CN105692553A - Preparation process for nanometer magnesium-based hydrogen storage alloy hydride - Google Patents
Preparation process for nanometer magnesium-based hydrogen storage alloy hydride Download PDFInfo
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- CN105692553A CN105692553A CN201610025351.7A CN201610025351A CN105692553A CN 105692553 A CN105692553 A CN 105692553A CN 201610025351 A CN201610025351 A CN 201610025351A CN 105692553 A CN105692553 A CN 105692553A
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 55
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 55
- 239000011777 magnesium Substances 0.000 title claims abstract description 51
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 150000004678 hydrides Chemical class 0.000 title claims abstract description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000956 alloy Substances 0.000 title abstract description 15
- 229910045601 alloy Inorganic materials 0.000 title abstract description 15
- 238000003860 storage Methods 0.000 title abstract description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000000151 deposition Methods 0.000 claims abstract description 20
- 230000008020 evaporation Effects 0.000 claims abstract description 20
- 238000001704 evaporation Methods 0.000 claims abstract description 20
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 17
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 4
- 239000001996 bearing alloy Substances 0.000 claims description 16
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 16
- 238000009413 insulation Methods 0.000 claims description 16
- 229910052759 nickel Inorganic materials 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- 238000005516 engineering process Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 150000002431 hydrogen Chemical class 0.000 claims description 11
- 238000013508 migration Methods 0.000 claims description 5
- 229910052756 noble gas Inorganic materials 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 3
- 230000008021 deposition Effects 0.000 abstract 3
- 238000005275 alloying Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000011261 inert gas Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 238000001228 spectrum Methods 0.000 description 12
- 239000012071 phase Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 6
- 238000010926 purge Methods 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- 239000011232 storage material Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000010406 cathode material Substances 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 229910052987 metal hydride Inorganic materials 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910019758 Mg2Ni Inorganic materials 0.000 description 1
- 229910017961 MgNi Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910012375 magnesium hydride Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000001330 spinodal decomposition reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/24—Hydrides containing at least two metals; Addition complexes thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B3/0078—Composite solid storage mediums, i.e. coherent or loose mixtures of different solid constituents, chemically or structurally heterogeneous solid masses, coated solids or solids having a chemically modified surface region
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Hydrogen, Water And Hydrids (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention provides a preparation process for nanometer magnesium-based hydrogen storage alloy hydride. The preparation process for nanometer magnesium-based hydrogen storage alloy hydride is characterized in that magnesium powder serves as an evaporation source, nanometer nickel powder carried by a multiwalled carbon nanotube serves as a deposition base, the evaporation source and the deposition base are separately put in the same reactor, inert gas is introduced into the reactor, vacuumizing is performed, then hydrogen is introduced before the temperature is raised and the pressure is maintained, the evaporation source is transferred to the deposition base through a gas phase, an alloying and hydrogenation reaction is performed, the temperature is dropped, and finally nanometer magnesium-based hydrogen storage alloy hydride with high activity is obtained. Through the preparation process, nanometer magnesium-based hydrogen storage alloy hydride can be synthesized in one step, and the synthesized product has the advantages that the particle size is small, dispersity is good, and activity is high; meanwhile, the product is controllable in composition and can be widely applied to the field of gas-state and electrochemical hydrogen storage. The preparation process is simple and suitable for industrial production.
Description
Technical field
The present invention relates to the preparation technology of a kind of nano Mg base hydrogen bearing alloy hydride, be specifically related to the nano Mg base hydrogen bearing alloy hydride prosperity preparation technology that one can be used as the accumulating of nickel-metal hydrides (Ni-MH) secondary battery cathode material and hydrogen。
Background technology
In solid-state hydrogen storage material system, Mg base hydrogen bearing alloy is interesting because of its advantage such as high hydrogen-storage density, cheap, aboundresources, is the important candidate of novel energy-storing material。But the mg-based material belonging to middle warm type hydrogen bearing alloy typically require about 300 DEG C could effectively inhale put hydrogen and inhale hydrogen desorption kinetics poor；As nickel-hydrogen battery negative pole material, Mg2Ni theoretical electrochemistry capacity is 999mAh/g, is much higher than the AB having been carried out industrialization5Type alloy (372mAh/g), but in actual applications, due to its hydride at room temperature stable and not easily dehydrogenation cause Mg2The available capacity of Ni is low, so Mg system alloy not yet can apply to Ni-MH battery。
The intrinsic drag of restriction magnesium system hydrogen storage material development is higher thus having higher thermodynamic stability (decomposition temperature under 0.1MPa is 288 DEG C) owing to its hydride TiFe_xM_y alloy。On the one hand, by adopting magnesium-yttrium-transition metal can be effectively improved the thermodynamic property of material with magnesium chemical combination formation magnesium base alloy；On the other hand, Theoretical Calculation shows, puts hydrogen enthalpy make hydride spinodal decomposition when particle size nanorize can significantly reduce, thus reducing desorption temperature；Meanwhile, nano material has higher specific surface area, abundant crystal boundary and defect concentration, is conducive to hydrogen to spread。In view of the many advantages of nano hydrogen-storage material, develop controlled, volume production, the nano Mg base material preparation technology of low energy consumption is considered as the important channel that this system hydrogen storage material can obtain that internal is broken through。
Chen etc. report and utilize vapor phase growth without supporting the correlation technique namely synthesizing Mg nano wire, this nanowire diameter 30-170nm, wherein the Mg nano wire of 30-50nm demonstrates the suction hydrogen desorption kinetics performance [W.Y.Lietal.JournaloftheAmericanChemicalSociety.129 (2007) 6710～6711] of excellence。But yet there are no relevant with the present invention at present both at home and abroad, adopt any report of gas-migration technology one-step synthesis nano Mg base hydrogen bearing alloy hydride。
Summary of the invention
It is an object of the invention to provide the preparation technology of a kind of highly active nano Mg base hydrogen bearing alloy hydride in order to improve the deficiencies in the prior art；This nano Mg base hydrogen bearing alloy hydride can be applicable to nickel-metal hydrides (Ni-MH) secondary battery cathode material and other need in the occasions such as the storage of hydrogen, transport。
The technical scheme is that the preparation technology of a kind of nano Mg base hydrogen bearing alloy hydride, it is characterized in that with magnesium powder for evaporation source, nano nickel powder is carried for depositing base with multi-walled carbon nano-tubes, and both are separately placed in same reactor, pass into noble gas evacuation (air to remove in reactor), heat up and pressurize after then passing to hydrogen, evaporation source is by gas-migration to the concurrent intercrescence aurification of depositing base and hydrogenation, cooling, finally gives highly active nano Mg base hydrogen bearing alloy hydride。
In preferred feedstock magnesium powder and multi-walled carbon nano-tubes load nano nickel powder, magnesium is 2.0-5.0 with the mol ratio of nickel。
The preferably above-mentioned load nickel quality in multi-walled carbon nano-tubes load nano nickel powder is 10-40%。The preparation method of multi-walled carbon nano-tubes load nano nickel powder with reference to this seminar publish thesis [Yang Yang et al.. Rare Metals Materials and engineering .42 (2013) 1459～1463]。
550-600 DEG C it is warmed up to, heat-insulation pressure keeping 15 minutes to 10 hours after being preferably pressed into hydrogen；Preferred pressurize hydrogen pressure is 0.1-2.0MPa；Evaporation source passes through gas-migration to the concurrent intercrescence aurification of depositing base and hydrogenation, it is preferable that cooling is first to be cooled to 300-360 DEG C, heat-insulation pressure keeping 15 minutes to 4 hours, and last natural cooling obtains nano Mg base hydrogen bearing alloy hydride。
The markets such as above-mentioned magnesium powder and multi-wall carbon nano-tube pipe powder are all on sale。
Nano Mg base hydrogen bearing alloy hydride prepared by the present invention can nickel-metal hydrides (Ni-MH) secondary battery cathode material and other need in the occasions such as the storage of hydrogen, transport apply。
Beneficial effect:
1. utilizing technology of preparing provided by the present invention, it is possible to one-step synthesis high-activity nano Mg base hydrogen bearing alloy hydride, preparation process technique is simple, is suitable for industrialized production。
2. the present invention obtains magnesium gaseous atom by evaporation source gas-migration, carry at multi-walled carbon nano-tubes afterwards and obtain nanoscale magnesium base alloy hydride under the restriction effect of nano nickel depositing base, product not only granule is tiny, and has good homogeneity, dispersivity, is not susceptible to particle agglomeration。
3. product component can be carried out Reasonable Regulation And Control to realize product application in electrochemical hydrogen storage and other hydrogen accumulating occasion by process optimization。
Accompanying drawing explanation
The X ray diffracting spectrum of Fig. 1 embodiment 1 synthetic product；
The X ray diffracting spectrum of the 2-in-1 one-tenth product of Fig. 2 embodiment；
The X ray diffracting spectrum of Fig. 3 embodiment 3 synthetic product；
The X ray diffracting spectrum of Fig. 4 embodiment 4 synthetic product；
The X ray diffracting spectrum of Fig. 5 embodiment 5 synthetic product；
The X ray diffracting spectrum of Fig. 6 embodiment 6 synthetic product。
Detailed description of the invention
By the examples below the present invention is elaborated；Multi-walled carbon nano-tubes load nano nickel powder described in following example with reference to this seminar publish thesis [Yang Yang et al.. Rare Metals Materials and engineering .42 (2013) 1459～1463] prepare。
Embodiment 1
With magnesium powder for evaporation source, carry nano nickel (load nickel amount is for 40wt.%) powder for depositing base with multi-walled carbon nano-tubes。Wherein magnesium is 2.0 with the mol ratio of nickel。Respectively by separated for above two powder in same reactor, argon purge reactor burner hearth 3 times evacuation is utilized to remove air, being warming up to 550 DEG C after passing into hydrogen, under 2.0MPa hydrogen pressure, heat-insulation pressure keeping is cooled to 300 DEG C after 5 hours, at such a temperature heat-insulation pressure keeping natural cooling after 1 hour。The X ray diffracting spectrum of product is shown in Fig. 1, it has been found that with magnesium base alloy hydride Mg except C peak2NiH4For principal phase, contain a certain amount of non-hydride phase MgNi simultaneously2。
Embodiment 2
With magnesium powder for evaporation source, carry nano nickel (load nickel amount is for 10wt.%) powder for depositing base with multi-walled carbon nano-tubes。Wherein magnesium is 5.0 with the mol ratio of nickel。Respectively by separated to evaporation source and depositing base in reactor, argon purge reactor burner hearth 2 times evacuation is utilized to remove air, 600 DEG C it are warming up to after passing into hydrogen, under 0.1MPa hydrogen pressure, heat-insulation pressure keeping is cooled to 340 DEG C after 15 minutes, at such a temperature heat-insulation pressure keeping natural cooling after 15 minutes。The X ray diffracting spectrum of product is shown in Fig. 2, it has been found that mostly be magnesium-based hydride phase Mg except C peak2NiH4And MgH2, contain a small amount of MgO phase simultaneously。
Embodiment 3
With magnesium powder for evaporation source, carry nano nickel (load nickel amount is for 20wt.%) powder for depositing base with multi-walled carbon nano-tubes。Wherein magnesium is 4.0 with the mol ratio of nickel。Respectively by separated to evaporation source and depositing base in reactor, argon purge reactor burner hearth 3 times evacuation is utilized to remove air, 580 DEG C it are warming up to after passing into hydrogen, under 1.0MPa hydrogen pressure, heat-insulation pressure keeping is cooled to 360 DEG C after 10 hours, at such a temperature heat-insulation pressure keeping natural cooling after 4 hours。The X ray diffracting spectrum of product is shown in Fig. 3, with magnesium base alloy hydride Mg except C peak in sample2NiH4For principal phase, contain a small amount of MgH simultaneously2With MgO phase。
Embodiment 4
With magnesium powder for evaporation source, carry nano nickel (load nickel amount is for 40wt.%) powder for depositing base with multi-walled carbon nano-tubes。Wherein magnesium is 5.0 with the mol ratio of nickel。Respectively by separated to evaporation source and depositing base in reactor, argon purge reactor burner hearth 3 times evacuation is utilized to remove air, being warming up to 600 DEG C after passing into hydrogen, under 0.5MPa hydrogen pressure, heat-insulation pressure keeping is cooled to 340 DEG C after 2 hours, at such a temperature heat-insulation pressure keeping natural cooling after 1 hour。The X ray diffracting spectrum of product is shown in Fig. 4, with magnesium base alloy hydride Mg except C peak in sample2NiH4For principal phase, contain a small amount of MgH simultaneously2With MgO phase。
Embodiment 5
With magnesium powder for evaporation source, carry nano nickel (load nickel amount is for 20wt.%) powder for depositing base with multi-walled carbon nano-tubes。Wherein magnesium is 4.0 with the mol ratio of nickel。Respectively by separated to evaporation source and depositing base in reactor, argon purge reactor burner hearth 3 times evacuation is utilized to remove air, being warming up to 580 DEG C after passing into hydrogen, under 0.5MPa hydrogen pressure, heat-insulation pressure keeping is cooled to 340 DEG C after 5 hours, at such a temperature heat-insulation pressure keeping natural cooling after 2 hours。The X ray diffracting spectrum of product is shown in Fig. 5, with magnesium base alloy hydride Mg except C peak in sample2NiH4And Mg2NiH0.3For principal phase, contain a small amount of MgH simultaneously2With MgO phase。
Embodiment 6
With magnesium powder for evaporation source, carry nano nickel (load nickel amount is for 20wt.%) powder for depositing base with multi-walled carbon nano-tubes。Wherein magnesium is 3.0 with the mol ratio of nickel。Respectively by separated to evaporation source and depositing base in reactor, argon purge reactor burner hearth 3 times evacuation is utilized to remove air, 580 DEG C it are warming up to after passing into hydrogen, under 1.0MPa hydrogen pressure, heat-insulation pressure keeping is cooled to 340 DEG C after 10 hours, at such a temperature heat-insulation pressure keeping natural cooling after 2 hours。The X ray diffracting spectrum of product is shown in Fig. 6, with magnesium base alloy hydride Mg except C peak in sample2NiH4And Mg2NiH0.3For principal phase。
Claims (5)
1. the preparation technology of a nano Mg base hydrogen bearing alloy hydride, it is characterized in that with magnesium powder for evaporation source, nano nickel powder is carried for depositing base with multi-walled carbon nano-tubes, and both are separately placed in same reactor, passing into noble gas evacuation, heat up and pressurize after then passing to hydrogen, evaporation source is by gas-migration to the concurrent intercrescence aurification of depositing base and hydrogenation, cooling, finally gives highly active nano Mg base hydrogen bearing alloy hydride。
2. preparation technology according to claim 1, it is characterised in that: the described load nickel quality in multi-walled carbon nano-tubes load nano nickel powder is 10-40%。
3. preparation technology according to claim 1, it is characterised in that: it is warmed up to 550-600 DEG C after passing into hydrogen, heat-insulation pressure keeping 15 minutes to 10 hours；Described cooling is first to be cooled to 300-360 DEG C, heat-insulation pressure keeping 15 minutes to 4 hours, and last natural cooling obtains nano Mg base hydrogen bearing alloy hydride。
4. preparation technology according to claim 1, it is characterised in that: pressurize hydrogen pressure is 0.1-2.0MPa。
5. preparation technology according to claim 1, it is characterised in that: it is 2.0-5.0 that raw material magnesium powder and multi-walled carbon nano-tubes carry the mol ratio of magnesium and nickel in nano nickel powder。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637932A (en) * | 2016-11-15 | 2017-05-10 | 复旦大学 | Method for preparing hydrogen storage material, i.e., magnesium-nickel (Mg-Ni) alloy nanofiber |
| CN108118227A (en) * | 2017-11-09 | 2018-06-05 | 广德宝达精密电路有限公司 | Nano-magnesium-based hydrogen storage material for high-energy solid battery and preparation method thereof |
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| CN101767773A (en) * | 2010-01-21 | 2010-07-07 | 上海交通大学 | Polynary nanometer hydride particle preparation method based on metal gas phase and reaction vessel thereof |
| CN101896420A (en) * | 2007-12-11 | 2010-11-24 | 日产自动车株式会社 | Hydrogen storage material, production method of the hydrogen storage material, hydrogen supply system, fuel cell, internal combustion engine and vehicle |
| US9133025B2 (en) * | 2009-08-07 | 2015-09-15 | Ilika Technologies Limited | Hydrogen storage materials |
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- 2016-01-14 CN CN201610025351.7A patent/CN105692553B/en active Active
Patent Citations (4)
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| CN1557703A (en) * | 2004-02-05 | 2004-12-29 | 武汉理工大学 | Fullerene hydrogen storage material etched by microwave plasma and modified by hydrogen storage metal or alloy |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637932A (en) * | 2016-11-15 | 2017-05-10 | 复旦大学 | Method for preparing hydrogen storage material, i.e., magnesium-nickel (Mg-Ni) alloy nanofiber |
| CN108118227A (en) * | 2017-11-09 | 2018-06-05 | 广德宝达精密电路有限公司 | Nano-magnesium-based hydrogen storage material for high-energy solid battery and preparation method thereof |
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