CN108220728B - A kind of high capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material and preparation method - Google Patents
A kind of high capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material and preparation method Download PDFInfo
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Abstract
The present invention relates to a kind of high 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 following below formula: ReaMg100‑a‑b‑cAlbNic, wherein Re is one of rare-earth elements of lanthanum, cerium, praseodymium, neodymium, and a, b, c are the atomic percent of corresponding element, 5≤a≤20,5≤b≤40,0≤c≤10,10≤b+c≤40；Content meter accounts for the ratio of final hydrogen storage material to graphen catalyst GR by mass percentage are as follows: 1%≤GR≤10%.The present invention uses rich reserves in nature, cheap Mg, Al for main component, while in the rare earth element of the side alloy A addition variety classes and content, adding different content Ni element in the side B, and add 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, in particular to a kind of high capacity light graphite alkene catalytic rare earth magnesium-aluminum-based
Hydrogen storage material and preparation method.
Background technique
Currently, China's energy and environmental system face huge challenge, 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, the world, Chinese motor vehicle need to consume national petroleum 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 for developing clean energy resource driving, is me
State reduces the necessary behave of the gentle solution environmental pollution of consumption of petroleum.Currently, 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
It spends also relatively low, it is difficult to meet market demands.And hydrogen cell automobile discharge product only has water, can be realized 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 the 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.Currently, vehicle-mounted hydrogen storage system mainly have high-pressure gaseous storage hydrogen,
Low temperature liquid stores hydrogen and solid-state stores three kinds of hydrogen.Wherein, high-pressure gaseous storage hydrogen, low temperature liquid hydrogen storage technology are in the side such as safety, cost
Face is unable to satisfy 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 highly-safe.But it is 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.%, are unable to satisfy vehicle
Carry requirement of the storage hydrogen system to energy storage density.Therefore, developing a kind of high capacity, lightweight, safe, inexpensive hydrogen-storage alloy is mesh
The hot spot of preceding research.
Currently, high capacity hydrogen storage alloy most study is magnesium series hydrogen storage alloy, the quality hydrogen-storage density of pure magnesium is up to
7.6wt.%, and density is smaller, it is low in cost.But it inhales that hydrogen release condition is harsher, and thermodynamic stability is high, and hydride is not easy point
Solution, is not easy to realize quick charge and discharge hydrogen.
Summary of the invention
It is an object of the present invention to provide a kind of high capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage materials, lead to
The improvement for crossing alloying component makes hydrogen storage material have quick charge and discharge Hydrogen Energy power, reduces and inhales hydrogen discharging temperature, and 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 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 capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, the hydrogen storage material include the storage of rare earth magnesium-aluminum-based
Hydrogen alloy and graphen catalyst GR, in which: rare earth magnesium-aluminum-based hydrogen-storage alloy is formed with following below formula: ReaMg100-a-b- cAlbNic, wherein Re be one of rare-earth elements of lanthanum, cerium, praseodymium, neodymium, a, b, c be corresponding element atomic percent, 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 are as follows: 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 being added in ball milling step.
The optimal ingredient of the hydrogen storage material are as follows: 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 capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, the preparation method include such as
Lower step:
A. ingredient: raw material needed for being weighed by 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
Casting obtains alloy of ingot；
C. fast quenching: obtained alloy of ingot is placed in bottom in the quartz ampoule of slit, vacuumizes rear induction 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: being placed in airflow milling pulverizing chamber for obtained quenched alloy thin slice, by superonic flow nozzzle by nitrogen
Jet-impingement makes alloy sheet mutually clash crushing to pulverizing chamber, then required alloy powder is filtered out through grading wheel；
E. ball milling: stainless steel ball is packed into after the alloy powder filtered out is mixed with 1-10wt.% graphen catalyst GR
Grinding jar ball milling, be filled with high-purity argon gas as protection gas, Ball-milling Time be 10 ± 1h, ratio of grinding media to material be 15~20:1, revolving speed be 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 are as follows: load weighted raw material is placed in medium frequency induction melting furnace；Vacuum in furnace 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 into the water cooled copper mould for growing 8 ± 2cm, 3 ± 2cm of diameter, is obtained
Obtain alloy of ingot.
The step c are as follows: obtained alloy of ingot is placed in bottom in the quartz ampoule of 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 in obtain quenched alloy thin slice on the high-speed rotating water-cooled copper roller of 45 ± 5m/s.
In the step e, using the ball milling mode of 1.5~0.5h 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 is added not on the basis of magnesium alloy in the side A
With the rare earth element of type and content, Ni element is added in the side B, and hydrogen storage material is made to have quick charge and discharge Hydrogen Energy power, reduces and inhales hydrogen release
Temperature, hydrogen storage property are significantly improved.
Preparation method of the 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, 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 for main component in terms of composition design,
Simultaneously in the rare earth element of the side alloy A addition variety classes and content, different content Ni element is added in the side B, and pass through vacuum
Induction melting obtains alloy cast ingot, material needed for being made again with a certain proportion of graphene mixing and ball milling after fast quenching and mechanical crushing
Material.By the synergistic effect of the same side A, B element of catalyst, under the premise of keeping hydrogen storage material high capacity, reaches 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 has suction hydrogen discharging rate fast, and hydrogen storage capability is high, platform lags small and low hydrogen discharging temperature feature, is suitable for vehicle-mounted storage hydrogen system
System or hydrogenation stations.
Detailed description of the invention
Fig. 1 is 10 hydrogen storage material Nd of embodiment10Mg75Al10Ni5TEM figure after inhaling 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 of as cast condition schemes；
Fig. 4 is 10 hydrogen storage material Nd of embodiment10Mg75Al10Ni5The SEM of powder schemes.
Specific embodiment
With reference to the accompanying drawings and examples, specific embodiments of the present invention will be described in further detail.
The present invention provides a kind of high 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 of 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 are as follows: a=10, b=10, c=5；The content x=of graphen catalyst
5。
A kind of preparation method of high capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, through the following steps that real
Existing:
A. raw material needed for being weighed by 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 furnace is evacuated to 10-30.04MPa is injected after Pa
Helium is protected, and after preheated crucible 30min, power is adjusted to 5-20kW, until alloy is completely melt.10min is kept the temperature, will be melted
State alloy casting is to long 8cm, in the water cooled copper mould of diameter 3cm, obtains alloy of ingot；
C. the cast alloy ingot being prepared is placed in bottom in the quartz ampoule of slit, is evacuated to 10-3Pa.Pass through
Induction coil heat to alloy in pipe until fusing, then passes to the high-purity helium of certain pressure for it from quartz ampoule slit
It sprays, is continuously injected in obtain quenched alloy thin slice on the high-speed rotating water-cooled copper roller of 45m/s；
D. obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is ejected into 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 is mixed with 1-10wt.% graphen catalyst (total 5g) 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 mode of rest 0.5h
Ball milling, ratio of grinding media to material 20:1, revolving speed are 350 revs/min.
Embodiment 1
Preparing chemical formula is La5Mg85Al10High capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
It is 5% that content, which calculates and accounts for the ratio of final hydrogen storage material, by mass percentage.Steps are as follows for preparation method:
A. it weighs: forming La by chemical formula5Mg85Al10Raw material needed for weighing.Weigh the rare earth that purity is all larger 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 (total 2kg) is placed in medium frequency induction melting furnace.Vacuum in furnace 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 bottom in the quartz ampoule of 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 obtain quenched alloy thin slice in the high-speed rotating water-cooled copper roller of 45m/s；
D. crush: obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
It is mapped to pulverizing chamber, 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 mode ball milling of rest 0.5h, ball material
Than for 20:1, revolving speed is 350 revs/min.Wherein, graphen catalyst GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5% (total 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)
At as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet tester test material, 1 the results are shown in Table.
Embodiment 2
Preparing chemical formula is Ce5Mg85Al10High capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
It is 5% that content, which calculates and accounts for the ratio of final hydrogen storage material, by mass percentage.Steps are as follows for preparation method:
A. it weighs: forming Ce by chemical formula5Mg85Al10Raw material needed for weighing.Weigh the rare earth that purity is all larger 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 (total 2kg) is placed in medium frequency induction melting furnace.Vacuum in furnace 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 bottom in the quartz ampoule of 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 obtain quenched alloy thin slice in the high-speed rotating water-cooled copper roller of 45m/s；
D. crush: obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
It is mapped to pulverizing chamber, 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 mode ball milling of rest 0.5h, ball material
Than for 20:1, revolving speed is 350 revs/min.Wherein, graphen catalyst GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5% (total 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)
At as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet tester test material, 1 the results are shown in Table.
Embodiment 3
Preparing chemical formula is Pr5Mg85Al10High capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
It is 5% that content, which calculates and accounts for the ratio of final hydrogen storage material, by mass percentage.Steps are as follows for preparation method:
A. it weighs: forming Pr by chemical formula5Mg85Al10Raw material needed for weighing.Weigh the rare earth that purity is all larger 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 (total 2kg) is placed in medium frequency induction melting furnace.Vacuum in furnace 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 bottom in the quartz ampoule of 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 obtain quenched alloy thin slice in the high-speed rotating water-cooled copper roller of 45m/s；
D. crush: obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
It is mapped to pulverizing chamber, 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 mode ball milling of rest 0.5h, ball material
Than for 20:1, revolving speed is 350 revs/min.Wherein, graphen catalyst GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5% (total 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)
At as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet tester test material, 1 the results are shown in Table.
Embodiment 4
Preparing chemical formula is Nd5Mg90Al5High capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
It is 5% that content, which calculates and accounts for the ratio of final hydrogen storage material, by mass percentage.Steps are as follows for preparation method:
A. it weighs: forming Nd by chemical formula5Mg85Al1Raw material needed for weighing.Weigh the rare earth that purity is all larger 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 (total 2kg) is placed in medium frequency induction melting furnace.Vacuum in furnace 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 bottom in the quartz ampoule of 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 obtain quenched alloy thin slice in the high-speed rotating water-cooled copper roller of 45m/s；
D. crush: obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
It is mapped to pulverizing chamber, 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 mode ball milling of rest 0.5h, ball material
Than for 20:1, revolving speed is 350 revs/min.Wherein, graphen catalyst GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5% (total 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)
At as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet tester test material, 1 the results are shown in Table.
Embodiment 5
Preparing chemical formula is Nd5Mg55Al40High capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
It is 5% that content, which calculates and accounts for the ratio of final hydrogen storage material, by mass percentage.Steps are as follows for preparation method:
A. it weighs: forming Nd by chemical formula5Mg55Al40Raw material needed for weighing.Weigh the rare earth that purity is all larger 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 (total 2kg) is placed in medium frequency induction melting furnace.Vacuum in furnace 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 bottom in the quartz ampoule of 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 obtain quenched alloy thin slice in the high-speed rotating water-cooled copper roller of 45m/s；
D. crush: obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
It is mapped to pulverizing chamber, 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 mode ball milling of rest 0.5h, ball material
Than for 20:1, revolving speed is 350 revs/min.Wherein, graphen catalyst GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5% (total 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)
At as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet tester test material, 1 the results are shown in Table.
Embodiment 6
Preparing chemical formula is Nd5Mg85Al10High capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
It is 5% that content, which calculates and accounts for the ratio of final hydrogen storage material, by mass percentage.Steps are as follows for preparation method:
A. it weighs: forming Nd by chemical formula5Mg85Al10Raw material needed for weighing.Weigh the rare earth that purity is all larger 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 (total 2kg) is placed in medium frequency induction melting furnace.Vacuum in furnace 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 bottom in the quartz ampoule of 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 obtain quenched alloy thin slice in the high-speed rotating water-cooled copper roller of 45m/s；
D. crush: obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
It is mapped to pulverizing chamber, 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 mode ball milling of rest 0.5h, ball material
Than for 20:1, revolving speed is 350 revs/min.Wherein, graphen catalyst GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5% (total 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)
At as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet tester test material, 1 the results are shown in Table.
Embodiment 7
Preparing chemical formula is Nd10Mg80Al10High capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
It is 5% that content, which calculates and accounts for the ratio of final hydrogen storage material, by mass percentage.Steps are as follows for preparation method:
A. it weighs: forming Nd by chemical formula10Mg80Al10Raw material needed for weighing.Weigh purity be all larger 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 (total 2kg) is placed in medium frequency induction melting furnace.Vacuum in furnace 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 bottom in the quartz ampoule of 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 obtain quenched alloy thin slice in the high-speed rotating water-cooled copper roller of 45m/s；
D. crush: obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
It is mapped to pulverizing chamber, 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 mode ball milling of rest 0.5h, ball material
Than for 20:1, revolving speed is 350 revs/min.Wherein, graphen catalyst GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5% (total 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)
At as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet tester test material, 1 the results are shown in Table.
Embodiment 8
Preparing chemical formula is Nd15Mg75Al10High capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
It is 5% that content, which calculates and accounts for the ratio of final hydrogen storage material, by mass percentage.Steps are as follows for preparation method:
A. it weighs: forming Nd by chemical formula15Mg75Al10Raw material needed for weighing.Weigh purity be all larger 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 (total 2kg) is placed in medium frequency induction melting furnace.Vacuum in furnace 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 bottom in the quartz ampoule of 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 obtain quenched alloy thin slice in the high-speed rotating water-cooled copper roller of 45m/s；
D. crush: obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
It is mapped to pulverizing chamber, 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 mode ball milling of rest 0.5h, ball material
Than for 20:1, revolving speed is 350 revs/min.Wherein, graphen catalyst GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5% (total 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)
At as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet tester test material, 1 the results are shown in Table.
Embodiment 9
Preparing chemical formula is Nd20Mg70Al10High capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material, wherein GR
It is 5% that content, which calculates and accounts for the ratio of final hydrogen storage material, by mass percentage.Steps are as follows for preparation method:
A. it weighs: forming Nd by chemical formula20Mg70Al10Raw material needed for weighing.Weigh purity be all larger 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 (total 2kg) is placed in medium frequency induction melting furnace.Vacuum in furnace 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 bottom in the quartz ampoule of 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 obtain quenched alloy thin slice in the high-speed rotating water-cooled copper roller of 45m/s；
D. crush: obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
It is mapped to pulverizing chamber, 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 mode ball milling of rest 0.5h, ball material
Than for 20:1, revolving speed is 350 revs/min.Wherein, graphen catalyst GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5% (total 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)
At as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet tester test material, 1 the results are shown in Table.
Embodiment 10
Preparing chemical formula is Nd10Mg75Al10Ni5High capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material,
The ratio that middle GR content calculating by mass percentage accounts for final hydrogen storage material is 5%.Steps are as follows for preparation method:
A. it weighs: forming Nd by chemical formula10Mg75Al10Ni5Raw material needed for weighing.It weighs purity and is all larger 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 (total 2kg) is placed in medium frequency induction melting furnace.Vacuum in furnace 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 bottom in the quartz ampoule of 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 obtain quenched alloy thin slice in the high-speed rotating water-cooled copper roller of 45m/s；
D. crush: obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
It is mapped to pulverizing chamber, 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 mode ball milling of rest 0.5h, ball material
Than for 20:1, revolving speed is 350 revs/min.Wherein, graphen catalyst GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5% (total 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)
At as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet tester test material, 1 the results are shown in Table.
Hydrogen storage material Nd is observed using transmission electron microscope (TEM)10Mg75Al10Ni5Microstructure after inhaling 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
Preparing chemical formula is Nd10Mg70Al10Ni10High capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material,
The ratio that middle GR content calculating by mass percentage accounts for final hydrogen storage material is 5%.Steps are as follows for preparation method:
A. it weighs: forming Nd by chemical formula10Mg70Al10Ni10Raw material needed for weighing.It weighs purity and is all larger 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 (total 2kg) is placed in medium frequency induction melting furnace.Vacuum in furnace 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 bottom in the quartz ampoule of 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 obtain quenched alloy thin slice in the high-speed rotating water-cooled copper roller of 45m/s；
D. crush: obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
It is mapped to pulverizing chamber, 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 mode ball milling of rest 0.5h, ball material
Than for 20:1, revolving speed is 350 revs/min.Wherein, graphen catalyst GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5% (total 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)
At as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet tester test material, 1 the results are shown in Table.
Comparative example 1
Preparing chemical formula is Mg90Al10Hydrogen storage material, wherein GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5%.Steps are as follows for preparation method:
A. it weighs: forming Mg by chemical formula90Al10Raw material needed for weighing.Weigh the magnesium ingot that purity is all larger 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 (total 2kg) is placed in medium frequency induction melting furnace.Vacuum in furnace 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 bottom in the quartz ampoule of 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 obtain quenched alloy thin slice in the high-speed rotating water-cooled copper roller of 45m/s；
D. crush: obtained quenched alloy thin slice is placed in airflow milling pulverizing chamber.Stream of nitrogen gas is sprayed by superonic flow nozzzle
It is mapped to pulverizing chamber, 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 mode ball milling of rest 0.5h, ball material
Than for 20:1, revolving speed is 350 revs/min.Wherein, graphen catalyst GR content calculating by mass percentage accounts for final storage hydrogen material
The ratio of material is 5% (total 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)
At as a result seeing Fig. 2.Using the gaseous state hydrogen storage property of semi-automatic Seviet tester 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 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, in which: rare earth magnesium-aluminum-based hydrogen-storage alloy
It is formed with following below formula: ReaMg100-a-b-cAlbNic, wherein Re is one of rare-earth elements of lanthanum, 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
Content meter accounts for the ratio of final hydrogen storage material by mass percentage are as follows: 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 being 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 are as follows: 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 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. ingredient: raw material needed for being weighed by 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
Obtain alloy of ingot；
C. fast quenching: being placed in bottom in the quartz ampoule of slit, vacuumizing rear induction heating to melting for obtained alloy of ingot,
Then molten alloy is sprayed with high-purity helium from quartz ampoule slit, is continuously injected on high-speed rotating water-cooled copper roller, obtains
To quenched alloy thin slice；
D. airflow milling: being placed in airflow milling pulverizing chamber for obtained quenched alloy thin slice, by superonic flow nozzzle by stream of nitrogen gas
It is ejected into pulverizing chamber, so that alloy sheet is mutually clashed 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 catalyst 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, and revolving 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 increases by 8% and 5% burning on the basis of stoichiometric respectively
Damage amount.
7. preparation method as claimed in claim 5, it is characterised in that:
The step b are as follows: load weighted raw material is placed in medium frequency induction melting furnace；Vacuum in furnace 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 into 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 are as follows: obtained alloy of ingot is placed in bottom in the quartz ampoule of slit, is evacuated to 10-5~10- 3Pa；Alloy in pipe heat by induction coil until fusing, then passes to the high-purity helium of certain pressure for it from stone
English pipe slit sprays, and is continuously injected in obtain quenched alloy thin slice on the high-speed rotating water-cooled copper roller of 45 ± 5m/s.
9. preparation method as claimed in claim 5, it is characterised in that: in the step e, using 1.5~0.5h of ball milling, rest
The ball milling mode of 1.5~0.5h.
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