CN105314598A - A high-pressure synthesis method for flaky La (Fe, si)13-based hydride bulk material with high-efficiency room-temperature magnetic refrigeration performance - Google Patents
A high-pressure synthesis method for flaky La (Fe, si)13-based hydride bulk material with high-efficiency room-temperature magnetic refrigeration performance Download PDFInfo
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- CN105314598A CN105314598A CN201510819969.6A CN201510819969A CN105314598A CN 105314598 A CN105314598 A CN 105314598A CN 201510819969 A CN201510819969 A CN 201510819969A CN 105314598 A CN105314598 A CN 105314598A
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Abstract
The invention belongs to the field of new function materials and provides a high atmospheric pressure synthetic method for a flaky La(Fe, Si)13-based hydride block with efficient room temperature magnetic refrigeration performance. According to the method, a La(Fe, Si)13-based compound with a NaZn13 structure is smashed before being placed in a high atmospheric pressure heat treatment device, and subjected to hydrogen absorption in a hydrogen atmosphere before being cooled to the room temperature, and then a saturated hydrogen absorption hydride is obtained; the saturated hydrogen absorption hydride is pressed into a flake, sintered and cooled naturally, and then the flaky hydride block is obtained. By the adoption of the method, the problem of hard molding to the La(Fe, Si)13-based hydride in practical application is solved, and a flaky La(Fe, Si)13-based magnetic refrigeration working medium with efficient room temperature magnetic refrigeration performance and capable of being used at a driving magnetic cold-accumulation refrigerator can be obtained.
Description
Technical field
The invention belongs to New function Material Field, be specifically related to a kind of sheet La (Fe, Si) with efficient room temperature magnetic refrigeration performance
13the high atmospheric pressure synthetic method of base hydride block.
Background technology
Low temperature and Refrigeration Technique play more and more important effect at society, and traditional gas refrigeration technology exists a lot of shortcomings such as refrigerating efficiency is low, influence of noise is large.Further, the compression working medium freonll-11 that gas refrigeration uses can havoc atmospheric environment.Comprehensive stopping along with the hydro carbons halides containing freonll-11 is produced and is used, and the advantages such as the magnetic Refrigeration Technique that the magnetothermal effect based on material grows up is high with its refrigerating efficiency, noise is little, environmentally safe are subject to extensive attention both domestic and external.Magnetothermal effect refers to the Process of absorption or liberation of heat phenomenon of magneticsubstance under additional the action of a magnetic field.At present, low temperature magnetic refrigeration (lower than 20K) technology comparative maturity.Be used widely in the sophisticated technology such as scientific research, spationautics field.Owing to having huge applications prospect in domestic refrigeration and industrial refrigeration system etc., the high-temp magnetic particularly room temperature magnetic refrigerating that freezes is subject to the great attention of countries in the world.Therefore, finding Curie temperature in room-temperature zone has the refrigerating material that large magnetic entropy becomes and becomes research emphasis both domestic and external.
In existing magnetic refrigerating material, there is a cube NaZn
13the La (Fe, Si) of structure
13based compound is excellent with magnetic heating performance, and the prices of raw and semifnished materials are cheap, and the advantage such as have no side effect, and becomes a kind of refrigeration working medium having market outlook and practical value.Studies have found that, the itinerant-electron metamagnetic of Magnetic Field-Induced has great effect to magnetothermal effect and magnetic hysteresis loss, and closely related with the change of transformation temperature.Therefore, at La (Fe, Si)
13in based compound, by suitable element substitution with introduce gap hydrogen atom, can obtain large magnetic entropy become and adjustable Curie temperature to room temperature, be a kind of effective ways obtaining desirable room temperature magnetic refrigerating working.
At near room temperature, active magnetic cold-storage (AMR) is magnetic refrigeration modes desirable at present.In practical application, the cold based on AMR technology requires that refrigeration working medium has large heat exchange area and improves thermo-efficiency, and therefore magnetic refrigeration working substance is often configured to porous block or sheet.But, directly to block La (Fe, Si)
13based compound hydrogenation can generate a large amount of crackle, causes sample to use.CN103468226A patent discloses the silica-based room temperature magnetic refrigerating matrix material of a kind of lanthanum iron and preparation method, the method by lanthanum iron silicon base compound is mixed with macromolecular material and auxiliary agent, then elevated cure aftershaping of colding pressing, but owing to adding non-magnetic binding agent and macromolecular material, the magnetic entropy that can reduce unit volume becomes.
La (Fe, Si)
13the Curie temperature of base hydride is very responsive for hydrogen atom content.Curie temperature is inhaled in the compound of hydrogen in the part of near room temperature, and ferromagnetic large volume phase coexists mutually with the small volume of paramagnetic.Can there is in room temperature hydrogen atom to be diffused into large volume phase mutually phenomenon from small volume, make whole compound occur two Curie temperature, thus the serious value reducing magnetic entropy and become.There are some researches show, high pressure nitrogen atmosphere is highly profitable to the high-quality nitride of synthesis.Therefore, under high pressure hydrogen atmosphere, synthesize the La (Fe, Si) of saturated suction hydrogen
13base hydride can address this problem.
Summary of the invention
The object of this invention is to provide a kind of sheet La (Fe, Si) with efficient room temperature magnetic refrigeration performance
13the high atmospheric pressure synthetic method of base hydride block, can obtain the sheet La (Fe, Si) with efficient room temperature magnetic refrigeration performance that can use in AMR cold by the method
13base hydride magnetic refrigeration working substance.
The technical solution used in the present invention is:
A kind of sheet La (Fe, Si) with efficient room temperature magnetic refrigeration performance
13the high atmospheric pressure synthetic method of base hydride block, comprises the following steps:
Step 1: will NaZn be had
13the La (Fe, Si) of structure
13based compound shatters and reaches 1-2mm to particle diameter and be placed in high atmospheric pressure thermal treatment unit, 300-500 DEG C, inhale hydrogen 3-5 hour in the hydrogen atmosphere that is more than or equal to 50MPa after be cooled to room temperature, obtain the hydride of saturated suction hydrogen;
Step 2: after the hydride of the saturated suction hydrogen in step 1 is slightly ground, diameter 10-20mm is compressed under 6-8MPa pressure, the thin slice of thickness 0.6-3mm, afterwards thin slice is placed in high atmospheric pressure thermal treatment unit, 500-650 DEG C, sinter 24-48 hour in the high pressure hydrogen atmosphere that is more than or equal to 50MPa after, naturally cool to room temperature, obtain sheet hydride block.
The room temperature process that is cooled in described step 1, step 2 remains on and is more than or equal in the high pressure hydrogen atmosphere of 50MPa;
The saturated suction hydrogen of sheet hydride block of described synthesis, hydrogen atom is present in La (Fe, Si)
13in gap.
α-Fe the content of the sheet hydride block of described synthesis and La (Fe, Si)
13based compound is compared without increasing.
In the sheet hydride block of described synthesis, be distributed with the micropore of a large amount of different size, the equivalent diameter of micropore is between 1-98 μm.
The magnetic entropy of sheet hydride block under 0-2T variation magnetic field of described synthesis becomes 7.5-20J/kgK, and transition temperature area is positioned at 280K-360K.
The magnetic hysteresis of sheet hydride block under 0-2T variation magnetic field of described synthesis is less than 2J/kg.
The present invention's beneficial effect is compared with prior art: provide a kind of La (Fe, Si) with efficient room temperature magnetic refrigeration performance
13the high atmospheric pressure synthetic method of base hydride block.The method can obtain the sheet La (Fe, Si) with efficient room temperature magnetic refrigeration performance that can use in AMR cold
13base hydride magnetic refrigeration working substance, solves La (Fe, Si) in practical application
13the problem that base hydride is difficult shaping.In room temperature range, under the variation magnetic field of 0-2T, magnetic entropy change reaches the change of 15J/kgK(volume magnetic entropy and reaches 106mJ/cm
3k).Meanwhile, the magnetic hysteresis of sheet hydride block is less than 2J/kg, can reach the requirement of actual room temperature magnetic refrigeration application.
Accompanying drawing explanation
Fig. 1 is sheet La
0.5pr
0.5fe
11.4si
1.6(a) and La
0.9ce
0.1fe
11.35mn
0.35si
1.3the XRD figure spectrum of (b) and hydride thereof.
Fig. 2 is sheet La
0.5pr
0.5fe
11.4si
1.6and La
0.9ce
0.1fe
11.35mn
0.35si
1.3the specific magnetising moment variation with temperature curve of hydride block, illustration is the photo in kind of sheet sample.
Fig. 3 is sheet La
0.5pr
0.5fe
11.4si
1.6(a) and La
0.9ce
0.1fe
11.35mn
0.35si
1.3the scanning electron microscopic picture of (b) hydride block.
Fig. 4 is sheet La
0.5pr
0.5fe
11.4si
1.6(a) and La
0.9ce
0.1fe
11.35mn
0.35si
1.3b () hydride block specific magnetising moment is at different temperatures with the change curve of foreign field.
Fig. 5 (a) is sheet La
0.5pr
0.5fe
11.4si
1.6the magnetic entropy of hydride block becomes variation with temperature curve, and illustration is that its volume magnetic entropy becomes variation with temperature curve; Fig. 5 (b) is sheet La
0.9ce
0.1fe
11.35mn
0.35si
1.3the magnetic entropy of hydride block becomes variation with temperature curve, and illustration is its adiabatic temperature varied curve.
Fig. 6 (a)-(c) is sheet La
0.5pr
0.5fe
11.4si
1.6the two dimensional image of the x-ray tomography of hydride block; Fig. 6 (d)-(f) is sheet La
0.9ce
0.1fe
11.35mn
0.35si
1.3the two dimensional image of the x-ray tomography of hydride block.
Fig. 7 is that tomoscan image rebuilds the sheet La obtained
0.5pr
0.5fe
11.4si
1.6(a) and La
0.9ce
0.1fe
11.35mn
0.35si
1.3the 3-D view of (b) hydride block.
Embodiment
Embodiment of the present invention are illustrated below in conjunction with accompanying drawing.
Embodiment one:
A cube NaZn will be had
13the La of structure
0.5pr
0.5fe
11.4si
1.6after the particle for diameter 1-2mm pulverized by mother alloy, being placed in autoclaving device inhales hydrogen 5 hours, inhales hydrogen temperature 500 DEG C, hydrogen pressure 50MPa.Hydrogen pressure 50MPa is kept to be cooled to the hydride particle that room temperature obtains saturated suction hydrogen.Get hydride particle and be ground to the powder that footpath particle size is less than 50 μm, under the pressure of 6MPa, be then pressed into diameter is 10mm, and thickness is the sheet block of 0.8mm.The sheet sample be pressed into is placed in high atmospheric pressure thermal treatment unit and carries out sintering processes, sintering time is 24 hours, and sintering temperature is 600 DEG C, and hydrogen pressure is 50MPa.Be cooled to room temperature in a hydrogen atmosphere after terminating, process of cooling keeps hydrogen pressure 50MPa, obtains sheet hydride block.
Embodiment two:
A cube NaZn will be had
13the La of structure
0.9ce
0.1fe
11.35mn
0.35si
1.3mother alloy inhales hydrogen 5 hours after pulverizing the particle for diameter 1-2mm in high atmospheric pressure thermal treatment unit, inhale hydrogen temperature 500 DEG C, hydrogen pressure 50MPa.Hydrogen pressure 50MPa is kept to be cooled to the hydride particle that room temperature obtains saturated suction hydrogen.Get hydride particle and be ground to the powder that footpath particle size is less than 50 μm, under the pressure of 6MPa, be then pressed into diameter is 10mm, and thickness is the sheet block of 0.8mm.The sheet sample be pressed into is placed in high atmospheric pressure thermal treatment unit and carries out sintering processes, sintering time is 48 hours, and sintering temperature is 500 DEG C, and hydrogen pressure is 50MPa.Be cooled to room temperature in a hydrogen atmosphere after terminating, process of cooling keeps hydrogen pressure 50MPa, obtains sheet hydride block.
Carry out test analysis to the sheet hydride block obtained by embodiment one and embodiment two, Fig. 1 shows that hydrogen atom is present in La (Fe, Si) with the form of interstitial atom
13lattice between, simultaneously α-Fe content is without increase.From Fig. 2 to find out, La
0.5pr
0.5fe
11.4si
1.6the Curie temperature of hydride is 329K, La
0.9ce
0.1fe
11.35mn
0.35si
1.3the Curie temperature of hydride is 290K, near room temperature between this refrigeration area showing the sheet hydride block prepared.Sample shown in Fig. 2 illustration is disc-like wafer, and diameter is 10mm, and thickness is 0.8mm.Fig. 3 scanning electron microscopic picture shows, the complete flawless of sheet hydride block surface, grain size is less than 50 μm.Fig. 4 is sheet La
0.5pr
0.5fe
11.4si
1.6(a) and La
0.9ce
0.1fe
11.35mn
0.35si
1.3b the isothermal magnetization curve of () hydride block, through calculating, under the variation magnetic field of 2T, magnetic hysteresis loss is less than 2J/kg.Fig. 5 (a) shows, in room temperature range, and sheet La
0.5pr
0.5fe
11.4si
1.6hydride block has and to become more than the magnetic entropy of 15J/KgK that (volume magnetic entropy becomes 106mJ/cm under the 0-2T variation magnetic field that tool has significant practical applications
3k), refrigeration performance is very excellent.As can be seen from Fig. 5 (b), after with the addition of Ce, Mn element, sheet La
0.9ce
0.1fe
11.35mn
0.35si
1.3the Curie temperature of hydride block can be reduced to room temperature range, shows that this sheet block can be used as room temperature magnetic refrigerating working.Fig. 6 and Fig. 7 is respectively sheet La
0.5pr
0.5fe
11.4si
1.6and La
0.9ce
0.1fe
11.35mn
0.35si
1.3the two and three dimensions image of the x-ray tomography of hydride block, can find out that sheet block hydride inside is dispersed with a large amount of equivalent diameter between the micropore of 1-98 μm, just because of the existence of these different size micropores, the magnetic hysteresis of sheet hydride block is reduced to lower than 2J/kg.
Embodiment three:
A cube NaZn will be had
13the La of structure
0.5pr
0.5fe
11.4si
1.6after the particle for diameter 1-2mm pulverized by mother alloy, being placed in autoclaving device inhales hydrogen 3 hours, inhales hydrogen temperature 400 DEG C, hydrogen pressure 60MPa.Hydrogen pressure 60MPa is kept to be cooled to the hydride particle that room temperature obtains saturated suction hydrogen.Get hydride particle and be ground to the powder that footpath particle size is less than 50 μm, under the pressure of 8MPa, be then pressed into diameter is 20mm, and thickness is the sheet block of 0.6mm.The sheet sample be pressed into is placed in high atmospheric pressure thermal treatment unit and carries out sintering processes, sintering time is 24 hours, sintering temperature for being respectively 650 DEG C, hydrogen atmosphere pressure 60MPa.Be cooled to room temperature in a hydrogen atmosphere after terminating, process of cooling keeps hydrogen pressure 60MPa, obtains sheet hydride block.
Embodiment four:
A cube NaZn will be had
13the La of structure
0.5pr
0.5fe
11.4si
1.6after the particle for diameter 1-2mm pulverized by mother alloy, being placed in autoclaving device inhales hydrogen 4 hours, inhales hydrogen temperature 300 DEG C, hydrogen pressure 70MPa.Hydrogen pressure 70MPa is kept to be cooled to the hydride particle that room temperature obtains saturated suction hydrogen.Get hydride particle and be ground to the powder that footpath particle size is less than 50 μm, under the pressure of 7MPa, be then pressed into diameter is 15mm, and thickness is the sheet block of 3mm.The sheet sample be pressed into is placed in high atmospheric pressure thermal treatment unit and carries out sintering processes, sintering time is 36 hours, sintering temperature for being respectively 500 DEG C, hydrogen atmosphere pressure 70MPa.Be cooled to room temperature in a hydrogen atmosphere after terminating, process of cooling keeps hydrogen pressure 70MPa, obtains sheet hydride block.
Claims (6)
1. one kind has the sheet La (Fe, Si) of efficient room temperature magnetic refrigeration performance
13the high atmospheric pressure synthetic method of base hydride block, is characterized in that, comprise the following steps:
Step 1: will NaZn be had
13the La (Fe, Si) of structure
13based compound shatters and reaches 1-2mm to particle diameter and be placed in high atmospheric pressure thermal treatment unit, 300-500 DEG C, inhale hydrogen 3-5 hour in the hydrogen atmosphere that is more than or equal to 50MPa after be cooled to room temperature, obtain the hydride of saturated suction hydrogen;
Step 2: after the hydride of the saturated suction hydrogen in step 1 is slightly ground, diameter 10-20mm is compressed under 6-8MPa pressure, the thin slice of thickness 0.6-3mm, afterwards thin slice is placed in high atmospheric pressure thermal treatment unit, 500-650 DEG C, sinter 24-48 hour in the high pressure hydrogen atmosphere that is more than or equal to 50MPa after, naturally cool to room temperature, obtain sheet hydride block.
2. the sheet La (Fe, Si) with efficient room temperature magnetic refrigeration performance according to claim 1
13the high atmospheric pressure synthetic method of base hydride block, is characterized in that:
The room temperature process that is cooled in described step 1, step 2 remains on and is more than or equal in the high pressure hydrogen atmosphere of 50MPa.
3. the sheet La (Fe, Si) with efficient room temperature magnetic refrigeration performance according to claim 1
13the high atmospheric pressure synthetic method of base hydride block, is characterized in that, the saturated suction hydrogen of sheet hydride block of described synthesis, hydrogen atom is present in La (Fe, Si)
13in gap.
4. the sheet La (Fe, Si) with efficient room temperature magnetic refrigeration performance according to claim 1
13the high atmospheric pressure synthetic method of base hydride block, is characterized in that, in the sheet hydride block of described synthesis, be distributed with the micropore of a large amount of different size, the equivalent diameter of micropore is between 1-98 μm.
5. the sheet La (Fe, Si) with efficient room temperature magnetic refrigeration performance according to claim 1
13the high atmospheric pressure synthetic method of base hydride block, is characterized in that, the magnetic entropy of sheet hydride block under 0-2T variation magnetic field of described synthesis becomes 7.5-20J/kgK, and transition temperature area is positioned at 280K-360K.
6. the sheet La (Fe, Si) with efficient room temperature magnetic refrigeration performance according to claim 1
13the sheet hydride block synthesized described in base hydride, is characterized in that, the magnetic hysteresis of sheet hydride block under 0-2T variation magnetic field of described synthesis is less than 2J/kg.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106270425A (en) * | 2016-08-10 | 2017-01-04 | 横店集团东磁股份有限公司 | A kind of magnetic refrigerating material mass production preparation method |
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| JP2003096547A (en) * | 2001-09-21 | 2003-04-03 | Toshiba Corp | Magnetic refrigeration material and producing method thereof |
| CN101554993A (en) * | 2009-05-19 | 2009-10-14 | 北京科技大学 | Method for preparing large magnetic entropy material hydride with main phase of NaZn13 type structure |
| CN101817078A (en) * | 2010-01-06 | 2010-09-01 | 北京科技大学 | Method for even hydrogenation of NaZn13 structured rare earth-iron cobalt silicon material |
| CN102087899A (en) * | 2009-12-02 | 2011-06-08 | 中国科学院物理研究所 | La (Fe, al)13-based hydride magnetic refrigerating material and its preparation method and application |
| US20130200293A1 (en) * | 2009-12-11 | 2013-08-08 | Hubei Quanyang Magnetic Materials Manufacturing Co., Ltd. | La(fe,si)13-based multi-interstitial atom hydride magnetic refrigeration material with high temperature stability and large magnetic entropy change and preparation method thereof |
-
2015
- 2015-11-24 CN CN201510819969.6A patent/CN105314598B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003096547A (en) * | 2001-09-21 | 2003-04-03 | Toshiba Corp | Magnetic refrigeration material and producing method thereof |
| CN101554993A (en) * | 2009-05-19 | 2009-10-14 | 北京科技大学 | Method for preparing large magnetic entropy material hydride with main phase of NaZn13 type structure |
| CN102087899A (en) * | 2009-12-02 | 2011-06-08 | 中国科学院物理研究所 | La (Fe, al)13-based hydride magnetic refrigerating material and its preparation method and application |
| US20130200293A1 (en) * | 2009-12-11 | 2013-08-08 | Hubei Quanyang Magnetic Materials Manufacturing Co., Ltd. | La(fe,si)13-based multi-interstitial atom hydride magnetic refrigeration material with high temperature stability and large magnetic entropy change and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106270425A (en) * | 2016-08-10 | 2017-01-04 | 横店集团东磁股份有限公司 | A kind of magnetic refrigerating material mass production preparation method |
| CN106270425B (en) * | 2016-08-10 | 2018-06-05 | 横店集团东磁股份有限公司 | A kind of magnetic refrigerating material mass production preparation method |
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