CN117504918B - Modified catalyst and application thereof in modification of aluminum hydride hydrogen storage system - Google Patents
Modified catalyst and application thereof in modification of aluminum hydride hydrogen storage system Download PDFInfo
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- CN117504918B CN117504918B CN202410021829.3A CN202410021829A CN117504918B CN 117504918 B CN117504918 B CN 117504918B CN 202410021829 A CN202410021829 A CN 202410021829A CN 117504918 B CN117504918 B CN 117504918B
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000001257 hydrogen Substances 0.000 title claims abstract description 60
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 60
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000003860 storage Methods 0.000 title abstract description 20
- 239000003054 catalyst Substances 0.000 title abstract description 9
- 238000012986 modification Methods 0.000 title abstract description 6
- 230000004048 modification Effects 0.000 title abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 31
- 239000011232 storage material Substances 0.000 claims abstract description 29
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000012298 atmosphere Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims description 30
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 20
- 239000002105 nanoparticle Substances 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- XZWVIKHJBNXWAT-UHFFFAOYSA-N argon;azane Chemical compound N.[Ar] XZWVIKHJBNXWAT-UHFFFAOYSA-N 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical group [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000006356 dehydrogenation reaction Methods 0.000 abstract description 37
- 239000010936 titanium Substances 0.000 abstract description 11
- 239000000654 additive Substances 0.000 abstract description 6
- 230000000996 additive effect Effects 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000027756 respiratory electron transport chain Effects 0.000 abstract description 2
- 239000012300 argon atmosphere Substances 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- 229910052987 metal hydride Inorganic materials 0.000 description 4
- 150000004681 metal hydrides Chemical class 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 229910000091 aluminium hydride Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- RSHAOIXHUHAZPM-UHFFFAOYSA-N magnesium hydride Chemical compound [MgH2] RSHAOIXHUHAZPM-UHFFFAOYSA-N 0.000 description 1
- 229910012375 magnesium hydride Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- -1 specifically Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Hydrogen, Water And Hydrids (AREA)
Abstract
The invention discloses a modified catalyst and application thereof in modification of an aluminum hydride hydrogen storage system, and belongs to the technical field of hydrogen storage materials and preparation thereof. The invention solves the problems of excessive additive dosage and poor low-temperature dynamics in the existing aluminum hydride composite hydrogen storage system. Firstly, titanium dioxide is used as a precursor, and Ti in the titanium dioxide is enabled to be in a reducing atmosphere 4+ Is reduced to Ti 3+ Higher catalytic activity is obtained. Meanwhile, the Ti element has the multi-valence characteristic which is more favorable for electron transfer in the dehydrogenation reaction process, reduces the dehydrogenation temperature of the aluminum hydride material, and improves the dehydrogenation dynamics of the low-temperature region of the aluminum hydride material. In addition, the preparation process of the composite hydrogen storage material provided by the invention is simple and mature, and the raw materials are cheap and easy to obtain, so that the preparation process is convenient for large-scale industrial production.
Description
Technical Field
The invention relates to a modified catalyst and application thereof in modification of an aluminum hydride hydrogen storage system, and belongs to the technical field of hydrogen storage materials and preparation thereof.
Background
The hydrogen source is gradually applied to the portable hydrogen fuel cell system at present, and plays an important role in transportation, energy storage, national defense construction and the like. However, the safe and efficient storage and transportation of hydrogen is still a major problem to be solved in the development and utilization of hydrogen energy. In particular, a hydrogen storage material as a portable hydrogen source must combine a high hydrogen storage density, mild dehydrogenation conditions, and high safety. Solid light metal hydrides are currently considered to be one of the most desirable materials. The hydrogen product has high purity, can be dehydrogenated by heating under normal pressure, and is suitable for being used as a direct hydrogen source of a portable hydrogen fuel cell. However, how to optimize the light metal hydride to construct a novel composite hydrogen storage material which meets the requirements better, and further research is needed.
Aluminium hydride (AlH) 3 ) Is one of many light metal hydrides, but is associated with magnesium hydride (MgH 2 ) Compared with other light metal hydrides, the portable hydrogen storage tank has higher hydrogen storage capacity (10.1-wt%) and lower dehydrogenation temperature (140 ℃), and is suitable for being used as a portable hydrogen storage tank content material. However, in view of the energy consumption issues associated with operating temperature zones and heater configuration of fuel cells, aluminum hydride hydrogen storage systems are also required to further reduce their dehydrogenation temperatures and improve their low temperature zone dehydrogenation kinetics. In the prior art, the dehydrogenation kinetics of the low-temperature region of the aluminum hydride hydrogen storage system is improved by adding additives, however, the dosage of the additives is higher than 5. 5wt percent, the capacity of the aluminum hydride composite hydrogen storage material is directly reduced to 9.5 wt percent at the highest, and the advantage of the high capacity of the aluminum hydride material is greatly destroyed.
Disclosure of Invention
Aiming at the problems of excessive additive dosage, poor low-temperature dynamics and the like in the existing aluminum hydride composite hydrogen storage system, the invention provides a modified catalyst and an application method thereof in the modification of the aluminum hydride hydrogen storage system.
The technical scheme of the invention is as follows:
the invention aims to provide a preparation method of a modified catalyst, specifically, titanium dioxide is used as a precursor, and titanium nitride nano particles are obtained by calcining under an ammonia-argon mixed atmosphere.
Further defined, the ammonia-argon mixed atmosphere consists of ammonia gas and argon gas according to a volume ratio of 5:95.
Further defined, the ammonia argon mixture flow is 10L/min.
Further defined, the calcination conditions are: heating to 750 ℃ at a speed of 1-2 ℃/min, heating to 900 ℃ at a speed of 1-2 ℃/min, and preserving heat for 1h.
Further defined, the calcination conditions are: heating to 750 ℃ at a speed of 2 ℃/min, heating to 900 ℃ at a speed of 1 ℃/min, and preserving heat for 1h.
Further defined, the titanium dioxide is nano titanium dioxide.
The second object of the present invention is to provide a composite hydrogen storage material comprising aluminum hydride powder and the modified catalyst obtained by the above-mentioned preparation method.
Further limited, the composite hydrogen storage material shows good hydrogen release performance at 60 DEG C
The invention further provides a preparation method of the composite hydrogen storage material, which comprises the steps of mixing aluminum hydride powder with titanium nitride nano particles, and performing ball milling treatment in a protective atmosphere to obtain the composite hydrogen storage material.
Further defined, the titanium nitride nanoparticles are present in a ratio of 1 to 5wt%.
Further defined, the ball milling treatment conditions are: ball-material ratio is 50:1, rotation speed of ball mill is 350 rpm, single ball milling time is 15min, interval is 10min, and repeating for 4 times.
Further defined, the protective atmosphere is argon.
The beneficial effects are that:
(1) Firstly, titanium dioxide is used as a precursor, and Ti in the titanium dioxide is enabled to be in a reducing atmosphere 4+ Is reduced to Ti 3+ Higher catalytic activity is obtained. Meanwhile, the Ti element has the polyvalent state characteristic which is more favorable for electron transfer in the dehydrogenation reaction process, thereby reducing aluminum hydrideThe dehydrogenation temperature of the material also improves the dehydrogenation kinetics in the low temperature zone of the aluminum hydride material.
(2) The composite hydrogen storage material prepared by the invention has extremely high capacity, mainly because the prepared titanium nitride nano particles have high catalytic activity, thus the dosage of the additive can be obviously reduced. When the addition amount is 1 wt%, the initial dehydrogenation temperature of the composite material is lower than 60 ℃, the effective hydrogen storage capacity of the composite material reaches 8.02 wt% at 100 ℃ for 2 hours, and 1.04 wt% of hydrogen can still be discharged within 2 hours at 60 ℃.
(3) When the titanium nitride nano particles and the aluminum hydride powder are mixed, the ball milling treatment time is only 1 hour, so the capacity loss of the ball milling treatment is smaller, and the research result shows that the theoretical capacity of the composite material prepared by the invention is 9.97 and wt%, the actual capacity is 9.90 and wt%, the capacity retention rate reaches 99.3%, and the ball milling capacity loss is only 0.7%.
(4) The preparation process of the composite hydrogen storage material provided by the invention is simple and mature, and the raw materials are cheap and easy to obtain, so that the preparation process is convenient for large-scale industrial production.
Drawings
FIG. 1 is a high resolution transmission electron microscope image of modified catalyst titanium nitride nanoparticles prepared in example 1;
FIG. 2 is a graph showing the XRD spectra of the composite hydrogen storage materials prepared in example 1 and example 2;
FIG. 3 is a temperature-controlled dehydrogenation curve of the composite hydrogen storage material prepared in example 1 and example 2 as such, and aluminum hydride;
FIG. 4 is a differential curve of the temperature-controlled dehydrogenation curves of the composite hydrogen storage materials prepared in examples 1 and 2 as such and aluminum hydride;
FIG. 5 is a constant temperature dehydrogenation curve at 100℃for the composite hydrogen storage materials prepared in example 1 and example 2 as such and aluminum hydride;
FIG. 6 is a graph showing the constant temperature dehydrogenation curves at 60℃for the hydrogen occluding materials prepared in example 1 and example 2.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, methods and apparatus used, without any particular description, are those conventional in the art and are commercially available to those skilled in the art.
Example 1
(1) Preparation of modified catalyst titanium nitride nano-particles
The nano titanium dioxide precursor with the grain diameter of 100nm of 0.1. 0.1 g is weighed and evenly paved on the bottom of the porcelain crucible, and gaps are reserved among grains. The porcelain crucible paved with the precursor is placed in a tube furnace, and ammonia-argon mixed gas is introduced into the porcelain crucible, wherein the volume ratio of ammonia gas to argon gas in the mixed gas is 5:95, and the gas flow rate is 10L/min. After the gas is introduced for 30min, the temperature is raised, and the temperature raising process is divided into two sections: the temperature is firstly increased to 750 ℃ from room temperature at the heating rate of 2 ℃/min, then is increased to 900 ℃ from 750 ℃ at the heating rate of 1 ℃/min, and the temperature is kept stable after the temperature is increased to 900 ℃, so that the precursor reacts at the temperature of 900 ℃ for 1h. And stopping introducing the mixed gas after the reaction is finished and the sample is cooled to room temperature, and collecting the reacted titanium nitride nano particles for later use.
Characterization of the obtained titanium nitride nanoparticles, fig. 1 is a high resolution transmission electron microscope image, and as can be seen from fig. 1, the titanium nitride nanoparticles obtained by the reaction are exposed on the (111) crystal face of the surface layer, which is titanium nitride.
(2) Preparation of titanium nitride-aluminum hydride composite hydrogen storage material
0.594g of aluminum hydride sample and 0.006g of titanium nitride nanoparticle sample obtained in the step (1) are weighed and uniformly mixed in an argon atmosphere, and the total mass is 0.6 g. The uniformly mixed sample is put into a ball milling tank, and stainless steel balls (30 g of total mass) are added into the ball milling tank according to the proportion of 50:1 of ball-to-material ratio. And sealing the ball milling tank in an argon atmosphere, and placing the sealed ball milling tank in a planetary ball mill for mechanical ball milling. The ball mill rotation speed was 350 rpm and the ball milling time was 1h. In order to prevent aluminum hydride from being heated and decomposed due to the overhigh temperature of the tank body, the ball milling time is equally divided into 4 sections, each section is 15 minutes, and the ball milling time is kept stand for 10 minutes between every two sections. And after the ball milling process is finished, taking out the ball milling tank, opening the tank in an argon atmosphere, and collecting a titanium nitride-aluminum hydride composite hydrogen storage material product which is named as TiN-0.01. XRD spectra of the composite hydrogen storage material prepared in this example are shown in FIG. 2.
Example 2
This embodiment differs from embodiment 1 in that: (2) The amount of titanium nitride nanoparticles added was 5wt%, and the rest of the process steps and parameters were set as in example 1. The preparation process of the specific (2) is as follows:
0.57g of aluminum hydride sample and 0.03g of titanium nitride sample were weighed separately, and mixed uniformly in an argon atmosphere, with a total mass of 0.6. 0.6 g. The uniformly mixed sample is put into a ball milling tank, and stainless steel balls (30 g of total mass) are added into the ball milling tank according to the proportion of 50:1 of ball-to-material ratio. And sealing the ball milling tank in an argon atmosphere, and placing the sealed ball milling tank in a planetary ball mill for mechanical ball milling. The ball mill rotation speed was 350 rpm and the ball milling time was 1h. In order to prevent aluminum hydride from being heated and decomposed due to the overhigh temperature of the tank body, the ball milling time is equally divided into 4 sections, each section is 15 minutes, and the ball milling time is kept stand for 10 minutes between every two sections. And after the ball milling process is finished, taking out the ball milling tank, opening the tank in an argon atmosphere, and collecting a titanium nitride-aluminum hydride composite hydrogen storage material product which is named as TiN-0.05. XRD spectra of the composite hydrogen storage material prepared in this example are shown in FIG. 2.
The TiN-0.01 composite hydrogen storage material prepared in example 1, the TiN-0.05 composite hydrogen storage material prepared in example 2 and an aluminum hydride sample (named as is) were subjected to a temperature-controlled dehydrogenation test and a constant temperature dehydrogenation test at 100 ℃, and the corresponding dehydrogenation amounts were calibrated. The specific temperature-controlled dehydrogenation test is that the temperature is increased at a constant rate, the temperature-increasing rate is 2 ℃/min, the calibrated initial dehydrogenation temperature is the zero temperature (the temperature is used as a reference and is used for comparison and does not represent that the dehydrogenation reaction of the hydrogen storage material does not occur at all under the temperature) when y is constant more than 0 in the differential curve of the temperature-controlled dehydrogenation curve. In addition, considering the actual working time of the portable tank body, the dehydrogenation capacity within 2 hours is selected as the effective capacity of constant-temperature dehydrogenation at 100 ℃.
As shown in the test results of FIGS. 3-6, the overall analysis revealed that the initial dehydrogenation temperature of aluminum hydride was 140℃and the total dehydrogenation amount was 10.1 wt%, and that the effective hydrogen storage capacity of 2h at 100℃was 0.19 wt% and that no dehydrogenation was performed at 60 ℃. The initial dehydrogenation temperature of the titanium nitride-aluminum hydride composite hydrogen storage material (example 1) with the addition amount of the titanium nitride nano particles after ball milling being 1 wt percent is 57 ℃, the initial dehydrogenation temperature is reduced by about 83 ℃ compared with the initial dehydrogenation temperature of aluminum hydride in an aluminum hydride sample (initial) and the initial dehydrogenation temperature can be 9.90 wt percent compared with the initial dehydrogenation temperature of aluminum hydride in the initial aluminum hydride sample, the effective hydrogen storage capacity of 2h reaches 8.02 wt percent at 100 ℃, and the effective hydrogen storage capacity is 1.04 wt percent within 2 hours at 60 ℃. And the theoretical capacity of the composite material of the example 1 is 9.97 and wt percent, the actual capacity is 9.90 and wt percent, and the capacity retention rate reaches 99.3 percent. The initial dehydrogenation temperature of the titanium nitride-aluminum hydride composite hydrogen storage material (example 2) with the addition amount of the titanium nitride nano particles after ball milling of 5wt percent is 52 ℃, and the hydrogen capacity can reach 9.46 wt percent. The effective hydrogen storage capacity of 2h at 100 ℃ is 7.66 wt%, and the effective hydrogen storage capacity of 1.13 wt% within 2h at 60 ℃.
In summary, when the additive amount of the composite hydrogen storage material provided by the invention is low, the high capacity characteristic of the aluminum hydride is ensured, the dehydrogenation temperature of the aluminum hydride material is reduced, the dehydrogenation reaction kinetics of the aluminum hydride material is improved, and the low-temperature rapid dehydrogenation of the aluminum hydride material is realized.
While the invention has been described in terms of preferred embodiments, it is not intended to be limited thereto, but rather to enable any person skilled in the art to make various changes and modifications without departing from the spirit and scope of the present invention, which is therefore to be limited only by the appended claims.
Claims (3)
1. The preparation method of the composite hydrogen storage material is characterized in that aluminum hydride powder and titanium nitride nano particles are mixed and ball-milled under a protective atmosphere to obtain the composite hydrogen storage material;
the titanium nitride nano-particles account for 1-5wt%;
the preparation method of the titanium nitride nano-particles comprises the steps of taking titanium dioxide as a precursor, and calcining under an ammonia-argon mixed atmosphere to obtain the titanium nitride nano-particles;
the ammonia-argon mixed atmosphere consists of ammonia gas and argon gas according to the volume ratio of 5:95;
the flow rate of the ammonia-argon mixed gas is 10L/min;
the calcination conditions are as follows: firstly, heating to 750 ℃ at the speed of 2 ℃/min, then heating to 900 ℃ at the speed of 1 ℃/min, and preserving heat for 1h;
the titanium dioxide is nano titanium dioxide.
2. The method according to claim 1, wherein the ball milling conditions are: ball-material ratio is 50:1, rotation speed of ball mill is 350 rpm, single ball milling time is 15min, interval is 10min, and repeating for 4 times.
3. The method of claim 1, wherein the protective atmosphere is argon.
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