CN107299268A - A kind of Mg base hydrogen bearing alloy with ultra-fine long period ordered structure and preparation method thereof - Google Patents

A kind of Mg base hydrogen bearing alloy with ultra-fine long period ordered structure and preparation method thereof Download PDF

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CN107299268A
CN107299268A CN201710324891.XA CN201710324891A CN107299268A CN 107299268 A CN107299268 A CN 107299268A CN 201710324891 A CN201710324891 A CN 201710324891A CN 107299268 A CN107299268 A CN 107299268A
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alloy
ultra
long period
hydrogen bearing
bearing alloy
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CN107299268B (en
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彭秋明
王栋彬
孙勇
刘先玉
赵翠玲
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Yanshan University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • 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
    • C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/383—Hydrogen absorbing alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/46—Alloys based on magnesium or aluminium
    • H01M4/466—Magnesium based
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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
    • Y02E60/10—Energy storage using batteries

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Hydrogen, Water And Hydrids (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

A kind of Mg base hydrogen bearing alloy with ultra-fine long period ordered structure, its chemical molecular formula is Mg aX bY, wherein, X represents one kind in Ni, Al, V, Co, Pt, a, b representation quality percentages, 6.52%≤a≤13.53%, 20.41%≤b≤21.50%；Surplus is Mg；The preparation method of above-mentioned Mg base hydrogen bearing alloy is mainly loads induction melting furnace by the alloying pellet of mentioned component, melting under an argon atmosphere, then to melted magnesium base alloy surface preparation, polishing, polishing, cleaning, and wrapped up with boron nitride tube, it is placed in high pressure cubic hydraulic press and enters horizontal high voltage compacting, 3 4GPa, temperature is increased to 800 1300 DEG C, 30 60min is incubated, obtains the Mg base hydrogen bearing alloy with ultra-fine long period ordered structure.Present invention process equipment is simple and easy to control, cost is low, obtained Mg base hydrogen bearing alloy compared to common process magnesium base alloy, inhale hydrogen discharging temperature it is lower, inhale hydrogen desorption kineticses performance it is more preferable.

Description

A kind of Mg base hydrogen bearing alloy with ultra-fine long period ordered structure and preparation method thereof
Technical field
The invention belongs to field of material technology, more particularly to a kind of hydrogen bearing alloy and preparation method thereof.
Background technology
With development in science and technology, petroleum resources, increasingly deficient and ecological environment constantly deteriorates, and new energy development turns into the whole mankind One urgent problem of urgent need to resolve.Hydrogen Energy is so that rich reserves, wide material sources, calorific value be high, clean pollution-free, regenerative resource and It is acknowledged as the preferable energy of human future.The exploitation of hydrogen storage material is the pass for solving hydrogen memory technology problem in Hydrogen Energy application Key.Hydrogen storage material is because of energy reversible absorption and releases hydrogen, is a kind of important carrier in the storage of hydrogen and course of conveying, plus Hydrogen and hydrogen storage material be " green " environment-friendly products, new energy development and environmental protection to future will play immeasurable Effect.In current all hydrogen storage modes, hydrogen bearing alloy absorbs hydrogen in the form of metal hydride, be a kind of safety, economy and Effective hydrogen storage mode.
Wherein, although Mg base hydrogen bearing alloy, which exists, inhales the defects such as hydrogen discharging temperature is high, suction hydrogen discharging rate is slow, because it has height Theoretical hydrogen storage capability, aboundresources, it is with low cost the advantages of be acknowledged as one of most potential light hydrogen occluding material, More particularly there is the appearance of the Mg base hydrogen bearing alloy of good hydrogen storage property, with its excellent mechanical property and physical property Have been widely used for the every field such as electronics industry, auto industry.
LaMg have studied with regard to someone early in the eighties in last century12、CeMg12、MmMg12、La2Mg17And La2Mg16Ni storage Hydrogen performance, although finding that this kind of Mg based alloys can inhale hydrogen at a lower temperature, hydrogen absorption capacity is relatively low, less than 4wt%, and And hydrogen discharging temperature is still very high, more than 300 DEG C.2011, Zhang Qingan et al. handled Mg using rapid solidification12During YNi alloys, hair Existing its has 18R type LPSO structures.When studying its hydrogen storage property, Mg is found12YNi shows good suction hydrogen desorption kineticses Energy.However, its hydrogen discharging temperature is still higher, and the microstructure of phase and suction put structural evolution during hydrogen not specifically It is bright.
The content of the invention
It is an object of the invention to provide a kind of technique it is simple, with low cost, the initial of magnesium-base hydrogen storage material can be reduced Hydrogen discharging temperature improves Mg base hydrogen bearing alloy of suction hydrogen discharging rate and preparation method thereof simultaneously.
The chemical molecular formula of the Mg base hydrogen bearing alloy with ultra-fine long period ordered structure of the present invention is Mg-aX-bY, X Represent one kind in Ni, Al, V, Co, Pt, a, b representation quality percentages, 6.52%≤a≤13.53%, 20.41%≤b≤ 21.50%；Surplus is Mg.
Above-mentioned element is simple metal powder.
The preparation method of the present invention is as follows：
1st, the melting of magnesium base alloy：
The alloying pellet of mentioned component chemical raw material is loaded into induction melting furnace, it is molten with conventional method under an argon atmosphere Refining；
2nd, magnesium base alloy surface preparation：
First, magnesium base alloy sand for surface paper is polished clean, successively from 180#, 320#, 600#, 1200#, 2000# Sand paper is polished alloy surface, it was observed that alloy surface cut direction is consistent, is then rushed with deionized water and alcohol Wash, polished magnesium base alloy material surface by the way of water throwing using polishing cloth, using absolute ethyl alcohol as cleaning agent, cleaning temperature For 15 DEG C, scavenging period is 10-15min；
3rd, high-voltage samples are assembled：
The magnesium base alloy that first step 2 is handled is fitted into boron nitride crucible with smooth parcel, crucible is integrally put into graphite In stove, then its top and bottom is sealed respectively with graphite-pipe external diameter identical graphite flake with two panels diameter, then by graphite Stove is integrally put into the pyrophillite groove of standard, and both sides are respectively put into graphite flake and conduction above and below the graphite crucible in pyrophillite groove Steel cap；
4th, high pressure is suppressed：
The high-voltage samples that step 3 is assembled are placed on the cavity position of high pressure cubic hinge press, by pressure rise to 3- 4GPa, 800-1300 DEG C is increased to 10 DEG C/min heating rate by temperature, is incubated 30-60min, is then shut off power supply stopping Heating, takes out high-voltage samples after being air-cooled to room temperature, release, obtains the Mg base hydrogen bearing alloy with ultra-fine long period ordered structure.
The present invention has the following advantages that compared with prior art：
1st, process equipment is simple, without adding catalyst, operates easily controllable.
2nd, in traditional induction melting technique, the operation of HIGH PRESSURE TREATMENT is with the addition of, there is the long period in alloy structure Sequence distributed mutually is more uniform, more finely, and the passage of hydrogen transport is finer and close, so as to greatly reinforce the hydrogen storage of alloy Energy.
3rd, obtained Mg base hydrogen bearing alloy has the advantages that hydrogen storage content is big, initial hydrogen discharging temperature is low, it is fast to inhale hydrogen discharging rate.
4th, it is cheap, it can be suitably used for producing in enormous quantities.
Brief description of the drawings
Fig. 1 is the obtained Mg with ultra-fine long period ordered structure of the embodiment of the present invention 112NiY alloys 250 DEG C, Hydrogen desorption kineticses curve map under the conditions of 1Mpa in 10 minutes.
Fig. 2 is the obtained Mg with ultra-fine long period ordered structure of the embodiment of the present invention 212AlY alloys 250 DEG C, PCT curve maps under the conditions of 1Mpa.
Fig. 3 is the obtained Mg with ultra-fine long period ordered structure of the embodiment of the present invention 312VY alloys are in 250 DEG C, 1Mpa Under the conditions of hydrogen desorption kineticses curve map in 10 minutes.
Fig. 4 is the obtained Mg with ultra-fine long period ordered structure of the embodiment of the present invention 412CoY alloys 250 DEG C, PCT curve maps under the conditions of 1Mpa.
Embodiment
Embodiment 1
The pure magnesium powders of 33.05g, 6.77g nickel powders and 10.18g yttrium powders are weighed, after being selected with 200 mesh sieves, is fitted into smelting furnace, is melted Refine 5 times and obtain Mg12NiY alloys, by the alloy wire cutting machine cutting into Φ 10mm × 8mm cylindrical specimens, are used successively 180#, 320#, 600#, 1200#, 2000# sand paper are polished alloy surface, it was observed that alloy surface cut direction is unanimously Can, then with deionized water and alcohol rinse, magnesium base alloy material surface is polished by the way of water throwing using polishing cloth, with Absolute ethyl alcohol is cleaning agent, and cleaning temperature is 15 DEG C, and scavenging period is 10min；
Then the alloy is fitted into boron nitride crucible with smooth parcel, crucible is integrally put into graphite furnace, then used Two panels diameter respectively seals its top and bottom with graphite-pipe external diameter identical graphite flake, and then graphite furnace is integrally put into mark In accurate pyrophillite groove, both sides are respectively put into graphite flake and conductive steel cap above and below the graphite crucible in pyrophillite groove, complete high Press the assembling of sample.
The above-mentioned high-voltage samples assembled are placed on to the cavity position of high pressure cubic hinge press, by pressure rise to 3GPa, Temperature is increased to 800 DEG C with 10 DEG C/min heating rate, 60min is incubated, power supply is then shut off and stops heating, be air-cooled to room High-voltage samples are taken out after temperature, release, the Mg base hydrogen bearing alloy with ultra-fine long period ordered structure is obtained.Test the suction of the alloy Hydrogen discharging performance, as shown in figure 1,250 DEG C when putting hydrogen, has completed to put hydrogen, compared to the Mg of traditional handicraft in 10 minutes12NiY is closed Gold, hydrogen storage total amount increases, and hydrogen discharging rate has also been accelerated.
Embodiment 2
The pure magnesium powders of 35.99g, 3.26g aluminium powders and 10.75g yttrium powders are weighed, after being selected with 200 mesh sieves, is fitted into smelting furnace, is melted Refine 5 times and obtain Mg12AlY alloys, by the alloy wire cutting machine cutting into Φ 10mm × 8mm cylindrical specimens, are used successively 180#, 320#, 600#, 1200#, 2000# sand paper are polished alloy surface, it was observed that alloy surface cut direction is unanimously Can, then with deionized water and alcohol rinse, magnesium base alloy material surface is polished by the way of water throwing using polishing cloth, with Absolute ethyl alcohol is cleaning agent, and cleaning temperature is 15 DEG C, and scavenging period is 15min；
Then the alloy is fitted into boron nitride crucible with smooth parcel, crucible is integrally put into graphite furnace, then used Two panels diameter respectively seals its top and bottom with graphite-pipe external diameter identical graphite flake, and then graphite furnace is integrally put into mark In accurate pyrophillite groove, both sides are respectively put into graphite flake and conductive steel cap above and below the graphite crucible in pyrophillite groove, complete high Press the assembling of sample.
The above-mentioned high-voltage samples assembled are placed on to the cavity position of high pressure cubic hinge press, by pressure rise to 4GPa, Temperature is increased to 1300 DEG C with 10 DEG C/min heating rate, 30min is incubated, power supply is then shut off and stops heating, be air-cooled to High-voltage samples are taken out after room temperature, release, the Mg base hydrogen bearing alloy with ultra-fine long period ordered structure is obtained.Test the alloy Hydrogen storage property, PCT curves as shown in Figure 2, at 250 DEG C, the alloy hydrogen absorption and desorption total amount reaches 5.1% or so, inhales/put hydrogen platform Press as 0.29/0.11MPa, compared to the Mg of traditional handicraft12AlY alloys, hydrogen storage total amount increases, and platform pressure reduces, Hysteresis quality reduces.
Embodiment 3
The pure magnesium powders of 33.64g, 5.96g vanadium powders and 10.40g yttrium powders are weighed, after being selected with 200 mesh sieves, is fitted into smelting furnace, is melted Refine 5 times and obtain Mg12VY alloys, by the alloy wire cutting machine cutting into Φ 10mm × 8mm cylindrical specimens, are used successively 180#, 320#, 600#, 1200#, 2000# sand paper are polished alloy surface, it was observed that alloy surface cut direction is unanimously Can, then with deionized water and alcohol rinse, magnesium base alloy material surface is polished by the way of water throwing using polishing cloth, with Absolute ethyl alcohol is cleaning agent, and cleaning temperature is 15 DEG C, and scavenging period is 12min；
Then the alloy is fitted into boron nitride crucible with smooth parcel, crucible is integrally put into graphite furnace, then used Two panels diameter respectively seals its top and bottom with graphite-pipe external diameter identical graphite flake, and then graphite furnace is integrally put into mark In accurate pyrophillite groove, both sides are respectively put into graphite flake and conductive steel cap above and below the graphite crucible in pyrophillite groove, complete high Press the assembling of sample.
The above-mentioned high-voltage samples assembled are placed on to the cavity position of high pressure cubic hinge press, by pressure rise to 3GPa, Temperature is increased to 1000 DEG C with 10 DEG C/min heating rate, 50min is incubated, power supply is then shut off and stops heating, be air-cooled to High-voltage samples are taken out after room temperature, release, the Mg base hydrogen bearing alloy with ultra-fine long period ordered structure is obtained.Test the alloy Hydrogen storage property, as shown in figure 3,250 DEG C when putting hydrogen, has completed to put hydrogen, compared to the Mg of traditional handicraft in 10 minutes12VY is closed Gold, hydrogen storage total amount increases, and hydrogen discharging rate has also been accelerated.
Embodiment 4
The pure magnesium powders of 33.03g, 6.76g cobalt powders and 10.21g yttrium powders are weighed, after being selected with 200 mesh sieves, is fitted into smelting furnace, is melted Refine 5 times and obtain Mg12CoY alloys, by the alloy wire cutting machine cutting into Φ 10mm × 8mm cylindrical specimens, are used successively 180#, 320#, 600#, 1200#, 2000# sand paper are polished alloy surface, it was observed that alloy surface cut direction is unanimously Can, then with deionized water and alcohol rinse, magnesium base alloy material surface is polished by the way of water throwing using polishing cloth, with Absolute ethyl alcohol is cleaning agent, and cleaning temperature is 15 DEG C, and scavenging period is 13min；
Then the alloy is fitted into boron nitride crucible with smooth parcel, crucible is integrally put into graphite furnace, then used Two panels diameter respectively seals its top and bottom with graphite-pipe external diameter identical graphite flake, and then graphite furnace is integrally put into mark In accurate pyrophillite groove, both sides are respectively put into graphite flake and conductive steel cap above and below the graphite crucible in pyrophillite groove, complete high Press the assembling of sample.
The above-mentioned high-voltage samples assembled are placed on to the cavity position of high pressure cubic hinge press, by pressure rise to 4GPa, Temperature is increased to 1200 DEG C with 10 DEG C/min heating rate, 40min is incubated, power supply is then shut off and stops heating, be air-cooled to High-voltage samples are taken out after room temperature, release, the Mg base hydrogen bearing alloy with ultra-fine long period ordered structure is obtained.Test the alloy Hydrogen storage property, PCT curves as shown in Figure 4, at 250 DEG C, the alloy hydrogen absorption and desorption total amount reaches 5.0% or so, inhales/put hydrogen platform Press as 0.27/0.1MPa, compared to the Mg of traditional handicraft12CoY alloys, hydrogen storage total amount increases, and platform pressure reduces, stagnant Property reduces afterwards.

Claims (3)

1. a kind of Mg base hydrogen bearing alloy with ultra-fine long period ordered structure, it is characterised in that：Its chemical molecular formula is Mg- AX-bY, X represent one kind in Ni, Al, V, Co, Pt, a, b representation quality percentage, 6.52%≤a≤13.53%, 20.41% ≤ b≤21.50%；Surplus is Mg.
2. the Mg base hydrogen bearing alloy according to claim 1 with ultra-fine long period ordered structure, it is characterised in that：It is described Raw material is simple metal powder.
3. the preparation method of the Mg base hydrogen bearing alloy with ultra-fine long period ordered structure described in claim 1, its feature exists In：
(1) melting of magnesium base alloy：
The alloying pellet of mentioned component chemical raw material is loaded into induction melting furnace, under an argon atmosphere melting；
(2) magnesium base alloy surface preparation：
First, magnesium base alloy sand for surface paper is polished clean, successively from 180#, 320#, 600#, 1200#, 2000# sand paper Alloy surface is polished, it was observed that alloy surface cut direction is consistent, then with deionized water and alcohol rinse, profit Magnesium base alloy material surface is polished by the way of water throwing with polishing cloth, using absolute ethyl alcohol as cleaning agent, cleaning temperature is 15 DEG C, scavenging period is 10-15min；
(3) high-voltage samples are assembled：
First the magnesium base alloy of step (2) processing is fitted into boron nitride crucible with smooth parcel, crucible is integrally put into graphite furnace In, then its top and bottom is sealed respectively with graphite-pipe external diameter identical graphite flake with two panels diameter, then by graphite furnace Entirety is put into the pyrophillite groove of standard, and both sides are respectively put into graphite flake and conductive steel above and below the graphite crucible in pyrophillite groove Cap；
(4) high pressure is suppressed：
The high-voltage samples that step (3) is assembled are placed on the cavity position of high pressure cubic hinge press, by pressure rise to 3-4GPa, Temperature is increased to 800-1300 DEG C with 10 DEG C/min heating rate, 30-60min is incubated, power supply is then shut off and stops heating, High-voltage samples are taken out after being air-cooled to room temperature, release, the Mg base hydrogen bearing alloy with ultra-fine long period ordered structure is obtained.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108707802A (en) * 2018-06-12 2018-10-26 上海大学 Mg-Ni-Y alloys of the ordered phase containing long period and preparation method thereof
CN110697652A (en) * 2019-11-20 2020-01-17 榆林学院 Preparation method of yttrium/graphene modified magnesium-aluminum hydrogen storage composite material
CN116115818A (en) * 2021-11-12 2023-05-16 刘庄 Active metal microsphere, composite embolic agent based on active metal microsphere and application of composite embolic agent

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108707802A (en) * 2018-06-12 2018-10-26 上海大学 Mg-Ni-Y alloys of the ordered phase containing long period and preparation method thereof
CN110697652A (en) * 2019-11-20 2020-01-17 榆林学院 Preparation method of yttrium/graphene modified magnesium-aluminum hydrogen storage composite material
CN116115818A (en) * 2021-11-12 2023-05-16 刘庄 Active metal microsphere, composite embolic agent based on active metal microsphere and application of composite embolic agent

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