CN106637932A - Method for preparing hydrogen storage material, i.e., magnesium-nickel (Mg-Ni) alloy nanofiber - Google Patents
Method for preparing hydrogen storage material, i.e., magnesium-nickel (Mg-Ni) alloy nanofiber Download PDFInfo
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- CN106637932A CN106637932A CN201611004228.3A CN201611004228A CN106637932A CN 106637932 A CN106637932 A CN 106637932A CN 201611004228 A CN201611004228 A CN 201611004228A CN 106637932 A CN106637932 A CN 106637932A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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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
- 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
- C01B3/0031—Intermetallic compounds; Metal alloys; Treatment thereof
- C01B3/0042—Intermetallic compounds; Metal alloys; Treatment thereof only containing magnesium and nickel; Treatment thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- 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
Abstract
The invention belongs to the technical field of preparation of hydrogen storage materials, and in particular relates to a method for preparing a hydrogen storage material, i.e., magnesium-nickel (Mg-Ni) alloy nanofiber. The method comprises the steps of synthesizing bamboo-like Ni nanofiber as an Ni source by changing the calcination conditions of an electrospinning method for preparing Ni(NO3)2/ polyvinyl pyrrolidone (PVP) fiber, evaporating Mg onto the surface of the Ni nanofiber by using a high-temperature thermal evaporation method and carrying out in-situ reaction to obtain the Mg-Ni alloy nanofiber. The total hydrogen storage capacity of the Mg-Ni alloy nanofiber synthesized by the method is 2.25wt%, and the Mg-Ni alloy nanofiber can absorb 1.31wt% of hydrogen at the temperature of 100 DE G C within 100min; after hydrogen absorption is finished, the Mg-Ni alloy nanofiber can rapidly release 1.5wt% of the hydrogen at the temperature of 265 DE G C within 1min, and the total hydrogen desorption capacity is 2.13wt%; therefore, the Mg-Ni alloy nanofiber has higher hydrogen absorption and desorption dynamics performance.
Description
Technical field
The invention belongs to hydrogen storage technical field of material, and in particular to prepare hydrogen storage material magnesium-nickel alloy Nanowire
The method of dimension.
Background technology
The swift and violent of human economy has been got in a large amount of consumption of non-renewable fossil energy, going from bad to worse for environment for human survival in return
Development, the energy is the important source that the mankind depend on for existence, produce and live, in order to meet demand of the whole world to clean energy resource, solution
Certainly increasingly serious energy crisis, finds the strategic objective that suitable fungible energy source is various countries.[1] In various fungible energy sources
In, because of its rich reserves, burning capacity density value is high, combustion product for Hydrogen Energy（Water）A series of advantages such as cleanliness without any pollution become most
Preferable secondary energy sources.How safely and efficiently to store Hydrogen Energy is the applicable bottleneck problem of current hydrogen.[2,3]With hydrogen economy
Development, many hydrogen storage materials are continuously developed, such as alloy, light metal hydride, CNT etc..Magnesium-base hydrogen storage material is with it
Abundant deposit, cheap price, and capacity are high, receive much concern the features such as good reversibility, but it also has high suction
Hydrogen discharging temperature and slow dynamics the two mainly apply obstacle, MgH2With high thermodynamic stability, decompose enthalpy change
Up to 74.6 KJ/ (molH2).Often more than 350 DEG C, which has limited its reality in terms of hydrogen storage should for hydrogen discharging temperature
With, and by the way that MgH can be changed with the alloying such as Ni, Cu, Al2Decomposition path-ways, reduce its thermodynamic stability such that it is able to
Significantly improve MgH2Thermodynamic property, Ni as a kind of metal cheap and easy to get, its bianry alloy product Mg with Mg2Ni has
There are of a relatively high theoretical hydrogen content (3.6 wt.%) and Rapid reversible to inhale to put the performance of hydrogen and be subject to widely studied.But close at present
Into Mg2There are a variety of deficiencies in the method for Ni.Such as conventional eutectic method is due to the low melting point of Mg, high volatile and MgNi metals
Between high different melting points be restricted and be difficult to prepare highly purified Mg2Ni alloys.[4-6]There are some researches show that the method for mechanical ball mill can
To synthesize Mg2Ni。[7-10]But time-consuming for this method, and final product homogeneity and purity can be subject to rotational speed of ball-mill, ratio of grinding media to material,
The impact of many factors such as Ball-milling Time.Additionally, long Ball-milling Time easily aoxidizes sample.Ask to solve this
Topic, Sun seminars propose two-step method synthesis Mg2Ni.First by after Mg powder and the simple min of ball milling 20 of Ni powder again at 500 DEG C, Ar
Solid state reaction kinetics Mg is carried out under atmosphere2Ni。[11]But this method step is relatively complicated.Later Li et al. adopted H plasma methods
Synthesis Mg, Ni nano particles, then in 4 MPa hydrogen pressures, under the conditions of 350 DEG C, using Mg, Ni nano particles are synthesized
Mg2NiH4, then pure Mg is just obtained Jing after follow-up dehydrogenation2Ni。[12,13]But this method has introduced H plasma apparatus, can only answer at present
For laboratory synthesis, be not suitable for industrialized mass production.Initiative utilization high temperature thermal evaporation of the invention is evaporated to Mg
Ni nanofiber surfaces carry out reaction in-situ and prepare Mg-Ni nanofibers.
Bibliography:
【1】. Schmitz, B., Virtual Reality: On the Brink of Greatness [J].
Computer Aided Engineering, Vol. 12, No. 4, 1993, pp.26~32.
【2】. Jayaram, S., Connacher, H.I., and Lyons, K.W., Virtual Assembly
Using Virtual Reality Techniques [J]. Computer Aided Design, Vol. 29, No. 8,
1997, pp. 575~584.
【3】. Jung, B., Hoffhenke, M., and Wachsmuth, I., Virtual Assembly With
Construction Kits [M]. Proceedings of 1997 ASME Design Engineering Technical
Conference, September 14-17, 1997, Sacramento, DETC97/DFM-4363.
【4】. Hsu C-W, Lee S-L, Jeng R-R, Lin J-C. Mass production of Mg2Ni alloy
bulk by isothermal evaporation casting process [J]. Int J Hydrogen Energy,
2007,32:4907-4911.
【5】. Sun D, Enoki H, Gingl F, Akiba E. New approach for synthesizing Mg-
based alloys [J]. J Alloys Compd., 1999, 285:279-283.
【6】. Knight Jr L, Brittain R, Duncan M, Joyner C. Unusual behavior of
vaporaized magnesium under low pressure conditions [J]. J Phys Chem., 1975,
79: 1183-1190.
【7】. Ebrahimi-Purkani A, Kashani-Bozorg SF, Nanocrystalline Mg2Ni-based
powders produced by high-energy ball milling and subsequent annealing [J]. J
Alloys Compd., 2008,456:211-215.
【8】. Simicic MV, Zdujic M, Dimitrijevic R, Nikolic-Bujanovic L, Popovic
NH. Hydrogen absorption and elecdtrochemical properties of Mg2Ni-type alloys
synthesized by mechanical alloying [J]. J Power Sources, 2006, 158: 730-734.
【9】. Zaluski L, Zaluska A, Stromolsen JO. Hydrogen absorption in
nanocrystalling Mg2Ni formed by mechanical alloying [J]. J Alloys Compd.,
1995, 217: 245-249.
【10】. Lee HY, Goo NH, Jeong WT, Lee KS. The surface state of
nanocrystalline and amorphous Mg2Ni alloys prepared by mechanical alloying
[J]. J Alloys Compd., 2000, 313: 258-262.
【11】. Zhao B, Fang F, Sun D, Zhang Q, Wei S, Cao F, er al. Formation of
Mg2Ni with enhanced kinetics: Using MgH2 instead of Mg as a starting material
[J]. J Solid State Chem., 2012, 192: 210-214.
【12】. Shao H, Liu T, Li X. Preparation of the Mg2Ni compound from
ultrafine particles and its hydrogen storage properties [J]. Nanotechnology,
2003,14: L1-L3.
【13】. Shao HY, Liu T, Wang YT, Xu HR, Li XG. Preparation of Mg-based
hydrogen storage materials from metal nanoparticles [J]. J Alloys Compd.,
2008, 456: 527-533.。
The content of the invention
It is an object of the present invention to provide a kind of process is simple prepares magnesium nickel（Mg-Ni）The method of alloy nano fiber.
The method for preparing magnesium-nickel alloy nanofiber that the present invention is provided, by changing method of electrostatic spinning Ni (NO are prepared3)2/
The calcination condition of PVP fibers, synthesizes the Ni nanofibers of Bamboo-shaped as Ni sources, and Mg is evaporated to into Ni using high temperature thermal evaporation
Nanofiber surface carries out reaction in-situ, prepares Mg-Ni nanofibers.Concretely comprise the following steps：
（1）Synthesize the Ni nanofibers of Bamboo-shaped with method of electrostatic spinning：
Will be dissolved with Ni (NO3)2Ni (NO are prepared with the DMF/ ethanol solutions of PVP with method of electrostatic spinning3)2/ PVP fibers, then,
By Ni (NO in tube furnace3)2/ PVP fibers are sintered in atmosphere NiO fibers, finally in H2/N2It is under mixing gas shielded that NiO is fine
Dimension is reduced to Ni fibers；
（2）Mg powder is evaporated to into Ni nanofiber surfaces with thermal evaporation：
The porcelain boat that will be equipped with Ni fibers is placed in the big porcelain boat for being paved with Mg powder, sealing, then under protective gas Ar, uses tube furnace
It is calcined, Mg powder is steamed to Ni nanofiber surfaces, and reaction in-situ is carried out with Ni, generate Mg-Ni nanofibers.
Step of the present invention（1）In, the calcining Ni (NO3)2The condition of/PVP fibers is：With 1 ~ 5 DEG C/min ramps
To 190 ~ 220 DEG C, 1 ~ 3 h is incubated；Then proceed to this ramp to 500 ~ 550 DEG C, 2 ~ 4 h are incubated at this temperature；
The condition of the reduction NiO fibers is：H2/N2Under the protection of gaseous mixture, with 1 ~ 5 DEG C/min ramps to 380-420 DEG C,
2 ~ 4 h are incubated at a temperature of this, room temperature is cooled to after terminating.
Step of the present invention（2）In, the calcination condition is：With 1 ~ 5 DEG C/min ramps to 500-550 DEG C, immediately
Again from this temperature with 2-3 DEG C/min ramps to 600 ~ 650 DEG C, in 2 ~ 3h of this temperature, be subsequently cooled to room temperature.
Mg-Ni alloy nano fibers synthesized by the present invention, are piled up by many nanocrystals and are formed, and fiber size is in 80-
200 nm.
Mg-Ni alloy nano fibers synthesized by the present invention are preferable hydrogen storage materials in, and in hydrogen 30 bar are pressed, 100
It is the hydrogen of adsorbable 1.31 wt.% in 100 min at DEG C；At 235 DEG C, hydrogen-sucking amount can just reach 1 wt.% in 1 min, always
Hydrogen storage capability be 2.25 wt.%；After sucking hydrogen, at 265 DEG C, the hydrogen of 1.5 wt.% can be quickly released in 1 min, always
Hydrogen desorption capacity is 2.13 wt.%.
The present invention has the following aspects remarkable advantage：
（1）Using Mg-Ni alloy nanos fiber as hydrogen source material, a large amount of High Purity Hydrogens can be obtained under relatively low heating-up temperature
Gas；
（2）Preparation equipment is simple, it is easy to accomplish；
（3）Process is simple, synthesis is convenient, moderate cost.
Description of the drawings
The NiO nanofibers of Fig. 1 method of electrostatic spinning synthesis（NiO NFs）, the Ni fibers after reduction（Ni NFs）, Mg-Ni
Alloy nano fiber（Mg-Ni NFs）XRD.
Fig. 2 is NiO nanofibers, Ni nanofibers, the relevant picture of Mg-Ni alloy nano fibers.Wherein, a is quiet
The TEM photos of NiO nanofibers prepared by electrical spinning method；B is the TEM photos of the Ni nanofibers of Bamboo-shaped；C is Mg-Ni conjunctions
The TEM photos of gold nano fiber；D is the HRTEM photos of Mg-Ni alloy nano fibers；E is single TEM photos, and f is unit in e
Plain Ni spectrograms, g is the element M g spectrogram in e.
Fig. 3 Mg-Ni alloy nano fiber pyrolytic energy spectrum diagrams.Wherein, black line, is adding for Mg-Ni alloy nano fibers
The mass spectrogram of hydrogen product；Red line is the mass spectrogram of the hydrogenation products of Mg-Ni powder samples.
Fig. 4 products are inhaled and put the XRD spectra after hydrogen, wherein, a is that Mg-Ni alloy nanos fiber inhales the product after hydrogen；B is
Mg-Ni alloy nano fibers put the product after hydrogen.
Suction hydrogen curve under Fig. 5 Mg-Ni alloy fiber condition of different temperatures（On）.
Hydrogen desorption isotherms under Fig. 6 Mg-Ni alloy fiber condition of different temperatures（Under）.
Specific embodiment
The present invention is further illustrated below by embodiment.
Embodiment 1：
The preparation of 1.Ni nanofibers：It is divided into three steps.First, the DMF and ethanol of 1.25 ml are measured, is well mixed.Then exist
In the organic solvent of mixing, the PVP of 0.17 g, stirring a few minutes dissolving is added to add the Ni of 0.101g（NO3）2·6H2O,
Continue to stir the green solution for obtaining clarifying after 5 h, for electrostatic spinning.Parameter setting：The KV of voltage 12, spinning head is away from reception
The cm of plate 15, flow rate of liquid be 0.25 ml/h, spinning at ambient temperature.Second step, by the Ni received on negative plate（NO3）2/
PVP forerunner's fiber is calcined obtain NiO fibers in atmosphere.Calcination procedure is 1 DEG C/min to 190 DEG C, and 2 h are follow-up of continuing rising for insulation
Temperature is incubated 3 h to 500 DEG C.3rd step, reduces NiO fibers, at 400 DEG C, H2/N22 h are incubated under the protection of gaseous mixture, can be with
NiO is set to be reduced into Ni fibers.
It is prepared by 2.Mg-Ni alloy nanos fiber：The mg of Ni lines 25 is weighed in little porcelain boat A, porcelain boat A is placed in into bottom paving
Inside full Mg powder (400 mg) porcelain boat B greatly, porcelain boat cover seal is covered.Porcelain boat B is moved in quartz ampoule, tube furnace is placed in and is added
Heat, leads to protective gas Ar.Heat treatment process is：First 5 DEG C/min to 500 DEG C, then with 2 DEG C/min to 650 DEG C of 2 h of insulation,
After be cooled to room temperature.As a comparison, weigh equivalent Ni powder and synthesize Mg by the same way2Ni powder samples.
3.Mg-Ni nanofiber hydrogenation processes：In weighing 20 mg samples and autoclave, the hydrogen pressure of 30 bar is added,
Room temperature is cooled to after being incubated 5 h at 300 DEG C.By the same way the Mg-Ni powder samples to synthesizing carry out hydroprocessing conduct
Contrast test.The XRD of product as shown in figure 1, synthetic product morphology characterization as shown in Fig. 2 Fig. 3 be Mg-Ni nanofibers and
The thermal decomposition performance collection of illustrative plates of its comparative sample, and Mg-Ni nanofibers inhale hydrogen and put the product analysis after hydrogen as shown in figure 4, most
Afterwards, the hydrogen storage property of Mg-Ni nanofibers is as seen in figs. 5-6.
Embodiment 2：
The preparation of 1.Ni nanofibers：It is divided into three steps.First, the DMF and ethanol of 2.5 ml are measured, is well mixed.Then exist
In the organic solvent of mixing, the PVP of 0.34g, stirring a few minutes dissolving is added to add the Ni of 0.202g（NO3）2·6H2O, after
The green solution clarified is obtained after 5 h of continuous stirring, for electrostatic spinning.Parameter setting：The KV of voltage 12, spinning head is away from receiver board
15 cm, flow rate of liquid be 0.25 ml/h, spinning at ambient temperature.Second step, by the Ni received on negative plate（NO3）2/PVP
Forerunner's fiber is calcined obtain NiO fibers in atmosphere.Calcination procedure is 3 DEG C/min to 220 DEG C, is continued with this after 2 h of insulation
Ramp is incubated 3 h to 550 DEG C.3rd step, reduces NiO fibers, in H2/N2Under the protection of gaseous mixture, with 5 DEG C/min liters
To 400 DEG C, 3 h are incubated at 400 DEG C, NiO can be made to be reduced into Ni fibers.
It is prepared by 2.Mg-Ni alloy nanos fiber：The mg of Ni lines 25 is weighed in little porcelain boat A, porcelain boat A is placed in into bottom paving
Inside full Mg powder (400 mg) porcelain boat B greatly, porcelain boat cover seal is covered.Porcelain boat B is moved in quartz ampoule, tube furnace is placed in and is added
Heat, leads to protective gas Ar.Heat treatment process is：First 5 DEG C/min to 500 DEG C, then with 2 DEG C/min to 600 DEG C of 3 h of insulation,
After be cooled to room temperature.As a comparison, weigh equivalent Ni powder and synthesize Mg by the same way2Ni powder samples.
3.Mg-Ni nanofiber hydrogenation processes：In weighing 20 mg samples and autoclave, the hydrogen pressure of 30 bar is added,
Room temperature is cooled to after being incubated 5 h at 300 DEG C.By the same way the Mg-Ni powder samples to synthesizing carry out hydroprocessing conduct
Contrast test.
Claims (3)
1. a kind of method for preparing hydrogen storage material magnesium-nickel alloy nanofiber, it is characterised in that by changing electrostatic spinning legal system
Standby Ni (NO3)2The calcination condition of/PVP fibers, synthesizes the Ni nanofibers of Bamboo-shaped as Ni sources, will using high temperature thermal evaporation
Mg is evaporated to Ni nanofiber surfaces and carries out reaction in-situ, prepares Mg-Ni nanofibers；Concretely comprise the following steps：
（1）Synthesize the Ni nanofibers of Bamboo-shaped with method of electrostatic spinning：
Will be dissolved with Ni (NO3)2Ni (NO are prepared with the DMF/ ethanol solutions of PVP with method of electrostatic spinning3)2/ PVP fibers, then, in pipe
By Ni (NO in formula stove3)2/ PVP fibers are sintered in atmosphere NiO fibers, finally in H2/N2By NiO fibers under mixing gas shielded
It is reduced to Ni fibers；
（2）Mg powder is evaporated to into Ni nanofiber surfaces with thermal evaporation：
The porcelain boat that will be equipped with Ni fibers is placed in the big porcelain boat for being paved with Mg powder, sealing, then under protective gas Ar, uses tube furnace
It is calcined, Mg powder is steamed to Ni nanofiber surfaces, and reaction in-situ is carried out with Ni, generate Mg-Ni nanofibers；
Step（1）Described in calcine Ni (NO3)2The condition of/PVP fibers is：With 1 ~ 5 DEG C/min ramps to 190 ~ 220
DEG C, it is incubated 1 ~ 3 h；Then proceed to this ramp to 500 ~ 550 DEG C, 2 ~ 4 h are incubated at this temperature；The reduction NiO
The condition of fiber is：H2/N2Under the protection of gaseous mixture, with 1 ~ 5 DEG C/min ramps to 380-420 DEG C, protect at this temperature
2 ~ 4 h of temperature, are cooled to room temperature after terminating.
2. method according to claim 1, it is characterised in that step（2）The calcination condition is：With 1 ~ 5 DEG C/min
Ramp to 500-550 DEG C, immediately again from this temperature with 2-3 DEG C/min ramps to 600 ~ 650 DEG C, in this temperature
2 ~ 3h of insulation, is subsequently cooled to room temperature.
3. method according to claim 1, it is characterised in that synthesized Mg-Ni alloy nanos fiber is by many nanometers
Crystal grain is piled up and is formed, and fiber size is 80-200 nm.
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Cited By (3)
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| CN108941610A (en) * | 2018-09-19 | 2018-12-07 | 西京学院 | A method of hydrogen storage magnesium-nickel alloy nanometer powder is prepared based on polyol process |
| CN114411028A (en) * | 2022-01-21 | 2022-04-29 | 徐州工程学院 | Trace nickel composite layered magnesium composite material and preparation method and application thereof |
| CN114918421A (en) * | 2022-04-21 | 2022-08-19 | 北京航空航天大学 | Fiber space limited domain preparation method of ZrCo alloy and application thereof |
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| CN114918421A (en) * | 2022-04-21 | 2022-08-19 | 北京航空航天大学 | Fiber space limited domain preparation method of ZrCo alloy and application thereof |
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Application publication date: 20170510 |