CN107142419A - A kind of preparation method of LaFeSiH materials - Google Patents
A kind of preparation method of LaFeSiH materials Download PDFInfo
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- CN107142419A CN107142419A CN201710255250.3A CN201710255250A CN107142419A CN 107142419 A CN107142419 A CN 107142419A CN 201710255250 A CN201710255250 A CN 201710255250A CN 107142419 A CN107142419 A CN 107142419A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/012—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials adapted for magnetic entropy change by magnetocaloric effect, e.g. used as magnetic refrigerating material
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- Power Engineering (AREA)
- Hard Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of preparation method of LaFeSiH materials.It specifically includes following steps：(1) La is chosen1‑xRx(Fe13‑y‑bMy)SibHcAlloy is flushed with hydrogen powder；(2) bonding agent being mixed to get in proportion using epoxy resin and curing agent；(3) with bonding agent and alloy be flushed with hydrogen powder and be put into container, and pour into acetone as solvent, be stirred, being flushed with hydrogen powder after bonding agent and alloy is well mixed and after acetone volatilizees, is granulated, re-compacted shaping；(4) sample after being molded solidifies at low temperature, and wherein low temperature is not higher than 80 DEG C.The beneficial effects of the invention are as follows：While the intensity and performance of alloy is ensured, moreover it is possible to ensure alloy not dehydrogenation, the performance of magnetic refrigerating material is not influenceed, and adiabatic temperature becomes, Curie temperature and magnetic entropy become and can be guaranteed.
Description
Technical field
The present invention relates to magnetic refrigerating material correlative technology field, a kind of preparation method of LaFeSiH materials is referred in particular to.
Background technology
Room temperature magnetic refrigerating technology has environmental protection, it is energy-efficient, reliable and stable the characteristics of, generation has been caused in the last few years
The extensive concern of boundary's scope.Society always consumes energy more than 15% is accounted for because refrigeration industry consumes energy, and is used in vapor compression refrigeration
Gas refrigerant can destroy atmospheric ozone layer and cause greenhouse effects, so the advantage that room-temperature magnetic refrigerator possesses so that this
Technology is expected to replace traditional vapor compression refrigeration.Several type high temps or even room temperature that the U.S., China, Holland, Japan find in succession
Area's materials with the giant magnetocaloric effect has promoted expectation of the people to environmental protection magnetic Refrigeration Technique significantly, for example：Gd-Si-Ge、LaCaMnO3、
The compound such as the based compound of Ni-Mn-Ga, La (Fe, Si) 13, Mn-Fe-P-As, MnAs.These new giant magnetio-caloric effects materials
Common feature is that magnetic entropy change is above traditional room temperature magnetic refrigerating material Gd, and phase transition property is one-level, and majority is presented strongly
Magnetocrystalline coupling characteristics, magnetic phase transition with significant crystal structure phase transformation generation.These new materials also show different materials
Expect characteristic, for example, Gd-Si-Ge is expensive, needed in preparation process to the further purification of raw material, Mn-Fe-P-As, MnAs
It is poisonous etc. Deng compound starting material.
The research of room-temperature magnetic refrigerator and application are also constantly improving, the U.S., China, France, Britain, Italy,
Denmark, Canada, Japan, Spain etc. have developed various room-temperature magnetic refrigerators in succession.Room-temperature magnetic refrigerator uses electromagnetism at first
Iron or superconductor make magnetic field, but superconduction and electromagnet are expensive, and maintenance cost is high, is restricted for commercialization.At present,
The magnetic field of room-temperature magnetic refrigerator is provided by permanent magnet, while realizing high-power, high-frequency.
With the development of room-temperature magnetic refrigerator, it is believed that in magnetic refrigerating material, most application prospect is LaFeSi systems
Alloy.It is frangible and the first order phase change magnetic refrigerating material that LaFeSi systems alloy is obtained after being flushed with hydrogen can become very crisp.So magnetothermal effect
The shaping of material also turns into the problem of needing urgent solve.Magnetic refrigerating material in the regenerator of magnetic refrigerator needs to be processed into
Type, is made required shape, this needs is bonded together powdered LaFeSi materials with adhesive, and retentivity as far as possible
Can, re-compacted shaping makes moulded products keep high intensity by techniques such as solidifications.And conventionally used bonding agent needs to solidify temperature
80-180 DEG C of degree, heats 0.5h-2h in this temperature range, can lose substantial amounts of hydrogen atom, cause the LaFeSi systems of first order phase change
Alloy property is reduced, and influences the performance of magnetic refrigerating material, and adiabatic temperature change, Curie temperature and magnetic entropy become and can all declined.
The content of the invention
The present invention is above-mentioned to ensure alloy not dehydrogenation and property there is provided one kind to overcome the shortcomings of to exist in the prior art
The preparation method of constant LaFeSiH materials can be kept.
To achieve these goals, the present invention uses following technical scheme：
A kind of preparation method of LaFeSiH materials, specifically includes following steps：
(1) La is chosen1-xRx(Fe13-y-bMy)SibHcAlloy is flushed with hydrogen powder；
(2) bonding agent being mixed to get in proportion using epoxy resin and curing agent；
(3) bonding agent matched somebody with somebody is flushed with hydrogen powder with alloy and is put into container, and pours into acetone as solvent, is stirred,
After bonding agent and alloy be flushed with hydrogen powder be well mixed and after acetone volatilization after, granulated, re-compacted shaping；
(4) sample after being molded solidifies at low temperature, and wherein low temperature is not higher than 80 DEG C.
It can make to lose substantial amounts of hydrogen in alloy using hot setting in the curing process, so the present invention is by using epoxy instead
The solidification bonding agent that resin and curing agent proportioning are obtained, its solidification temperature is not more than 80 DEG C, and the intensity and performance of such alloy can
To be guaranteed simultaneously, alloy not dehydrogenation is also ensured in addition.
Preferably, in step (1), R is one or several kinds of compositions of following rare earth elements, the rare earth member
Element is：Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Sc、Y；X scope is：0≤x≤0.3；M be Mn,
One kind in Ti, V, Cr, Co, Ni, Cu, Zn, Ga；Y scope is：0.003≤y≤0.5；B scope is：1.0≤b≤1.5；
C scope is：0≤c≤3.0.
Preferably, in step (1), La1-xRx(Fe13-y-bMy)SibHcThe powder diameter control that alloy is flushed with hydrogen powder exists
Less than 300 μm.If powder diameter is too big, mobility is too poor in pressing process, is molded for the more box-shaped pressed compact of seamed edge
It is difficult.
Preferably, in step (2), the ratio of epoxy resin and curing agent is 1~2: 1.
Preferably, in step (2), bonding agent accounts for alloy and is flushed with hydrogen the mass fraction of powder for 1.5%-3%.If viscous
The mass fraction for connecing agent is too high, then alloy powder viscosity is too big, is unfavorable for granulation.
The beneficial effects of the invention are as follows：While the intensity and performance of alloy is ensured, moreover it is possible to ensure alloy not dehydrogenation, no
The performance of magnetic refrigerating material is influenceed, adiabatic temperature becomes, Curie temperature and magnetic entropy become and can be guaranteed.
Brief description of the drawings
Fig. 1 is La0.7Ce0.3Fe11.30Mn0.20Si1.5HxIt is flushed with hydrogen the Entropy Changes and temperature relation figure of powder；
Fig. 2 is La0.7Ce0.3Fe11.30Mn0.20Si1.5HxAlloy is using the Entropy Changes after the solidification of room temperature curing agent bonding sheet and temperature
Spend graph of a relation；
Fig. 3 is La0.7Ce0.3Fe11.30Mn0.20Si1.5HxAlloy is using the Entropy Changes after the solidification of high-temperature curing agent bonding sheet and temperature
Spend graph of a relation；
Fig. 4 is La0.7Ce0.3Fe11.4Mn0.28i1.4HxWith La0.7Ce0.3Fe11.45Mn0.15Si1.4HxTwo kinds of curie points are flushed with hydrogen
Alloy powder and the thermal insulation temperature of each self-corresponding compressing become graph of a relation.
Wherein：Fig. 1, Fig. 2 and Fig. 3 abscissa all represent temperature, and using Kelvin, unit is used as using K；Ordinate
Represent Entropy Changes value Δ S, unit Jkg-1K-1.The corresponding abscissa of the peak value of curve represents Curie temperature in figure.Same figure
In three curves be respectively the corresponding different temperatures under three kinds of magnetic flux densities (0.5T, 0.8T, 1T) Entropy Changes value.In Fig. 4
Powder 1 (closed square, solid line) represents La respectively with piece 1 (hollow square, dotted line)0.7Ce0.3Fe11.4Mn0.2Si1.4HxMaterial is consolidated
Powder and solidification aftershaping piece before changing, powder 2 (filled circles, solid line) are represented respectively with piece 2 (open circles, dotted line)
La0.7Ce0.3Fei1.45Mn0.15Si1.4HxPowder and solidification aftershaping piece before material solidification；Abscissa represents temperature and uses Kelvin temperature
Degree, using K as unit, ordinate represents adiabatic temperature change Δ T, unit K or DEG C.
Embodiment
The present invention will be further described with reference to the accompanying drawings and detailed description.
LaFeSiH alloy powders to keep its excellent performance, then need when the regenerator of magnetic refrigerator is made
Ensure alloy not dehydrogenation, so 80 DEG C of bonding agent should be not higher than using solidification temperature.So, the intensity and performance of alloy can
To ensure simultaneously.Choose La1-xCex(Fe13-y-bMny)SibHcAlloy is flushed with hydrogen powder 50g and makees molded test, wherein：X scope
It is：0≤x≤0.5, y scope is：0.003≤y≤0.5, b scope is：1.0≤b≤1.5, c scope is：0≤c≤
3.0.Alloy is flushed with hydrogen the control of the powder diameter of powder below 300 μm, if powder diameter is too big, in pressing process, mobility is too
Difference, for the more box-shaped pressed compact difficult forming of seamed edge.Here the alloy chosen is flushed with hydrogen powder
La0.7Ce0.3Fe11.30Mn0.20Si1.5Hx。
Using E44 epoxy resin and the polyamide of curing agent 650 1: 1 bonding agent being mixed to get in proportion, quality point
Number is 2.5%.With bonding agent and alloy powder be put into container, and pour into acetone as solvent, be stirred, wait to be bonded
Agent is well mixed with alloy powder and after after acetone volatilization, granulated, re-compacted shaping, the sample after shaping is at 40 DEG C or so
Solidification, Entropy Changes is held essentially constant, and data are shown in Table 1, and the Entropy Changes value under 0.8T magnetic field intensities is 8.85Jkg-1K-1, is occupied
In temperature be 287K.Curve is as depicted in figs. 1 and 2.
Rear powder 50g is flushed with hydrogen with identical LaFeSiH series alloy powders, using E51 epoxy resin and dicy-curing agent
The bonding agent of mixing, both ratios are according to 5: 1, and the mass fraction of bonding agent is 2.5%.Bonding agent is put into container with alloy powder
In, and acetone is poured into as solvent, it is stirred, is well mixed and after acetone volatilization, is made with alloy powder after bonding agent
Grain, re-compacted shaping, the sample after shaping solidifies at 160 DEG C, and the hydrogen content in sample is decreased obviously, in 0.8T magnetic field intensities
8.93Jkg-1K-1 of the lower Entropy Changes value before solidifying is reduced to 4.93Jkg-1K-1 after solidification.As shown in Figure 3.
Choose La0.7Ce0.3Fe11.30Mn0.20Si1.5HxPowder is flushed with hydrogen, is mixed with E51 epoxy resin with dicy-curing agent
Bonding agent, both ratios are according to 5: 1, and the mass fraction of bonding agent is 2.5%.Bonding agent and alloy powder are all put into container
In, and acetone is poured into as solvent, it is stirred, treats that bonding agent is well mixed acetone volatilization with alloy powder, granulated, made
Alloy powder after grain, tests hydrogen content, and hydrogen mass fraction is 0.3857%；LaFeSiH systems alloy after shaping is made at solidification
Reason, treats that sample is fully cured, and the mass fraction for measuring hydrogen content is 0.3392%.It can be seen that metal dust matrix band is solid
Hydrogen content change before and after changing, the hydrogen content after solidification in alloy declines, and hot setting causes dehydrogenation in alloy, the performance of alloy
It can decline therewith.
In order to obtain optimal solidification effect, do tests below not influenceing metal to be flushed with hydrogen under the premise of the performance of powder.
The proportioning of E44 epoxy resin and 650 polyamide curing agent is respectively adopted 1: 1,1.5: 1,2: 1；The mass fraction of bonding agent
It is 2.5%, 3%, solidification temperature uses 160 DEG C, 80 DEG C and 40 DEG C；10 minutes, 1 hour, 2 hours hardening time.It is measured
Obtain the hydrogen content change of alloy powder, such as table 2.The proportioning of E44 epoxy resin and 650 polyamide curing agent be 1: 1,
When 1.5: 1,2: 1, in the case of the mass fraction 2.5% of bonding agent, in bonding agent hydrogen content be respectively 0.194%,
0.158%th, 0.141%；In the case of the mass fraction 3% of bonding agent, in bonding agent hydrogen content be respectively 0.244%,
0.197%th, 0.175%.Through measuring the hydrogen content about 0.21% or so of such a alloy in itself.Hydrogen content includes three aspects,
Protium in the protium of alloy in itself, bonding agent, the hydrogen content for also having remaining acetone.The protium of alloy powder after granulation
Including this three, after being fully cured, it is believed that acetone volatilizees completely, the above two are only existed.If solidification temperature is too high, close
The golden hydrogen of itself can overflow on a small quantity.And have two kinds the reason for reduced with the growth hydrogen content of hardening time, in the case of a high temperature
Final hydrogen content, which is reduced, includes in two parts, a small amount of alloy hydrogen and acetone from being not completely evaporated into complete volatilization；At 40 DEG C
In the case of left and right, hydrogen content changes over time the volatilization for being primarily due to acetone.Wherein 40 DEG C solidifications, final protium content
Keep constant after acetone volatilizees completely, now the mass fraction of protium includes the protium in two parts, alloy in alloy
With the protium in bonding agent.
Wherein, after 40 DEG C of temperatures above solidify 2 hours, hydrogen content and bonding agent after alloy solidification are granulated from table 2
Compared with the difference of hydrogen content and alloy powder itself hydrogen content 0.21%, it can be seen that hydrogen content has all declined in alloy, 40
DEG C solidification hydrogen content be held essentially constant.In order to improve intensity, high-temperature curing agent can not be using cryogenic temperature solidification.Therefore to select
Selecting the solidification of 80 DEG C of temperature below can keep that hydrogen content is constant in alloy and can also meet the bonding agent of intensity requirement.
Meanwhile, in 160 DEG C of sheet samples solidified compared with the prilling powder before solidification, adiabatic temperature, which becomes Δ T, also to be had substantially
Decline, the corresponding Curie temperature Tc of peak point that adiabatic temperature becomes also is decreased obviously.As shown in figure 4, powder 1 and powder 2 into
It is respectively La0.7Ce0.3Fe11.4Mn0.2Si1.4HxWith La0.7Ce0.3Fe11.45Mn0.15Si1.4Hx；The powder that is flushed with hydrogen of two kinds of alloys exists
It is 2.5K and 2.4K respectively that thermal insulation temperature under 0.8T magnetic field intensities, which becomes,.Two kinds of alloy materials are granulated with identical curing agent, compacting
Slabbing sample, 160 DEG C solidify 1 hour after, measured under 0.8T magnetic field intensities thermal insulation temperature become be respectively 1.8K with
1.68K；Adiabatic temperature becomes the corresponding corresponding temperature of peak point also to be reduced respectively by original 283K (10 DEG C) and 293K (20 DEG C)
For 272K (- 1 DEG C) and 283K (10 DEG C).The sheet sample for being flushed with hydrogen powder, hot setting of two kinds of materials is in 0.8T magnetic field intensities
Under thermal insulation temperature become data be shown in Table 3.
Wherein：When the mass fraction of bonding agent is 3%, alloy powder viscosity is too big, is unfavorable for granulation.E44 epoxy resin
It is much better in 1: 1 granulation outcome with 650 polyamide ratios.
The bond samples for being flushed with hydrogen powder, the sheet sample of hot setting and cold curing of the material of table 1 are strong in different magnetic field
Entropy Changes under degree
Table it is 2-in-1 gold in hydrogen content with solidification temperature change
Thermal insulation temperature of the sheet sample for being flushed with hydrogen powder, hot setting of the material of table 3 under 0.8T magnetic field intensities becomes
Claims (5)
1. a kind of preparation method of LaFeSiH materials, it is characterized in that, specifically include following steps：
(1) La is chosen1-xRx(Fe13-y-bMy)SibHcAlloy is flushed with hydrogen powder；
(2) bonding agent being mixed to get in proportion using epoxy resin and curing agent；
(3) bonding agent matched somebody with somebody is flushed with hydrogen powder with alloy and is put into container, and pours into acetone as solvent, is stirred, waits to glue
Connect agent and alloy and be flushed with hydrogen powder and be well mixed and after after acetone volatilization, granulated, re-compacted shaping；
(4) sample after being molded solidifies at low temperature, and wherein low temperature is not higher than 80 DEG C.
2. a kind of preparation method of LaFeSiH materials according to claim 1, it is characterized in that, in step (1), under R is
One or several kinds of compositions of rare earth element are stated, the rare earth element is：Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、
Er、Tm、Yb、Lu、Sc、Y；X scope is：0≤x≤0.5；M is one kind in Mn, Ti, V, Cr, Co, Ni, Cu, Zn, Ga；Y's
Scope is：0.003≤y≤0.5；B scope is：1.0≤b≤1.5；C scope is：0≤c≤3.0.
3. a kind of preparation method of LaFeSiH materials according to claim 1 or 2, it is characterized in that, in step (1),
La1-xRx(Fe13-y-bMy)SibHcAlloy is flushed with hydrogen the control of the powder diameter of powder below 300 μm.
4. a kind of preparation method of LaFeSiH materials according to claim 1, it is characterized in that, in step (2), epoxy
The ratio of resin and curing agent is 1~2: 1.
5. a kind of preparation method of LaFeSiH materials according to claim 1 or 4, it is characterized in that, in step (2), glue
Connect agent account for alloy be flushed with hydrogen powder mass fraction be 1.5%-3%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109378148A (en) * | 2018-07-25 | 2019-02-22 | 中国科学院宁波材料技术与工程研究所 | A kind of lanthanum iron silicon substrate magnetic refrigerating material and preparation method thereof |
| CN112885549A (en) * | 2021-01-08 | 2021-06-01 | 哈尔滨工业大学 | Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system |
| CN115368711A (en) * | 2022-08-11 | 2022-11-22 | 湖北航泰科技有限公司 | Strong magnetocaloric effect fast curing epoxy resin |
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| CN112885549A (en) * | 2021-01-08 | 2021-06-01 | 哈尔滨工业大学 | Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system |
| CN112885549B (en) * | 2021-01-08 | 2022-09-20 | 哈尔滨工业大学 | Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system |
| CN115368711A (en) * | 2022-08-11 | 2022-11-22 | 湖北航泰科技有限公司 | Strong magnetocaloric effect fast curing epoxy resin |
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Application publication date: 20170908 |