finely tune the size of magnetic entropy.
Other features of material of the present invention are to be under the 2T in changes of magnetic field, and on the temperature variant curve of magnetic entropy, the product (relative refrigerating capacity RCP) of half corresponding temperature range Δ T of maximum magnetic entropy variable value and maximum magnetic entropy variable value is greater than 155, less than 300.And in changes of magnetic field is under the 2T, and the maximum magnetic entropy variable value is greater than 3J/Kg.K, less than 8J/Kg.K.。The present invention is to provide a kind of material, because the content of Al is lower, so just can obtain bigger magnetic entropy change and refrigerating capacity after the match low with big refrigerating capacity.
The method of The compounds of this invention is: La, Fe, Co, Al raw material are pressed La (Nd, Pr) (Fe
yCo
1-y)
13-xAl
xCarry out proportioning, put into smelting furnace, be evacuated to 4 * 10 before the melting
-3More than the Pa, feed argon gas then, evenly melting; The compound that obtains after the even melting was handled 120～360 hours 900～1100 ℃ of following homogenizing, put into frozen water then and cool off, to obtain single NaZn
13Phase.Best annealing time 240 hours.
Smelting furnace of the present invention is a vacuum arc furnace ignition, induction furnace or other smelting furnace.
The invention has the advantages that the working temperature of material is more than room temperature, and in the magnetic field range that permanent magnet can provide, refrigerating capacity and maximum magnetic entropy variable are big relatively, and preparation is simple, and Curie temperature is adjustable, do not have heat stagnation and magnetic hysteresis, can be widely used in the magnetic Refrigeration Technique.
Description of drawings
Fig. 1 is La (Fe of the present invention
0.919Co
0.081)
11.7Al
1.3X ray diffracting spectrum at room temperature.Wherein, abscissa is the angle of diffraction, and ordinate is an intensity.
Fig. 2 is La (Fe of the present invention
0.919Co
0.081)
11.7Al
1.3The M-T curve.Wherein, abscissa is a temperature, and ordinate is the magnetization.
Fig. 3 is La (Fe of the present invention
0.919Co
0.081)
11.7Al
1.3Magnetization curve, wherein, abscissa is magnetic field, ordinate is the magnetization.
Fig. 4 is La (Fe of the present invention
0.919Co
0.081)
11.7Al
1.3The curve of Arrott.Wherein, abscissa is μ
0H/M, ordinate are M
2
Fig. 5 is La (Fe of the present invention
0.919Co
0.81)
11.7Al
1.3Magnetic entropy becomes with the variation of temperature curve under 2T magnetic field.Wherein, abscissa is a temperature, and ordinate is that magnetic entropy becomes.
Fig. 6 is La of the present invention
0.8Nd
0.2(Fe
0.919Co
0.081)
11.7Al
1.3X ray diffracting spectrum at room temperature.Wherein, abscissa is the angle of diffraction, and ordinate is an intensity.
Fig. 7 is La of the present invention
0.8Nd
0.2(Fe
0.919Co
0.081)
11.7Al
1.3Magnetic entropy becomes with the variation of temperature curve under 2T magnetic field.Wherein, abscissa is a temperature, and ordinate is that magnetic entropy becomes.
Fig. 8 is La of the present invention
0.8Nd
0.2(Fe
0.919Co
0.081)
11.7Al
1.3RCP with the change curve of Δ H, wherein, abscissa is the change in magnetic field, ordinate is RCP.
Embodiment
Embodiment 1:
With La, Fe, Si, raw material such as Co are by chemical constituent La (Fe
0.919Co
0.081)
11.7Al
1.3Proportioning is put into vacuum arc furnace ignition, in induction furnace or other smelting furnace, is evacuated to 4 * 10
-3Pa or more than, feed argon gas, obtain the compound of uniform ingredients after the melt back cooling.The compound that melting obtains was handled 240 hours 1000 ℃ of following homogenizing, directly put into the frozen water fast quenching then.For preventing the sample oxidation, homogenizing is handled and annealing process can be carried out under vacuum or argon shield.Sample proves single NaZn through X-ray diffraction
13Phase is seen Fig. 1.Adopt SQUID to measure magnetization curve and vary with temperature, as Fig. 2,3.Through the compound that above-mentioned steps makes, Curie temperature is 315K, sees Fig. 2.And be second-order phase transistion, see Fig. 4.Result of calculation shows that under 2T magnetic field, magnetic entropy becomes 3.6J/kgK, sees Fig. 5.Refrigerating capacity RCP (Relative Cooling Power) value is by the maximum magnetic entropy variable absolute value relatively | Δ S|
MaxWarm area width δ T with magnetic entropy varied curve half-peak height place
FWHMMultiply each other and draw:
RCP＝|ΔS|
max×δT
FWHM
According to computing formula, La (Fe
0.919Co
0.081)
11.7Al
1.3RCP=168.6J/kg under Δ H=1.9T, result of calculation is listed in the table 1.In table 1, also listed some that from document, obtain and had the RCP that huge magnetic entropy becomes material at high temperature.Therefrom as can be known, though La (Fe
0.919Co
0.081)
11.7Al
1.3The magnetic entropy of material becomes and is not very big, but its RCP ability and MnFeP
0.45As
0.65, La (Fe
0.88Si
0.12)
13H
yAnd La (Fe
0.99Mn
0.01)
11.7Si
1.3H
yQuite.But La is (Fe
0.919Co
0.081)
11.7Al
1.3Material is owing to have second-order phase transistion, so material performance when using as refrigeration working medium is very stable, and preparation is simple relatively.It is a kind of magnetic cooling air conditioner material of great practical value.
The RCP value of the magnetic refrigerating material of several Curie temperature of table 1 more than room temperature is (Δ H=2T) relatively
| Material | Curie temperature (K) | |ΔS| max(J/(kg·K)) | RCP(J/kg) |
| Comparative example: La (Fe 0.88Si 0.12) 13H 1.5 | 323 | 19 | 146.6 |
| Comparative example: MnFeP 0.45As 0.65 | 332 | 11.8 | 146.9 |
| Comparative example: Gd | 295 | 4 | 169.4 |
| Comparative example: La (Fe 0.98Mn 0.02) 11.7Si 1.3H y (y≈2.0) | 315 | 12.9 | 132.3 |
| Comparative example: La (Fe 0.99Mn 0.01) 11.7Si 1.3H y (≈2.0) | 339 | 16 | 155.4 |
| Example of the present invention: La (Fe 0.919Co 0.081) 11.7Al 1.3 | 315 | 3.6 | 168.6 |
Embodiment 2:
With La, Nd, Fe, Si, raw material such as Co are by chemical constituent La
0.8Nd
0.2(Fe
0.919Co
0.081)
11.7Al
1.3Proportioning is put into vacuum arc furnace ignition, in induction furnace or other smelting furnace, is evacuated to 4 * 10
-3Pa or more than, feed argon gas, obtain the compound of uniform ingredients after the melt back cooling.The compound that melting obtains was handled 240 hours 1100 ℃ of following homogenizing, directly put into the frozen water fast quenching then.For preventing the sample oxidation, homogenizing is handled and annealing process can be carried out under vacuum or argon shield.Sample proves single NaZn through X-ray diffraction
13Phase is seen Fig. 6.Adopting SQUID to measure magnetization curve varies with temperature.Through the compound that above-mentioned steps makes, Curie temperature is 313K, and under 2T magnetic field, magnetic entropy becomes 4.5J/kg K, sees Fig. 7.The RCP of material sees Fig. 8 with Δ H variation relation curve.As Fig. 7, shown in 8, resulting La behind the adding Nd
0.8Nd
0.2(Fe
0.919Co
0.081)
11.7Al
1.3No matter be | Δ S|
MaxStill RCP has remarkable rising.The alternative La of adding Nd can improve magnetic refrigerating material | Δ S|
MaxAnd RCP.
Claims (10)
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|---|---|---|---|
| CNB2007100993777A CN100501882C (en) | 2007-05-18 | 2007-05-18 | A kind of high temperature low magnetic field large magnetic entropy material compound and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101105996A true CN101105996A (en) | 2008-01-16 |
| CN100501882C CN100501882C (en) | 2009-06-17 |
Family
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101368243B (en) * | 2008-09-24 | 2010-04-21 | 上海大学 | Preparation method of room temperature magnetic refrigeration material Y2Fe17 |
| CN101831278A (en) * | 2010-02-09 | 2010-09-15 | 江苏大学 | Preparation method of stratified compound magnetic cooling working medium |
| CN102017026B (en) * | 2008-03-31 | 2014-04-09 | 亨利庞加莱南锡第一大学 | Intermetallic compounds, their use and process for preparing same |
| WO2014115057A1 (en) * | 2013-01-24 | 2014-07-31 | Basf Se | Performance improvement of magnetocaloric cascades through optimized material arrangement |
| CN104559943A (en) * | 2013-10-09 | 2015-04-29 | 中国科学院宁波材料技术与工程研究所 | Crystalline-state magnetic refrigeration metal material and preparation method thereof |
| US9245673B2 (en) | 2013-01-24 | 2016-01-26 | Basf Se | Performance improvement of magnetocaloric cascades through optimized material arrangement |
| CN105834407A (en) * | 2015-01-15 | 2016-08-10 | 中国科学院宁波材料技术与工程研究所 | Preparation method of rare earth iron-based alloy compound with NaZn13 type structure |
| CN112368790A (en) * | 2018-02-22 | 2021-02-12 | 通用工程与研究有限责任公司 | Magnetocaloric alloys for magnetic refrigeration applications |
-
2007
- 2007-05-18 CN CNB2007100993777A patent/CN100501882C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102017026B (en) * | 2008-03-31 | 2014-04-09 | 亨利庞加莱南锡第一大学 | Intermetallic compounds, their use and process for preparing same |
| CN101368243B (en) * | 2008-09-24 | 2010-04-21 | 上海大学 | Preparation method of room temperature magnetic refrigeration material Y2Fe17 |
| CN101831278A (en) * | 2010-02-09 | 2010-09-15 | 江苏大学 | Preparation method of stratified compound magnetic cooling working medium |
| WO2014115057A1 (en) * | 2013-01-24 | 2014-07-31 | Basf Se | Performance improvement of magnetocaloric cascades through optimized material arrangement |
| US9245673B2 (en) | 2013-01-24 | 2016-01-26 | Basf Se | Performance improvement of magnetocaloric cascades through optimized material arrangement |
| US9915447B2 (en) | 2013-01-24 | 2018-03-13 | Basf Se | Performance improvement of magnetocaloric cascades through optimized material arrangement |
| CN104559943A (en) * | 2013-10-09 | 2015-04-29 | 中国科学院宁波材料技术与工程研究所 | Crystalline-state magnetic refrigeration metal material and preparation method thereof |
| CN105834407A (en) * | 2015-01-15 | 2016-08-10 | 中国科学院宁波材料技术与工程研究所 | Preparation method of rare earth iron-based alloy compound with NaZn13 type structure |
| CN105834407B (en) * | 2015-01-15 | 2018-07-27 | 中国科学院宁波材料技术与工程研究所 | With NaZn13The preparation method of the rare-earth iron-based alloy cpd of type structure |
| CN112368790A (en) * | 2018-02-22 | 2021-02-12 | 通用工程与研究有限责任公司 | Magnetocaloric alloys for magnetic refrigeration applications |
| CN112368790B (en) * | 2018-02-22 | 2024-04-26 | 通用工程与研究有限责任公司 | Magnetocaloric alloys for magnetic refrigeration applications |
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|---|---|
| CN100501882C (en) | 2009-06-17 |
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