CN110257651A - A kind of Mg-Ni-Y hydrogen bearing alloy and preparation method thereof with polyphase eutectic tissue - Google Patents
A kind of Mg-Ni-Y hydrogen bearing alloy and preparation method thereof with polyphase eutectic tissue Download PDFInfo
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- CN110257651A CN110257651A CN201910631665.5A CN201910631665A CN110257651A CN 110257651 A CN110257651 A CN 110257651A CN 201910631665 A CN201910631665 A CN 201910631665A CN 110257651 A CN110257651 A CN 110257651A
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The present invention provides a kind of high-performance Mg-Ni-Y hydrogen bearing alloy and preparation method thereof with polyphase eutectic tissue, chemical constitution formula Mg100‑x‑yNiyYx, wherein MgYNi is contained in 5≤x≤11,8≤y≤134, Mg2Ni and long period stacking order structure (LPSO) and Mg phase polyphase eutectic tissue; the preparation of alloy is using Mg, Mg-30Y, Y and Mg-50Ni metal as raw material; Mg-Ni-Y hydrogen bearing alloy is arrived by coverture Protection Code molten alloy using graphite crucible in well formula resistance furnace；Mg-Ni-Y hydrogen bearing alloy provided by the present invention has very high activity, can normally inhale hydrogen release after once inhaling hydrogen release activation；Add nickel and yttrium in Mg base hydrogen bearing alloy, the suction hydrogen discharging temperature of alloy is substantially reduced, Mg-Ni-Y hydrogen bearing alloy provided by the invention has good activity function and good suction hydrogen desorption kinetics performance, 2min interior suction hydrogen 3.5wt.% is depressed in 300 DEG C, 3MPa hydrogen, reach the 80% of total hydrogen-sucking amount 4.4wt.%, preparation method of the present invention is simple, and the Mg base hydrogen bearing alloy containing polyphase eutectic tissue prepared has good hydrogen storage property, is suitble to industrialized production.
Description
Technical field
The invention belongs to hydrogen storage material technical fields, relate to the use of Mg-Ni-Y phasor and organization optimization design Mg-base hydrogen-bearing
A kind of method of alloy, and in particular to Mg-Ni-Y hydrogen bearing alloy and preparation method thereof with polyphase eutectic tissue.
Background technique
Hydrogen is known as 21 century secondary energy sources most with prospects, applies in Aeronautics and Astronautics, navigation and fuel cell vapour
The fields such as vehicle can also be used as abandonment in other clean energy resource development and abandon the energy carrier that light abandons electricity comprehensive utilization, are also simultaneously
The important source material of the fossil energies clean utilization such as grade of oil upgrading and coal clean energy resource, the development and utilization of hydrogen have obtained the world
The highest attention of various countries.But the Mass storage and transportation problem of hydrogen are not still resolved, and have seriously affected hydrogen energy source
Application.
The theoretical hydrogen storage content of magnesium metal is up to 7.6wt%, is that hydrogen-storage density is highest in all metal hydrogen storage materials, remote high
In conventional high-pressure gaseous state hydrogen storage content (less than 1wt%).In addition magnesium resource is abundant, cheap, in the large scale storage side of hydrogen
The great application prospect in face, Mg base hydrogen bearing alloy are considered as a kind of ideal hydrogen storage material of most possible large-scale application.But gold
Belong to magnesium and inhale that hydrogen discharging temperature is high, rate is slow etc. and limits its practical application.Recent study personnel use a variety of methods to improve
These are insufficient, such as addition transition metal or rare earth element, mechanical alloying.
Some researches show that, the size of catalytic phase and its with main suction hydrogen phase distribution, to the suction hydrogen release of Mg base hydrogen bearing alloy
Performance is most important.The catalytic phase of fine uniform distribution, is expected to further increase the hydrogen storage property of Mg base hydrogen bearing alloy.Although
Lot of domestic and foreign scholar has carried out extensive research to Mg base hydrogen bearing alloy, but still needing further to design to find has high property
The magnesium base alloy of energy, to reduce cost and there are good suction hydrogen desorption kinetics.
Summary of the invention
In order to solve the problems in the existing technology, the present invention provides a kind of Mg-Ni-Y with polyphase eutectic tissue
Hydrogen bearing alloy and preparation method improve the suction hydrogen desorption kinetics performance and hydrogen storage property of Mg base hydrogen bearing alloy.
To achieve the goals above, the technical solution adopted by the present invention is that, a kind of Mg-Ni-Y with polyphase eutectic tissue
Hydrogen bearing alloy, alloying component is at the rich magnesium end of Mg-Ni-Y ternary phase diagrams, in ternary eutectic point and eutectic line, Mg-Ni-Y storage
Hydrogen alloy formula is Mg100-x-yNiyYx, wherein 5≤x≤11,8≤y≤13, the Mg-Ni-Y hydrogen bearing alloy have multiphase
Eutectic structure.
The polyphase eutectic tissue includes MgYNi4Phase, Mg2Ni phase, Mg and long period stacking order structure phase.
It is 60%-70% that the long period stacking order structure, which mutually accounts for the Mg-Ni-Y hydrogen bearing alloy volume, remaining is
MgYNi4、Mg2Ni and Mg.
Further, x=10.35, y=12.78.
The preparation method of Mg-Ni-Y hydrogen bearing alloy of the present invention, comprising the following steps:
According to melting component melting Mg-Ni-Y hydrogen bearing alloy described in claim 1, obtainMolten stateMg-Ni-Y hydrogen storage is closed
Gold；By the molten state Mg-Ni-Y hydrogen bearing alloy furnace cooling, as cast condition Mg-Ni-Y hydrogen bearing alloy is obtained.
Smelting temperature is 850 ± 15 DEG C.
On the surface of raw material, paving spills RJ-2 type coverture.
Melting is carried out in well formula resistance furnace using graphite crucible.
The raw material used is Mg, Mg-30Y, Y and Mg-50Ni, and the purity of the raw material is all larger than 99%.
Compared with prior art, the present invention at least has the advantages that Mg-Ni-Y hydrogen storage provided by the present invention is closed
Fitting has very high activity, can normally inhale hydrogen release after once inhaling hydrogen release activation；By being added in Mg base hydrogen bearing alloy
Metallic element nickel and rare earth element yttrium are crossed, the suction hydrogen discharging temperature of alloy is substantially reduced, and at the same time, the suction hydrogen discharging rate of alloy is bright
Aobvious to improve, Y itself has good catalytic action, furthermore the Mg that Mg and Ni is formed2Ni also shows efficient catalytic action；This
The prepared Mg-Ni-Y hydrogen bearing alloy of invention contains Mg2Ni, Mg, MgYNi4With long period stacking order structure (LPSO), wherein
Mg、MgYNi4It is ternary eutectic phase with long period stacking order structure (LPSO), and long period stacking order structure (LPSO) accounts for
To 60%-70% percent by volume, the reversible hydrogen-sucking amount of Mg-Ni-Y hydrogen bearing alloy prepared by the present invention up to 4.4wt.%,
300 DEG C, 3MPa hydrogen pressure 2min interior suction hydrogen 3.5wt.%, reach the 80% of total hydrogen-sucking amount, are guaranteeing magnesium alloy circulation suction hydrogen release
Under the premise of total amount, greatly improves and inhale hydrogen speed；Preparation process of the present invention is simple, is suitble to industrialized production.
Detailed description of the invention
Fig. 1 is the ternary phase diagrams of Mg-Ni-Y alloy；
Fig. 2 is prepared Mg76.87Ni12.78Y10.35、Mg82.35Ni12.11Y5.54、Mg88.7Ni8.3Y5The SEM of cast alloy
Figure；
Fig. 3 is prepared Mg76.87Ni12.78Y10.35The TEM of cast alloy schemes；
Fig. 4 is prepared Mg76.87Ni12.78Y10.35Dynamic isotherms of hydrogen absorption figure of the cast alloy at 300 DEG C, 3MPa；
Fig. 5 is prepared Mg76.87Ni12.78Y10.35PCT curve graph of the cast alloy at 300 DEG C, 3MPa；
Fig. 6 is prepared Mg76.87Ni12.78Y10.35Cast alloy saturation inhales the XRD diagram after hydrogen.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
A kind of Mg-Ni-Y hydrogen bearing alloy with polyphase eutectic tissue, rich magnesium of the alloying component in Mg-Ni-Y ternary phase diagrams
End, in ternary eutectic point and eutectic line, Mg-Ni-Y hydrogen bearing alloy chemical formula is Mg100-x-yNiyYx, wherein 5≤x≤11,
8≤y≤13, the Mg-Ni-Y hydrogen bearing alloy have polyphase eutectic tissue.
The polyphase eutectic tissue includes MgYNi4Phase, Mg2Ni phase, Mg and long period stacking order structure phase.
It is 60%-70% that the long period stacking order structure, which mutually accounts for the Mg-Ni-Y hydrogen bearing alloy volume, remaining is
MgYNi4、Mg2Ni and Mg.
The preparation method of Mg-Ni-Y hydrogen bearing alloy, comprising the following steps:
It is Mg according to Mg-Ni-Y hydrogen bearing alloy chemical formula100-x-yNiyYx, wherein 5≤x≤11%, 8≤y≤13；Melting
Mg-Ni-Y hydrogen bearing alloy obtains molten state Mg-Ni-Y hydrogen bearing alloy；The molten state Mg-Ni-Y hydrogen bearing alloy is cold with furnace
But, as cast condition Mg-Ni-Y hydrogen bearing alloy is obtained；
Smelting temperature is 850 ± 15 DEG C.
On the surface of raw material, paving spills RJ-2 type coverture.
Melting is carried out in well formula resistance furnace using graphite crucible.
The raw material used is Mg, Mg-30Y, Y and Mg-50Ni, and the purity of the raw material is all larger than 99%.
Embodiment 1
According to Mg100-x-yNiyYxChemical constitution formula, in the present embodiment, x=10.35；Y=12.78；Mg member is considered simultaneously
The melting loss of element, calculates and weighs raw material Mg, Mg-30Y, Y and Mg-50Ni purity and be all larger than 99%, by the raw material
It is put into graphite crucible, uniformly paving spills one layer of RJ-2 coverture, is smelted into reality under 850 DEG C of ± 15 DEG C of high temperature using well formula resistance furnace
Border chemical constitution formula is Mg76.87Ni12.78Y10.35Alloy cast ingot.
Embodiment 2
According to Mg100-x-yNiyYxChemical constitution formula, for the present embodiment: x=5.54；Y=12.11, while considering Mg
The melting loss of element, calculates and weighs raw material Mg, Mg-30Y, Y and Mg-50Ni, and the purity of the raw material is all larger than
99%, graphite crucible is put raw materials into, uniformly paving spills one layer of RJ-2 coverture, using well formula resistance furnace at 850 DEG C ± 15 DEG C
It is Mg that practical chemical constitution formula is smelted under high temperature82.35Ni12.11Y5.54Alloy cast ingot.
Embodiment 3, according to Mg100-x-yNiyYxChemical constitution formula, for the present embodiment, x=5；Y=8.3 considers simultaneously
The melting loss of Mg element, calculates and weighs raw material Mg, Mg-30Y, Y and Mg-50Ni, and the purity of the raw material is all larger than
99%, graphite crucible is put raw materials into, uniformly paving spills one layer of RJ-2 coverture, using well formula resistance furnace at 850 DEG C ± 15 DEG C
It is Mg that practical chemical constitution formula is smelted under high temperature88.7Ni8.3Y5Alloy cast ingot.
Fig. 2-1 is Mg76.87Ni12.78Y10.35The microscopic examination of cast alloy, the ingredient are Mg-Ni-Y ternary phase diagrams
Eutectic point E1, as seen from the figure, Mg76.87Ni12.78Y10.35The as-cast structure of cast alloy has white, black and three kinds of Dark grey
Contrast.In conjunction with EDS energy spectrum analysis it can be concluded that Mg76.87Ni12.78Y10.35Cast alloy is by white irregular bulk MgNi4Y, black
The wide strip LPSO of color, white needles slice Mg2Ni and black bar Mg composition.
Likewise, Fig. 2-2 is Mg82.35Ni12.11Y5.54The microscopic structure of cast alloy, EDS energy spectrum analysis can obtain the alloy
In white it is irregular blocky be Y phase, the wide item of white or fine acicular be Mg2Ni, black plum blossom-shaped are Mg phase.
Fig. 2-3 is Mg88.7Ni8.3Y5The microscopic structure of cast alloy, EDS energy spectrum analysis obtain Mg88.7Ni8.3Y5Cast alloy
Middle irregular bulk of white be still Y phase, black plum blossom-shaped be Mg phase, white fine acicular is Mg2Ni and the wide strip of black are LPSO
Structure.
Fig. 3 is Mg76.87Ni12.78Y10.35TEM image, selective electron diffraction style and the high-resolution TEM figure of cast alloy
Picture.Fig. 3-1 is Mg76.87Ni12.78Y10.35The TEM image and full resolution pricture of cast alloy, Fig. 3-2 are corresponding Selected area electron
Diffraction pattern.It include a large amount of LPSO structures in cast alloy, electron diffraction pattern and high-resolution TEM result show that it is
14H type LPSO structure.
By Mg76.87Ni12.78Y10.35Alloy cast ingot is cut into small cube, removes alloy surface oxide skin with sand paper polishing, adopts
The granular alloy for being 0.4~0.6mm at average grain diameter by small cube size degradation with the method for Mechanical Crushing, obtains Mg-base hydrogen-bearing
Alloy carries out the graininess alloy to inhale hydrogen test.
Absorption hydrogen with polyphase eutectic tissue is had excellent performance, as shown in figure 4, the alloy is in 300 DEG C and 3MPa hydrogen pressure
Total hydrogen-sucking amount reaches the 80% of total hydrogen-sucking amount in 2min interior suction hydrogen 3.5wt.% up to 4.4wt.% in lower 1h.As shown in figure 5,
Suction hydrogen release good cycle of the alloy at 300 DEG C, reversible hydrogen-sucking amount reach 4wt.%.
Fig. 6 is that material phase analysis of the as cast condition Mg-Ni-Y hydrogen bearing alloy after saturation inhales hydrogen is inhaled in saturation as seen from the figure
Mg-Ni-Y hydrogen bearing alloy after hydrogen is by MgH2、Mg2NiH0.3、Mg2NiH4、YH2And YH3Composition, existing research show that Mg-Ni-Y is stored up
LPSO is decomposed during hydrogen absorption hydrogen, and forms the Mg for the nanoscale that even dispersion is distributed within the scope of long-range2Ni and YH2；
MgYNi4Suction hydrogen mutually can be carried out in the case where temperature is 313K, the suction that the presence of the phase advantageously reduces Mg-Ni-Y hydrogen bearing alloy is put
Hydrogen temperature.LPSO structure and Mg at the same time2The presence of Ni phase inhales the promotion work that hydrogen plays catalysis to Mg-Ni-Y hydrogen bearing alloy
With so that Mg-Ni-Y hydrogen bearing alloy obtains higher hydrogen-sucking amount in a very short period of time.
Claims (9)
1. a kind of Mg-Ni-Y hydrogen bearing alloy with polyphase eutectic tissue, which is characterized in that alloying component is in Mg-Ni-Y ternary
The rich magnesium end of phasor, in ternary eutectic point and eutectic line, Mg-Ni-Y hydrogen bearing alloy chemical formula is Mg100-x-yNiyYx,
In, 5≤x≤11,8≤y≤13, the Mg-Ni-Y hydrogen bearing alloy is with polyphase eutectic tissue.
2. Mg-Ni-Y hydrogen bearing alloy according to claim 1, which is characterized in that the polyphase eutectic tissue includes MgYNi4
Phase, Mg2Ni phase, Mg and long period stacking order structure phase.
3. Mg-Ni-Y hydrogen bearing alloy according to claim 2, which is characterized in that the long period stacking order structure
Mutually accounting for the Mg-Ni-Y hydrogen bearing alloy volume is 60%-70%, remaining is MgYNi4、Mg2Ni and Mg.
4. Mg-Ni-Y hydrogen bearing alloy according to claim 2, which is characterized in that x=10.35, y=12.78.
5. a kind of preparation method of Mg-Ni-Y hydrogen bearing alloy, which is characterized in that according to melting component melting described in claim 1
Mg-Ni-Y hydrogen bearing alloy obtains molten state Mg-Ni-Y hydrogen bearing alloy；The molten state Mg-Ni-Y hydrogen bearing alloy is cold with furnace
But, as cast condition Mg-Ni-Y hydrogen bearing alloy is obtained.
6. the preparation method of Mg-Ni-Y hydrogen bearing alloy according to claim 5, which is characterized in that smelting temperature be 850 ±
15℃。
7. the preparation method of Mg-Ni-Y hydrogen bearing alloy according to claim 5, which is characterized in that on the surface of raw material
Paving spills RJ-2 type coverture.
8. the preparation method of Mg-Ni-Y hydrogen bearing alloy according to claim 5, which is characterized in that existed using graphite crucible
Well formula resistance furnace carries out melting.
9. the preparation method of Mg-Ni-Y hydrogen bearing alloy according to claim 5, which is characterized in that the raw material used for
Mg, Mg-30Y, Y and Mg-50Ni, and the purity of the raw material is all larger than 99%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113862536A (en) * | 2021-09-14 | 2021-12-31 | 钢铁研究总院 | Mg-Al-Y-based hydrogen storage material and preparation method thereof |
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| CN1962914A (en) * | 2006-12-07 | 2007-05-16 | 上海交通大学 | Cast magnesium alloy containing rare-earth and preparation method thereof |
| CN101008060A (en) * | 2006-11-30 | 2007-08-01 | 中国科学院长春应用化学研究所 | Heat-proof magnesium-base rare earth alloy and its preparation method |
| CN102337438A (en) * | 2011-09-26 | 2012-02-01 | 华南理工大学 | Magnesium-based hydrogen storage alloy with long period structure and preparation method thereof |
| CN107345282A (en) * | 2017-06-29 | 2017-11-14 | 上海大学 | Magnesium-base nanometer composite hydrogen-storing material of catalytic phase Dispersed precipitate and preparation method thereof |
| EP3330393A1 (en) * | 2007-06-28 | 2018-06-06 | Sumitomo Electric Industries, Ltd. | Magnesium alloy sheet |
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| CN101008060A (en) * | 2006-11-30 | 2007-08-01 | 中国科学院长春应用化学研究所 | Heat-proof magnesium-base rare earth alloy and its preparation method |
| CN1962914A (en) * | 2006-12-07 | 2007-05-16 | 上海交通大学 | Cast magnesium alloy containing rare-earth and preparation method thereof |
| EP3330393A1 (en) * | 2007-06-28 | 2018-06-06 | Sumitomo Electric Industries, Ltd. | Magnesium alloy sheet |
| CN102337438A (en) * | 2011-09-26 | 2012-02-01 | 华南理工大学 | Magnesium-based hydrogen storage alloy with long period structure and preparation method thereof |
| CN107345282A (en) * | 2017-06-29 | 2017-11-14 | 上海大学 | Magnesium-base nanometer composite hydrogen-storing material of catalytic phase Dispersed precipitate and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113862536A (en) * | 2021-09-14 | 2021-12-31 | 钢铁研究总院 | Mg-Al-Y-based hydrogen storage material and preparation method thereof |
| CN113862536B (en) * | 2021-09-14 | 2022-07-08 | 钢铁研究总院 | Mg-Al-Y-based hydrogen storage material and preparation method thereof |
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