CN108220728A - A kind of high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material and preparation method - Google Patents
A kind of high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material and preparation method Download PDFInfo
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- CN108220728A CN108220728A CN201711435962.XA CN201711435962A CN108220728A CN 108220728 A CN108220728 A CN 108220728A CN 201711435962 A CN201711435962 A CN 201711435962A CN 108220728 A CN108220728 A CN 108220728A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- 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
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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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- 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
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- 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
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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
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a kind of high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material and preparation methods.The hydrogen storage material includes rare earth magnesium-aluminum-based hydrogen-storage alloy and graphen catalyst GR, wherein, rare earth magnesium-aluminum-based hydrogen-storage alloy is formed with below formula:ReaMg100‑a‑b‑cAlbNic, wherein Re is rare-earth elements of lanthanum, one kind in cerium, praseodymium, neodymium, the atomic percent of a, b, c for corresponding element, 5≤a≤20,5≤b≤40,0≤c≤10,10≤b+c≤40;The graphen catalyst GR ratios that content meter accounts for final hydrogen storage material by mass percentage are:1%≤GR≤10%.The present invention uses rich reserves in nature, cheap Mg, Al as main component, while adds variety classes and the rare earth element of content in alloy A sides, and different content Ni elements are added in B sides, and adds graphene and carry out ball milling.It is low to have the characteristics that suction hydrogen discharging rate is fast, hydrogen storage capability is high, platform lags small and hydrogen discharging temperature by the hydrogen storage material that this method is prepared.
Description
Technical field
The invention belongs to hydrogen storage material technical field, more particularly to a kind of high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based
Hydrogen storage material and preparation method.
Background technology
At present, China's energy and environmental system face huge challenge, and automobile is as consumption of petroleum and CO2 emission
Rich and influential family, need fundamentally to be changed.Chinese environmental protection portion and american energy foundation data are shown:China continuous 8 years
As the first big country of motor vehicle production and marketing of the world, Chinese motor vehicle need to consume national oil total output 85% every year.Motor-vehicle tail-gas
Pollution has become the important sources of China's air pollution.Therefore, the novel traffic means of transport of development clean energy resource driving, is me
State's reduction consumption of petroleum, which eases up, solves the necessary behave of environmental pollution.At present, the main Types of new-energy automobile have pure electric automobile,
Hybrid vehicle and hydrogen cell automobile.Wherein, pure electric vehicle and plug-in hybrid-power automobile occupation rate of market are higher.But
Its lithium ion or lead-acid accumulator for carrying can still cause environment seriously to pollute.Also, existing Vehicular accumulator cell energy storage is close
Degree is also than relatively low, it is difficult to meet market demands.And hydrogen cell automobile discharge product only has water, can realize truly
Zero pollutant discharge.Hydrogen fuel cell generating efficiency is up to 60%, it is meant that it is with better economy and course continuation mileage.
Therefore, hydrogen cell automobile is the ultimate scheme of following human society transport facility.
Compared to the fast development of pure electric vehicle and hybrid vehicle, hydrogen cell automobile does not have commercial applications also
Condition.This is mainly due to lack safe and efficient storage hydrogen methods.At present, vehicle-mounted hydrogen storage system mainly have high-pressure gaseous storage hydrogen,
Low temperature liquid stores hydrogen and solid-state three kinds of hydrogen of storage.Wherein, high-pressure gaseous storage hydrogen, low temperature liquid hydrogen storage technology are in the side such as safety, cost
Face can not meet user's requirement.Another solid-state storage hydrogen mode with practical prospect is to store hydrogen using metal hydride.This
The principle of kind method is depressed in certain temperature and hydrogen, and hydrogen-storage alloy can largely inhale hydrogen, and hydrogen is stored in alloy crystalline substance in the form of atom
In born of the same parents, and form stable hydride.When temperature increases, the hydrogen being stored in structure cell passes through the processes such as diffusion, phase transformation and chemical combination
It is discharged again again.The reaction process of this method is controllable, make its product can Reusability, it is safe.It is but real at present
The hydrogen-storage alloy of existing marketization application, such as LaNi5Type hydrogen-storage alloy, theoretical hydrogen storage amount only have 1.36wt.%, can not meet vehicle
Carry requirement of the storage hydrogen system to energy storage density.Therefore, it is mesh to develop a kind of high power capacity, lightweight, safe, inexpensive hydrogen-storage alloy
The hot spot of preceding research.
At present, high capacity hydrogen storage alloy most study is magnesium series hydrogen storage alloy, and the quality hydrogen-storage density of pure magnesium is up to
7.6wt.%, and density is smaller, it is of low cost.But it inhales that put hydrogen condition harsher, and thermodynamic stability is high, and hydride is not easy point
Solution, is not easy to realize quick charge and discharge hydrogen.
Invention content
It is an object of the present invention to provide a kind of high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage materials, lead to
The improvement of alloying component is crossed, hydrogen storage material is made to have quick charge and discharge Hydrogen Energy power, reduces and inhales hydrogen discharging temperature, hydrogen storage property obtains greatly
Amplitude improves, and increased alloy element Al rich reserves, cheap.
It is a further object of the present invention to provide the systems of above-mentioned high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material
Preparation Method.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, the hydrogen storage material are store including rare earth magnesium-aluminum-based
Hydrogen alloy and graphen catalyst GR, wherein:Rare earth magnesium-aluminum-based hydrogen-storage alloy is formed with below formula:ReaMg100-a-b- cAlbNic, wherein Re is rare-earth elements of lanthanum, one kind in cerium, praseodymium, neodymium, the atomic percent of a, b, c for corresponding element, 5≤a≤
20,5≤b≤40,0≤c≤10,10≤b+c≤40;Content meter accounts for final storage hydrogen material to graphen catalyst GR by mass percentage
The ratio of material is:1%≤GR≤10%.
The hydrogen storage material is made by the steps:Weighing-melting-fast quenching-airflow milling-ball milling.
The graphene is the ball milling catalyst added in ball milling step.
The optimal ingredient of the hydrogen storage material is:A=10, b=10, c=5;The mass percent of graphen catalyst GR accounts for
The ratio of final hydrogen storage material is 5%.
A kind of preparation method of high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, the preparation method are included such as
Lower step:
A. dispensing:The raw material as needed for weighing the chemical formula composition of rare earth magnesium-aluminum-based hydrogen-storage alloy;
B. melting:Load weighted raw material is placed in induction melting furnace, the melting under vacuum and/or protective atmosphere, then
Cast obtains alloy of ingot;
C. fast quenching:Obtained alloy of ingot is placed in quartz ampoule of the bottom with slit, vacuumizes rear sensing heating extremely
Fusing, then with high-purity helium by molten alloy from quartz ampoule slit spray, be continuously injected in high-speed rotating water-cooled copper roller it
On, obtain quenched alloy thin slice;
D. airflow milling:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber, by superonic flow nozzzle by nitrogen
Jet-impingement makes alloy sheet mutually clash crushing, then filter out required alloy powder through grading wheel to pulverizing chamber;
E. ball milling:Stainless steel ball is packed into after the alloy powder filtered out is mixed with 1-10wt.% graphen catalysts GR
Grinding jar ball milling is filled with high-purity argon gas as protection gas, and Ball-milling Time is 10 ± 1h, and ratio of grinding media to material is 15~20:1, rotating speed for 350 ±
50 revs/min.
In the step a, the mass percent of magnesium metal and rare earth increases by 8% and 5% on the basis of stoichiometric respectively
Scaling loss amount.
The step b is:Load weighted raw material is placed in medium frequency induction melting furnace;Vacuum in stove is evacuated to 10-5~10-3It injects 0.04 ± 0.005MPa helium after Pa to be protected, after 30 ± 5min of preheated crucible, power is adjusted to 5~20kW, until closing
Gold is completely melt;10 ± 2min is kept the temperature, by molten state alloy casting to the water cooled copper mould for growing 8 ± 2cm, 3 ± 2cm of diameter, is obtained
Obtain alloy of ingot.
The step c is:Obtained alloy of ingot is placed in quartz ampoule of the bottom with slit, is evacuated to 10-5~
10-3Pa;Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected on the high-speed rotating water-cooled copper rollers of 45 ± 5m/s, to obtain quenched alloy thin slice.
In the step e, using the ball milling pattern of 1.5~0.5hh of ball milling, the 1.5~0.5h that rests.
The beneficial effects of the present invention are:
The present invention, by adding another lightweight element aluminium in magnesium metal, significantly reduces magnesium hydride in terms of ingredient
Hydrogen discharging temperature and enthalpy change.In order to further improve its hydrogen storage property, the present invention adds not on the basis of magnesium alloy in A sides
With the rare earth element of type and content, addition Ni elements in B sides make hydrogen storage material have quick charge and discharge Hydrogen Energy power, reduce to inhale and put hydrogen
Temperature, hydrogen storage property are significantly improved.
The preparation method of the present invention obtains alloy cast ingot by vacuum induction melting, again with one after fast quenching and mechanical crushing
Graphene catalytic rare earth magnesium-aluminum-based hydrogen storage material is made in the graphene mixing and ball milling of certainty ratio, so as to be hydrogen cell automobile system
The standby hydrogen-storage alloy with practical value.
The present invention uses rich reserves in nature, cheap Mg, Al as main component in composition design,
Variety classes and the rare earth element of content are added in alloy A sides simultaneously, different content Ni elements are added, and pass through vacuum in B sides
Induction melting obtains alloy cast ingot, and required material is made with a certain proportion of graphene mixing and ball milling again after fast quenching and mechanical crushing
Material.By the synergistic effect of same A, B side element of catalyst, under the premise of hydrogen storage material high power capacity is kept, reach raising suction and put
Hydroformylation reaction rate reduces hydrogen discharging temperature, improves the purpose of comprehensive hydrogen storage property.The mentioned component material being prepared by the technique
Material, which has, inhales the characteristics of hydrogen discharging rate is fast, and hydrogen storage capability is high, the small and hydrogen discharging temperature of platform lag is low, suitable for vehicle-mounted storage hydrogen system
System or hydrogenation stations.
Description of the drawings
Fig. 1 is 10 hydrogen storage material Nd of embodiment10Mg75Al10Ni5Inhale the TEM figures after hydrogen;
Fig. 2 is the XRD diagram of 1 hydrogen storage material of embodiment 1-11 and comparative example;
Fig. 3 is 10 hydrogen storage material Nd of embodiment10Mg75Al10Ni5The SEM figures of as cast condition;
Fig. 4 is 10 hydrogen storage material Nd of embodiment10Mg75Al10Ni5The SEM figures of powder.
Specific embodiment
With reference to the accompanying drawings and examples, the specific embodiment of the present invention is described in further detail.
The present invention provides a kind of high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, materials chemistry formula composition
It is as follows:ReaMg100-a-b-cAlbNic+ x wt.%GR, Re is one kind in rare-earth elements of lanthanum, cerium, praseodymium, neodymium in formula, and GR is graphite
Alkene catalyst, a, b, c are atomic ratio, and x is mass ratio, and 5≤a≤20,5≤b≤40,0≤c≤10,10≤b+c≤40,1≤
x≤10。
The optimal chemical formula composed atom ratio of material is:A=10, b=10, c=5;The content x=of graphen catalyst
5。
A kind of preparation method of high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, through the following steps that real
Existing:
A. the raw material as needed for weighing hydrogen storage material chemical formula composition.Wherein, magnesium metal and rare earth are respectively in stoichiometric
On the basis of increase 8wt.% and 5wt.% scaling loss amount;
B. load weighted raw material is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10-30.04MPa is injected after Pa
Helium is protected, and after preheated crucible 30min, power is adjusted to 5-20 kW, until alloy is completely melt.10min is kept the temperature, it will be molten
Melt state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, obtain alloy of ingot;
C. the cast alloy ingot being prepared is placed in quartz ampoule of the bottom with slit, is evacuated to 10-3Pa.Pass through
Alloy in pipe heat induction coil until fusing, then passes to the high-purity helium of certain pressure by it from quartz ampoule slit
It sprays, is continuously injected on the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is ejected by powder by superonic flow nozzzle
Broken room makes alloy sheet mutually clash crushing.Required alloy powder is filtered out through grading wheel again;
E. the alloy powder filtered out mixes with 1-10wt.% graphen catalysts (amounting to 5g) and is packed into stainless steel jar mill
Ball milling is filled with high-purity argon gas as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern of rest 0.5h
Ball milling, ratio of grinding media to material 20:1, rotating speed is 350 revs/min.
Embodiment 1
Chemical formula is prepared as La5Mg85Al10High power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
The ratio that content calculation by mass percentage accounts for final hydrogen storage material is 5%.Preparation method step is as follows:
A. it weighs:La is formed by chemical formula5Mg85Al10Raw material needed for weighing.Weigh the rare earth that purity is all higher than 99.5%
Lanthanum ingot 452g, metal magnesium ingot 1380g and metal aluminium ingot 168g.Wherein, magnesium metal and lanthanum increase on the basis of stoichiometric respectively
Add 8% and 5% scaling loss amount;
B. melting:Load weighted raw material (amounting to 2kg) is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10- 3It injects 0.04MPa helium after Pa to be protected, after preheated crucible 30min, power is adjusted to 5~20kW, until alloy is completely molten
Change.10min is kept the temperature, by molten state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, acquisition alloy of ingot;
C. fast quenching:The cast alloy ingot that 1kg is prepared is placed in quartz ampoule of the bottom with slit, is evacuated to
10-3Pa.Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected in the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. it crushes:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
Pulverizing chamber is mapped to, alloy sheet is made mutually to clash crushing.Required alloy powder is filtered out through grading wheel again;
E. ball milling:The alloy powder filtered out is mixed with graphen catalyst GR is packed into stainless steel jar mill ball milling, is filled with
High-purity argon gas is as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern ball milling of rest 0.5h, ball material
Than being 20:1, rotating speed is 350 revs/min.Wherein, graphen catalyst GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material was 5% (amounting to 5g).
Structural characterization and performance test are carried out to the hydrogen storage material of above-mentioned preparation.Phase group is observed using X-ray diffraction (XRD)
Into as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet testers test material, 1 the results are shown in Table.
Embodiment 2
Chemical formula is prepared as Ce5Mg85Al10High power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
The ratio that content calculation by mass percentage accounts for final hydrogen storage material is 5%.Preparation method step is as follows:
A. it weighs:Ce is formed by chemical formula5Mg85Al10Raw material needed for weighing.Weigh the rare earth that purity is all higher than 99.5%
Cerium ingot 455g, metal magnesium ingot 1380g and metal aluminium ingot 165g.Wherein, magnesium metal and cerium increase on the basis of stoichiometric respectively
Add 8% and 5% scaling loss amount;
B. melting:Load weighted raw material (amounting to 2kg) is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10- 3It injects 0.04MPa helium after Pa to be protected, after preheated crucible 30min, power is adjusted to 5~20kW, until alloy is completely molten
Change.10min is kept the temperature, by molten state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, acquisition alloy of ingot;
C. fast quenching:The cast alloy ingot that 1kg is prepared is placed in quartz ampoule of the bottom with slit, is evacuated to
10-3Pa.Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected in the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. it crushes:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
Pulverizing chamber is mapped to, alloy sheet is made mutually to clash crushing.Required alloy powder is filtered out through grading wheel again;
E. ball milling:The alloy powder filtered out is mixed with graphen catalyst GR is packed into stainless steel jar mill ball milling, is filled with
High-purity argon gas is as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern ball milling of rest 0.5h, ball material
Than being 20:1, rotating speed is 350 revs/min.Wherein, graphen catalyst GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material was 5% (amounting to 5g).
Structural characterization and performance test are carried out to the hydrogen storage material of above-mentioned preparation.Phase group is observed using X-ray diffraction (XRD)
Into as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet testers test material, 1 the results are shown in Table.
Embodiment 3
Chemical formula is prepared as Pr5Mg85Al10High power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
The ratio that content calculation by mass percentage accounts for final hydrogen storage material is 5%.Preparation method step is as follows:
A. it weighs:Pr is formed by chemical formula5Mg85Al10Raw material needed for weighing.Weigh the rare earth that purity is all higher than 99.5%
Praseodymium ingot 459g, metal magnesium ingot 1380g and metal aluminium ingot 161g.Wherein, magnesium metal and praseodymium increase on the basis of stoichiometric respectively
Add 8% and 5% scaling loss amount;
B. melting:Load weighted raw material (amounting to 2kg) is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10- 3It injects 0.04MPa helium after Pa to be protected, after preheated crucible 30min, power is adjusted to 5~20kW, until alloy is completely molten
Change.10min is kept the temperature, by molten state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, acquisition alloy of ingot;
C. fast quenching:The cast alloy ingot that 1kg is prepared is placed in quartz ampoule of the bottom with slit, is evacuated to
10-3Pa.Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected in the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. it crushes:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
Pulverizing chamber is mapped to, alloy sheet is made mutually to clash crushing.Required alloy powder is filtered out through grading wheel again;
E. ball milling:The alloy powder filtered out is mixed with graphen catalyst GR is packed into stainless steel jar mill ball milling, is filled with
High-purity argon gas is as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern ball milling of rest 0.5h, ball material
Than being 20:1, rotating speed is 350 revs/min.Wherein, graphen catalyst GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material was 5% (amounting to 5g).
Structural characterization and performance test are carried out to the hydrogen storage material of above-mentioned preparation.Phase group is observed using X-ray diffraction (XRD)
Into as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet testers test material, 1 the results are shown in Table.
Embodiment 4
Chemical formula is prepared as Nd5Mg90Al5High power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
The ratio that content calculation by mass percentage accounts for final hydrogen storage material is 5%.Preparation method step is as follows:
A. it weighs:Nd is formed by chemical formula5Mg85Al1Raw material needed for weighing.Weigh the rare earth that purity is all higher than 99.5%
Neodymium ingot 465g, metal magnesium ingot 1452g and metal aluminium ingot 83g.Wherein, magnesium metal and neodymium increase on the basis of stoichiometric respectively
8% and 5% scaling loss amount;
B. melting:Load weighted raw material (amounting to 2kg) is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10- 3It injects 0.04MPa helium after Pa to be protected, after preheated crucible 30min, power is adjusted to 5~20kW, until alloy is completely molten
Change.10min is kept the temperature, by molten state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, acquisition alloy of ingot;
C. fast quenching:The cast alloy ingot that 1kg is prepared is placed in quartz ampoule of the bottom with slit, is evacuated to
10-3Pa.Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected in the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. it crushes:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
Pulverizing chamber is mapped to, alloy sheet is made mutually to clash crushing.Required alloy powder is filtered out through grading wheel again;
E. ball milling:The alloy powder filtered out is mixed with graphen catalyst GR is packed into stainless steel jar mill ball milling, is filled with
High-purity argon gas is as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern ball milling of rest 0.5h, ball material
Than being 20:1, rotating speed is 350 revs/min.Wherein, graphen catalyst GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material was 5% (amounting to 5g).
Structural characterization and performance test are carried out to the hydrogen storage material of above-mentioned preparation.Phase group is observed using X-ray diffraction (XRD)
Into as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet testers test material, 1 the results are shown in Table.
Embodiment 5
Chemical formula is prepared as Nd5Mg55Al40High power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
The ratio that content calculation by mass percentage accounts for final hydrogen storage material is 5%.Preparation method step is as follows:
A. it weighs:Nd is formed by chemical formula5Mg55Al40Raw material needed for weighing.Weigh the rare earth that purity is all higher than 99.5%
Neodymium ingot 462g, metal magnesium ingot 880g and metal aluminium ingot 658g.Wherein, magnesium metal and neodymium increase on the basis of stoichiometric respectively
8% and 5% scaling loss amount;
B. melting:Load weighted raw material (amounting to 2kg) is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10- 3It injects 0.04MPa helium after Pa to be protected, after preheated crucible 30min, power is adjusted to 5~20kW, until alloy is completely molten
Change.10min is kept the temperature, by molten state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, acquisition alloy of ingot;
C. fast quenching:The cast alloy ingot that 1kg is prepared is placed in quartz ampoule of the bottom with slit, is evacuated to
10-3Pa.Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected in the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. it crushes:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
Pulverizing chamber is mapped to, alloy sheet is made mutually to clash crushing.Required alloy powder is filtered out through grading wheel again;
E. ball milling:The alloy powder filtered out is mixed with graphen catalyst GR is packed into stainless steel jar mill ball milling, is filled with
High-purity argon gas is as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern ball milling of rest 0.5h, ball material
Than being 20:1, rotating speed is 350 revs/min.Wherein, graphen catalyst GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material was 5% (amounting to 5g).
Structural characterization and performance test are carried out to the hydrogen storage material of above-mentioned preparation.Phase group is observed using X-ray diffraction (XRD)
Into as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet testers test material, 1 the results are shown in Table.
Embodiment 6
Chemical formula is prepared as Nd5Mg85Al10High power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
The ratio that content calculation by mass percentage accounts for final hydrogen storage material is 5%.Preparation method step is as follows:
A. it weighs:Nd is formed by chemical formula5Mg85Al10Raw material needed for weighing.Weigh the rare earth that purity is all higher than 99.5%
Neodymium ingot 464g, metal magnesium ingot 1368g and metal aluminium ingot 168g.Wherein, magnesium metal and neodymium increase on the basis of stoichiometric respectively
Add 8% and 5% scaling loss amount;
B. melting:Load weighted raw material (amounting to 2kg) is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10- 3It injects 0.04MPa helium after Pa to be protected, after preheated crucible 30min, power is adjusted to 5~20kW, until alloy is completely molten
Change.10min is kept the temperature, by molten state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, acquisition alloy of ingot;
C. fast quenching:The cast alloy ingot that 1kg is prepared is placed in quartz ampoule of the bottom with slit, is evacuated to
10-3Pa.Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected in the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. it crushes:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
Pulverizing chamber is mapped to, alloy sheet is made mutually to clash crushing.Required alloy powder is filtered out through grading wheel again;
E. ball milling:The alloy powder filtered out is mixed with graphen catalyst GR is packed into stainless steel jar mill ball milling, is filled with
High-purity argon gas is as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern ball milling of rest 0.5h, ball material
Than being 20:1, rotating speed is 350 revs/min.Wherein, graphen catalyst GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material was 5% (amounting to 5g).
Structural characterization and performance test are carried out to the hydrogen storage material of above-mentioned preparation.Phase group is observed using X-ray diffraction (XRD)
Into as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet testers test material, 1 the results are shown in Table.
Embodiment 7
Chemical formula is prepared as Nd10Mg80Al10High power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
The ratio that content calculation by mass percentage accounts for final hydrogen storage material is 5%.Preparation method step is as follows:
A. it weighs:Nd is formed by chemical formula10Mg80Al10Raw material needed for weighing.Weigh purity be all higher than 99.5% it is dilute
Native neodymium ingot 756g, metal magnesium ingot 1080g and metal aluminium ingot 140g.Wherein, magnesium metal and neodymium are respectively on the basis of stoichiometric
Increase by 8% and 5% scaling loss amount;
B. melting:Load weighted raw material (amounting to 2kg) is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10- 3It injects 0.04MPa helium after Pa to be protected, after preheated crucible 30min, power is adjusted to 5~20kW, until alloy is completely molten
Change.10min is kept the temperature, by molten state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, acquisition alloy of ingot;
C. fast quenching:The cast alloy ingot that 1kg is prepared is placed in quartz ampoule of the bottom with slit, is evacuated to
10-3Pa.Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected in the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. it crushes:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
Pulverizing chamber is mapped to, alloy sheet is made mutually to clash crushing.Required alloy powder is filtered out through grading wheel again;
E. ball milling:The alloy powder filtered out is mixed with graphen catalyst GR is packed into stainless steel jar mill ball milling, is filled with
High-purity argon gas is as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern ball milling of rest 0.5h, ball material
Than being 20:1, rotating speed is 350 revs/min.Wherein, graphen catalyst GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material was 5% (amounting to 5g).
Structural characterization and performance test are carried out to the hydrogen storage material of above-mentioned preparation.Phase group is observed using X-ray diffraction (XRD)
Into as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet testers test material, 1 the results are shown in Table.
Embodiment 8
Chemical formula is prepared as Nd15Mg75Al10High power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
The ratio that content calculation by mass percentage accounts for final hydrogen storage material is 5%.Preparation method step is as follows:
A. it weighs:Nd is formed by chemical formula15Mg75Al10Raw material needed for weighing.Weigh purity be all higher than 99.5% it is dilute
Native neodymium ingot 1008g, metal magnesium ingot 872g and metal aluminium ingot 120g.Wherein, magnesium metal and neodymium are respectively on the basis of stoichiometric
Increase by 8% and 5% scaling loss amount;
B. melting:Load weighted raw material (amounting to 2kg) is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10- 3It injects 0.04MPa helium after Pa to be protected, after preheated crucible 30min, power is adjusted to 5~20kW, until alloy is completely molten
Change.10min is kept the temperature, by molten state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, acquisition alloy of ingot;
C. fast quenching:The cast alloy ingot that 1kg is prepared is placed in quartz ampoule of the bottom with slit, is evacuated to
10-3Pa.Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected in the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. it crushes:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
Pulverizing chamber is mapped to, alloy sheet is made mutually to clash crushing.Required alloy powder is filtered out through grading wheel again;
E. ball milling:The alloy powder filtered out is mixed with graphen catalyst GR is packed into stainless steel jar mill ball milling, is filled with
High-purity argon gas is as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern ball milling of rest 0.5h, ball material
Than being 20:1, rotating speed is 350 revs/min.Wherein, graphen catalyst GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material was 5% (amounting to 5g).
Structural characterization and performance test are carried out to the hydrogen storage material of above-mentioned preparation.Phase group is observed using X-ray diffraction (XRD)
Into as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet testers test material, 1 the results are shown in Table.
Embodiment 9
Chemical formula is prepared as Nd20Mg70Al10High power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
The ratio that content calculation by mass percentage accounts for final hydrogen storage material is 5%.Preparation method step is as follows:
A. it weighs:Nd is formed by chemical formula20Mg70Al10Raw material needed for weighing.Weigh purity be all higher than 99.5% it is dilute
Native neodymium ingot 1180g, metal magnesium ingot 716g and metal aluminium ingot 104g.Wherein, magnesium metal and neodymium are respectively on the basis of stoichiometric
Increase by 8% and 5% scaling loss amount;
B. melting:Load weighted raw material (amounting to 2kg) is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10- 3It injects 0.04MPa helium after Pa to be protected, after preheated crucible 30min, power is adjusted to 5~20kW, until alloy is completely molten
Change.10min is kept the temperature, by molten state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, acquisition alloy of ingot;
C. fast quenching:The cast alloy ingot that 1kg is prepared is placed in quartz ampoule of the bottom with slit, is evacuated to
10-3Pa.Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected in the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. it crushes:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
Pulverizing chamber is mapped to, alloy sheet is made mutually to clash crushing.Required alloy powder is filtered out through grading wheel again;
E. ball milling:The alloy powder filtered out is mixed with graphen catalyst GR is packed into stainless steel jar mill ball milling, is filled with
High-purity argon gas is as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern ball milling of rest 0.5h, ball material
Than being 20:1, rotating speed is 350 revs/min.Wherein, graphen catalyst GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material was 5% (amounting to 5g).
Structural characterization and performance test are carried out to the hydrogen storage material of above-mentioned preparation.Phase group is observed using X-ray diffraction (XRD)
Into as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet testers test material, 1 the results are shown in Table.
Embodiment 10
Chemical formula is prepared as Nd10Mg75Al10Ni5High power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material,
The ratio that middle GR content calculations by mass percentage account for final hydrogen storage material is 5%.Preparation method step is as follows:
A. it weighs:Nd is formed by chemical formula10Mg75Al10Ni5Raw material needed for weighing.It weighs purity and is all higher than 99.5%
Rare earth neodymium ingot 748g, metal magnesium ingot 972g, metal aluminium ingot 136g and electrolytic nickel sheet 144g.Wherein, magnesium metal and neodymium exist respectively
Increase by 8% and 5% scaling loss amount on the basis of stoichiometric;
B. melting:Load weighted raw material (amounting to 2kg) is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10- 3It injects 0.04MPa helium after Pa to be protected, after preheated crucible 30min, power is adjusted to 5~20kW, until alloy is completely molten
Change.10min is kept the temperature, by molten state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, acquisition alloy of ingot;
C. fast quenching:The cast alloy ingot that 1kg is prepared is placed in quartz ampoule of the bottom with slit, is evacuated to
10-3Pa.Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected in the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. it crushes:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
Pulverizing chamber is mapped to, alloy sheet is made mutually to clash crushing.Required alloy powder is filtered out through grading wheel again;
E. ball milling:The alloy powder filtered out is mixed with graphen catalyst GR is packed into stainless steel jar mill ball milling, is filled with
High-purity argon gas is as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern ball milling of rest 0.5h, ball material
Than being 20:1, rotating speed is 350 revs/min.Wherein, graphen catalyst GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material was 5% (amounting to 5g).
Structural characterization and performance test are carried out to the hydrogen storage material of above-mentioned preparation.Phase group is observed using X-ray diffraction (XRD)
Into as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet testers test material, 1 the results are shown in Table.
Hydrogen storage material Nd is observed using transmission electron microscope (TEM)10Mg75Al10Ni5Inhale the microstructure after hydrogen, knot
Fruit sees Fig. 1.Storage hydrogen material Nd is observed using scanning electron microscope (SEM)10Mg75Al10Ni5Cast alloy ingot casting cross-sectional view
As (backscattered electron phase), 3 are as a result seen.Nd is observed using scanning electron microscope (SEM)10Mg75Al10Ni5Alloying pellet phase
As a result looks are shown in Fig. 4.
Embodiment 11
Chemical formula is prepared as Nd10Mg70Al10Ni10High power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material,
The ratio that middle GR content calculations by mass percentage account for final hydrogen storage material is 5%.Preparation method step is as follows:
A. it weighs:Nd is formed by chemical formula10Mg70Al10Ni10Raw material needed for weighing.It weighs purity and is all higher than 99.5%
Rare earth neodymium ingot 720g, metal magnesium ingot 872g, metal aluminium ingot 128g and electrolytic nickel sheet 280g.Wherein, magnesium metal and neodymium exist respectively
Increase by 8% and 5% scaling loss amount on the basis of stoichiometric;;
B. melting:Load weighted raw material (amounting to 2kg) is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10- 3It injects 0.04MPa helium after Pa to be protected, after preheated crucible 30min, power is adjusted to 5~20kW, until alloy is completely molten
Change.10min is kept the temperature, by molten state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, acquisition alloy of ingot;
C. fast quenching:The cast alloy ingot that 1kg is prepared is placed in quartz ampoule of the bottom with slit, is evacuated to
10-3Pa.Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected in the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. it crushes:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
Pulverizing chamber is mapped to, alloy sheet is made mutually to clash crushing.Required alloy powder is filtered out through grading wheel again;
E. ball milling:The alloy powder filtered out is mixed with graphen catalyst GR is packed into stainless steel jar mill ball milling, is filled with
High-purity argon gas is as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern ball milling of rest 0.5h, ball material
Than being 20:1, rotating speed is 350 revs/min.Wherein, graphen catalyst GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material was 5% (amounting to 5g).
Structural characterization and performance test are carried out to the hydrogen storage material of above-mentioned preparation.Phase group is observed using X-ray diffraction (XRD)
Into as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet testers test material, 1 the results are shown in Table.
Comparative example 1
Chemical formula is prepared as Mg90Al10Hydrogen storage material, wherein GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material is 5%.Preparation method step is as follows:
A. it weighs:Mg is formed by chemical formula90Al10Raw material needed for weighing.Weigh the magnesium ingot that purity is all higher than 99.5%
1780g and metal aluminium ingot 220g.Wherein, magnesium metal increases by 8% scaling loss amount on the basis of stoichiometric;
B. melting:Load weighted raw material (amounting to 2kg) is placed in medium frequency induction melting furnace.Vacuum in stove is evacuated to 10- 3It injects 0.04MPa helium after Pa to be protected, after preheated crucible 30min, power is adjusted to 5~20kW, until alloy is completely molten
Change.10min is kept the temperature, by molten state alloy casting to long 8cm, in the water cooled copper mould of diameter 3cm, acquisition alloy of ingot;
C. fast quenching:The cast alloy ingot that 1kg is prepared is placed in quartz ampoule of the bottom with slit, is evacuated to
10-3Pa.Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by its from
Quartz ampoule slit sprays, and is continuously injected in the high-speed rotating water-cooled copper rollers of 45m/s, to obtain quenched alloy thin slice;
D. it crushes:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
Pulverizing chamber is mapped to, alloy sheet is made mutually to clash crushing.Required alloy powder is filtered out through grading wheel again;
E. ball milling:The alloy powder filtered out is mixed with graphen catalyst GR is packed into stainless steel jar mill ball milling, is filled with
High-purity argon gas is as protection gas.Ball-milling Time is set as 10h, using ball milling 0.5h, the ball milling pattern ball milling of rest 0.5h, ball material
Than being 20:1, rotating speed is 350 revs/min.Wherein, graphen catalyst GR content calculations by mass percentage account for final storage hydrogen material
The ratio of material was 5% (amounting to 5g).
Structural characterization and performance test are carried out to the hydrogen storage material of above-mentioned preparation.Phase group is observed using X-ray diffraction (XRD)
Into as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet testers test material, 1 the results are shown in Table.
1 embodiment of table and comparative example hydrogen storage material gaseous state hydrogen storage property
Claims (9)
1. a kind of high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, it is characterised in that:
The hydrogen storage material includes rare earth magnesium-aluminum-based hydrogen-storage alloy and graphen catalyst GR, wherein:Rare earth magnesium-aluminum-based hydrogen-storage alloy
It is formed with below formula:ReaMg100-a-b-cAlbNic, wherein Re is rare-earth elements of lanthanum, one kind in cerium, praseodymium, neodymium, a, b, c
For the atomic percent of corresponding element, 5≤a≤20,5≤b≤40,0≤c≤10,10≤b+c≤40;Graphen catalyst GR
The ratio that content meter accounts for final hydrogen storage material by mass percentage is:1%≤GR≤10%.
2. hydrogen storage material according to claim 1, it is characterised in that:
The hydrogen storage material is made by the steps:Weighing-melting-fast quenching-airflow milling-ball milling.
3. hydrogen storage material according to claim 1, it is characterised in that:
The graphene is the ball milling catalyst added in ball milling step.
4. hydrogen storage material according to claim 1, it is characterised in that:
The optimal ingredient of the hydrogen storage material is:A=10, b=10, c=5;The mass percent of graphen catalyst GR accounts for finally
The ratio of hydrogen storage material is 5%.
5. a kind of preparation side of high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material as described in claim 1
Method, it is characterised in that:The preparation method includes the following steps:
A. dispensing:The raw material as needed for weighing the chemical formula composition of rare earth magnesium-aluminum-based hydrogen-storage alloy;
B. melting:Load weighted raw material is placed in induction melting furnace, then the melting under vacuum and/or protective atmosphere is poured into a mould
Obtain alloy of ingot;
C. fast quenching:Obtained alloy of ingot is placed in quartz ampoule of the bottom with slit, rear sensing heating is vacuumized and extremely melts,
Then molten alloy from quartz ampoule slit is sprayed with high-purity helium, is continuously injected on high-speed rotating water-cooled copper roller, obtains
To quenched alloy thin slice;
D. airflow milling:Obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber, by superonic flow nozzzle by stream of nitrogen gas
Pulverizing chamber is ejected into, alloy sheet is made mutually to clash crushing, then filter out required alloy powder through grading wheel;
E. ball milling:Stainless steel jar mill is packed into after the alloy powder filtered out is mixed with 1-10wt.% graphen catalysts GR
Ball milling is filled with high-purity argon gas as protection gas, and Ball-milling Time is 10 ± 1h, and ratio of grinding media to material is 15~20:1, rotating speed is 350 ± 50
Rev/min.
6. preparation method as claimed in claim 5, it is characterised in that:
In the step a, the mass percent of magnesium metal and rare earth, respectively on the basis of stoichiometric increase by 8% and 5% burning
Damage amount.
7. preparation method as claimed in claim 5, it is characterised in that:
The step b is:Load weighted raw material is placed in medium frequency induction melting furnace;Vacuum in stove is evacuated to 10-5~10-3After Pa
Injection 0.04 ± 0.005MPa helium is protected, and after 30 ± 5min of preheated crucible, power is adjusted to 5~20kW, until alloy is complete
Running down;10 ± 2min is kept the temperature, by molten state alloy casting to the water cooled copper mould for growing 8 ± 2cm, 3 ± 2cm of diameter, is cast
Ingot alloy.
8. preparation method as claimed in claim 5, it is characterised in that:
The step c is:Obtained alloy of ingot is placed in quartz ampoule of the bottom with slit, is evacuated to 10-5~10- 3Pa;Alloy in pipe heat by induction coil until fusing, then pass to the high-purity helium of certain pressure by it from stone
English pipe slit sprays, and is continuously injected on the high-speed rotating water-cooled copper rollers of 45 ± 5m/s, to obtain quenched alloy thin slice.
9. preparation method as claimed in claim 5, it is characterised in that:In the step e, using ball milling 1.5~0.5h h, stop
Cease the ball milling pattern of 1.5~0.5h.
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CN108715962A (en) * | 2018-07-04 | 2018-10-30 | 南通志乐新材料有限公司 | A kind of rear-earth-doped Mg base hydrogenous alloys |
CN111515380A (en) * | 2020-05-11 | 2020-08-11 | 安泰科技股份有限公司 | High-capacity magnesium-based composite hydrogen storage material and preparation method thereof |
CN111515380B (en) * | 2020-05-11 | 2022-04-29 | 安泰科技股份有限公司 | High-capacity magnesium-based composite hydrogen storage material and preparation method thereof |
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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