CN101279716B - Method for preparing magnesium-based composite hydrogen storage material in magnetic field - Google Patents
Method for preparing magnesium-based composite hydrogen storage material in magnetic field Download PDFInfo
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- CN101279716B CN101279716B CN2008100377182A CN200810037718A CN101279716B CN 101279716 B CN101279716 B CN 101279716B CN 2008100377182 A CN2008100377182 A CN 2008100377182A CN 200810037718 A CN200810037718 A CN 200810037718A CN 101279716 B CN101279716 B CN 101279716B
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Abstract
The invention relates to a method for preparing mg-based composite hydrogen storage material under a magnetic field, which belongs to the technical field of metal functional materials. The method essentially comprises the following steps: La2Mg17 alloy prepared with molten-salt covering method is ground in a glove box after being mixed with 10wt percent of catalytic phase; the well mixed alloy powder is put in a self-made high-pressure reaction vessel after being wrapped with nickel plates; hydrogen is filled after repeated vacuum-pumping; the high-pressure reaction vessel is put in a 1-12T steady strong magnetic field and heated up to 350 DEG C and then heat preservation is carried out; the mg-based composite hydrogen storage material powder can be obtained after slow temperature reduction. The material prepared by the method has multiphase structure and has the advantages of high activity, even component and low content of impurity. The PCT test finds that the composite hydrogen storage material has high volume and good hydrogen absorption and desorption performances.
Description
Technical field
The present invention relates to a kind of method of preparing magnesium-based composite hydrogen storage material in magnetic field, belong to the Metallic Functional Materials technical field.
Background technology
In the near future, energy problem will further become the main bottleneck of restriction development of world economy.Hydrogen Energy is as a kind of renewable energy source, owing to itself have cleaning, advantage such as efficient, becomes the breach of energy revolution just gradually.The storage of hydrogen is the key that Hydrogen Energy is utilized, and in order to develop heavy body, hydrogen storage material cheaply, people have carried out big quantity research to hydrogen storage alloy.Wherein, Magnuminium receives much concern because it has possessed advantages such as density is little, hydrogen storage capability is high, aboundresources, and is cheap.
It is relatively harsher that but hydrogen condition is put in the suction of pure magnesium, need could react under 350 ℃ high temperature with hydrogen, and hydrogen desorption kinetics is also relatively poor, can not be as the hydrogen storage material of reality use.Discover that the major cause that magnesium is inhaled hydrogen kinetics difference is that hydrogen is at the initial one deck MgH that forms of hydride grain surface
2Spread slow on the epidermis.The then main high stability of hydrogen discharging temperature height owing to magnesium hydride.The interpolation of catalysis phase can improve surfactivity, increase diffusion admittance, improves the hydrogenation kinetics of magnesium, can reduce unit cell volume by additive simultaneously, makes the stability of the hydride of magnesium that decline be arranged slightly.The another kind of method that can change hydride stability changes its structure exactly.When the hydrogen storage material of preparing has amorphous or nanocrystalline, non-crystal structure, the suction hydrogen desorption kinetics performance of material will be improved.
It seems that comprehensively the exploitation of the nanometer of magnesium base alloy material structure and high catalytic performance polynary system alloy is a research direction from now on.Carry out the microstructure that catalysis is composite mixed, control hydrogen storage material, all have important theory and practical significance for the hydrogen storage property and the development of new composite hydrogen storage material that improve material.
Summary of the invention
The method that the purpose of this invention is to provide a kind of preparing magnesium-based composite hydrogen storage material in magnetic field.Adopt method of the present invention can prepare even, highly active complex phase alloy material storing hydrogen; The magnesium base composite hydrogen storage alloy of the inventive method preparation also has characteristics such as capacity height, hydrogenation dynamic performance are good.
For achieving the above object, the present invention is by the following technical solutions:
A kind of method of preparing magnesium-based composite hydrogen storage material in magnetic field is characterized in that this method has following processing step:
1) take by weighing each component according to Mg base hydrogen bearing alloy with catalysis proportioning mutually, described Mg base hydrogen bearing alloy matrix is La
2Mg
17Alloy, catalysis are Fe mutually
3O
4, Nb
2O
5Or a kind of in the Ni powder, the amount of wherein catalysis phase accounts for 5～15wt.% of gross weight, utilizes agate mortar to grind 10～20min in glove box and makes its thorough mixing;
2) be placed in stainless steel crucible with nickel sheet parcel said mixture and put into autoclave, vacuumize repeatedly 3～5 times, feed the hydrogen of purity 〉=99.999% subsequently, pressure leaves standstill 10～30min after reaching 1.0～5.0MPa;
3) autoclave is placed the steady strong magnetic field of 6～12T, the tubular oven of making by a weak magnetic material heats material, temperature rise rate is 3～10 ℃/min, be incubated 100～300min after being warming up to 350 ℃, be chilled to after the room temperature with stove material is taken out, will obtain Mg-based composite hydrogen storage material after its vacuum packaging.
Material hydrogenation recombination process described in the above-mentioned method for preparing the magnesium base composite hydrogen storage alloy is in the steady strong magnetic field of 5MPa hydrogen atmosphere and 6～12T, is heated to 350 ℃ and be incubated 180min by the temperature rise rate of 5 ℃/min.
Employed autoclave and tubular oven device are made by the stainless material of weak magnetic in the above-mentioned method for preparing the magnesium base composite hydrogen storage alloy.
The principle of the inventive method is: in the highly compressed hydrogen atmosphere, the energy that utilizes high-intensity magnetic field and heating source to provide, make alloy, catalysis and hydrogen generation interaction, form hydride and new catalysis mutually, wherein the formation of hydride is the gas-solid anoxycausis reaction under a kind of outer field action, the heat that reaction produces triggers the formation of cenotype again, is a kind of method for preparing Mg base hydrogen bearing alloy of efficient energy-saving.Simultaneously, the existence in magnetic field has reduced temperature of reaction, thereby has avoided alloy grain growing up at high temperature, plays the effect of crystal grain thinning.
The inventive method compared with prior art has the following advantages:
1) magnetic field is compared with traditional heat exchange pattern by influence electronic motion state in the material and it being transmitted energy, and it can more uniform transmission energy, thereby makes matrix material obtain uniformly distribution mutually;
2) Mg-based composite hydrogen storage material of preparation has purity and hydrogenation property preferably under the steady magnetic field, and magnetic field energy suppresses La (OH) to a certain extent
3Formation, promote La to form hydride simultaneously;
3) magnetic field energy produces the influence of intensive thermodynamics to chemical reaction in the hydrogen storage material preparation process and phase transformation, reduces temperature of reaction, shortens the reaction times, not only can play the effect of crystal grain thinning, more can reach the purpose of efficient energy-saving;
4) pressure-composition-temperature (PCT) and dynamic performance test shows, the Mg-based composite hydrogen storage material activation performance excellence of the inventive method preparation, hydrogen storage capability is big, dynamic performance good;
5) the hydrogen storage system of enumerating in embodiment, this method is applicable to that also other magnesium is the preparation of composite hydrogen storage material.
Description of drawings
Among Fig. 1 the present invention among the embodiment 1 XRD figure of Mg-based composite hydrogen storage material spectrum (preparation condition is: no outfield (following collection of illustrative plates); 6T magnetic field (middle collection of illustrative plates); 12T magnetic field (going up collection of illustrative plates));
Hydrogen curve contrast (it is 6T that magneticstrength is adopted in preparation, and temperature rise rate is 5 ℃/min, and putting the hydrogen initial condition is vacuum) is put in the matrix material temperature programming of each embodiment preparation among Fig. 2 the present invention;
The SEM feature image of Mg-based composite hydrogen storage material (it is 6T that magneticstrength is adopted in preparation) among the embodiment 3 among Fig. 3 the present invention;
Among Fig. 4 the present invention among the embodiment 4 Mg-based composite hydrogen storage material XRD figure spectrum (preparation condition is: no outfield (following collection of illustrative plates); 6T magnetic field (middle collection of illustrative plates); 12T magnetic field (going up collection of illustrative plates));
The PCT curve of Mg-based composite hydrogen storage material (it is 6T that magneticstrength is adopted in preparation) among the embodiment 4 among Fig. 5 the present invention;
Hydrogen curve (temperature rise rate is 5 ℃/min, and putting the hydrogen initial condition is vacuum) is put in Mg-based composite hydrogen storage material temperature programming among Fig. 6 the present invention among the embodiment 4.
Embodiment
The present invention is described in detail below by embodiment, but method of the present invention is not limited in embodiment.
Take by weighing La
2Mg
17Alloy 10g utilizes agate mortar to grind 10min in glove box it is fully pulverized; Be placed in stainless steel crucible with nickel sheet parcel alloy powder and put into autoclave, vacuumize the hydrogen that feeds purity 〉=99.999% after 3 times repeatedly, pressure leaves standstill 30min after reaching 5.0MPa; Autoclave is placed the steady strong magnetic field of 6T and 12T, by tubular oven material is heated, temperature rise rate is 5 ℃/min, is incubated 180min after being warming up to 350 ℃, be chilled to after the room temperature with stove material is taken out, will promptly obtain Mg-based composite hydrogen storage material after its vacuum packaging.For comparative analysis, under the constant situation of other processing parameters, we have also carried out hydrogen treatment to alloy when no outfield.Fig. 1 is the X-ray diffraction figure of material.As seen from the figure, for pure La
2Mg
17The phase composite influence after to hydrogenation of hydrogen storage alloy, magnetic field is smaller, but high-intensity magnetic field can suppress La (OH) to a certain extent
3Formation, promote La to form hydride simultaneously.Generally speaking, the hydride that mutually is mainly La and Mg of alloy after hydrogen treatment and a small amount of La (OH)
3, do not observe the existence of other dephasigns, illustrate that alloy has purity and hydrogenation property preferably.
According to La
2Mg
17-10wt.%Fe
3O
4Proportioning take by weighing altogether 10g of two kinds of components, in glove box, utilize agate mortar to grind 20min and make its thorough mixing; Be placed in stainless steel crucible with nickel sheet parcel said mixture and put into autoclave, vacuumize the hydrogen that feeds purity 〉=99.999% after 3 times repeatedly, pressure leaves standstill 30min after reaching 5.0MPa; Autoclave is placed the steady strong magnetic field of 6T and 12T, by tubular oven material is heated, temperature rise rate is 5 ℃/min, is incubated 180min after being warming up to 350 ℃, be chilled to after the room temperature with stove material is taken out, will promptly obtain Mg-based composite hydrogen storage material after its vacuum packaging.For comparative analysis, under the constant situation of other processing parameters, we have also carried out hydrogen treatment to this system material when no outfield.The temperature programming of Fig. 2 is inhaled the hydrogen experimental result and is shown Fe
3O
4Existence reduced La
2Mg
17The decomposition temperature of alloy, and its catalytic effect is better than Nb
2O
5Table 1 has provided the PCT test result of material: behind the 6T the action of a magnetic field, it is low that it inhales the pressure drop of hydrogen platform, puts the hydrogen platform and press slightly rising, and lag coefficient diminishes, and illustrates to add Fe
3O
4It is favourable that hydrogen is put in the suction of this system hydrogen storage material.Between 523～623K, the hydrogen-releasing rate of hydrogen storage alloy is all greater than 90%, and it is more thorough to put hydrogen; Add Fe
3O
4La
2Mg
17The alloy hydrogen-releasing rate will be higher than the La under the same processing
2Mg
17Alloy.
The matrix material hydrogen storage property contrast of table 1 embodiment 2 preparations
According to La
2Mg
17-10wt.%Nb
2O
5Proportioning take by weighing altogether 10g of two kinds of components, in glove box, utilize agate mortar to grind 20min and make its thorough mixing; Be placed in stainless steel crucible with nickel sheet parcel said mixture and put into autoclave, vacuumize the hydrogen that feeds purity 〉=99.999% after 3 times repeatedly, pressure leaves standstill 30min after reaching 5.0MPa; Autoclave is placed the steady strong magnetic field of 6T and 12T, by tubular oven material is heated, temperature rise rate is 5 ℃/min, is incubated 180min after being warming up to 350 ℃, be chilled to after the room temperature with stove material is taken out, will promptly obtain Mg-based composite hydrogen storage material after its vacuum packaging.Fig. 3 has provided La
2Mg
17-10wt.%Nb
2O
5The SEM photo of matrix material after hydrogen treatment under the 6T high-intensity magnetic field.Nb as can be seen from Figure
2O
5Be evenly distributed on La mutually as catalysis
2Mg
17The surface of alloy, particle surface has crackle to produce simultaneously.These catalysis that are evenly distributed on the surface help the absorption and the decomposition of hydrogen atom mutually, and the absorption and the diffusion of hydrogen atom then accelerated in the generation of crackle.The temperature programming of Fig. 2 is put the hydrogen experimental result and has been confirmed Nb
2O
5Existence can reduce La
2Mg
17The decomposition temperature of alloy.
According to La
2Mg
17The proportioning of-10wt.%Ni takes by weighing two kinds of components 10g altogether, utilizes agate mortar to grind 20min in glove box and makes its thorough mixing; Be placed in stainless steel crucible with nickel sheet parcel said mixture and put into autoclave, vacuumize the hydrogen that feeds purity 〉=99.999% after 3 times repeatedly, pressure leaves standstill 30min after reaching 5.0MPa; Autoclave is placed the steady strong magnetic field of 6T and 12T, by tubular oven material is heated, temperature rise rate is 5 ℃/min, is incubated 180min after being warming up to 350 ℃, be chilled to after the room temperature with stove material is taken out, will promptly obtain Mg-based composite hydrogen storage material after its vacuum packaging.For comparative analysis, under the constant situation of other processing parameters, we have also carried out hydrogen treatment to this system material when no outfield.Fig. 4 is the X-ray diffraction figure of material.As seen from the figure, the hydrogenation process of alloy all carries out relatively thoroughly, and phase composite is various forms of hydride and a spot of La (OH)
3Phase.Mg has all appearred in hydrotreated alloy under the different magnetic field
2NiH
4Diffraction peak, and along with the enhancing of magneticstrength, Mg
2NiH
4Peak value strengthen gradually, and the peak of Ni weakens gradually, when magneticstrength reached 12T, the completely dissolve of Ni peak illustrated that high-intensity magnetic field promotes Mg
2NiH
4Formation.Fig. 5 has provided the La after the 6T magnetic field treatment
2Mg
17-10wt.%Ni matrix material two platforms occurred at each temperature PCT curve in the curve, the platform that pressure is lower is put hydrogen corresponding to the suction of Mg, and this is smooth and broad, hydrogen is put in suction played main contribution; Higher relatively platform is corresponding to Mg
2Hydrogen is put in the suction of Ni phase, Mg
2Ni has played promotion and katalysis to putting hydrogen.According to the PCT curve, can use the Van't Hoff formula to calculate relation and corresponding Δ H and Δ S that material is inhaled equilibrium pressure and temperature when putting hydrogen, be listed in table 2.As seen from table, the material of 12T magnetic field preparation has less Δ H and Δ S value.For hydrogen storage material, little Δ H and Δ S help the carrying out of hydrogen discharge reaction, have advantage so this method prepares composite hydrogen storage material on thermodynamics.
The matrix material of table 2 embodiment 4 preparations is inhaled Van ' t Hoff relational expression and the enthalpy and the entropy of hydrogen discharge reaction
| Project | No outfield | 6T | 12T |
| Inhale hydrogen, (523K≤T≤623K) | lg(P/0.1MPa)＝-4225/T+7.671 | lg(P/0.1MPa)＝-3977/T+7.297 | lg(P/0.1MPa)＝-3761/T+6.916 |
| Put hydrogen, (523K≤T≤623K) | lg(P/0.1MPa)＝-4035/T+7.189 | lg(P/0.1MPa)＝-4290/T+7.571 | lg(P/0.1MPa)＝-3942/T+6966 |
| Δ S (suction hydrogen) | -147J/(mol·K) | -140J/(mol·K) | -132J/(mol·K) |
| Δ S (putting hydrogen) | 138J/(mol·K) | 145J/(mol·K) | 133J/(mol·K) |
| Δ H (suction hydrogen) | -81kJ/mol H 2 | -76kJ/mol H 2 | -72kJ/mol H 2 |
| Δ H (putting hydrogen) | 77kJ/molH 2 | 82kJ/molH 2 | 76kJ/mol H 2 |
Fig. 6 is that the hydrogen curve is put in the matrix material temperature programming of embodiment 4 preparations, and temperature rise rate is 5 ℃/min.As seen from the figure, the interaction energy of high-intensity magnetic field reduces the initial hydrogen discharging temperature of matrix material, and the initial hydrogen discharging temperature of (magneticstrength) material is followed successively by from low to high under the different preparation conditions: 12T＜6T＜0T.To hydrogenation compound material under the 12T high-intensity magnetic field, it puts the hydrogen curve can be divided into three parts, and the initial stage hydrogen discharging speed is very fast, and this process lasts till that hydrogen desorption capacity is about 0.4wt.%, and this stage is corresponding to Mg
2NiH
4The decomposition of phase.Is subordinate phase from putting hydrogen 0.5wt.% to 1.0wt.%.In this stage, the hydrogen discharging speed of system begins to reduce, corresponding to Mg
2NiH
4The decomposition of phase finishes and the decomposition of Mg hydride begins.Can find principal phase (La behind the interpolation Ni in conjunction with Fig. 2
2Mg
17) decomposition temperature of hydride is starkly lower than pure La
2Mg
17Decomposition temperature after the phase hydrogenation illustrates Mg
2Katalysis has been played in the decomposition of the relative hydride of Ni.Be the phase III to the end from putting hydrogen 1.0wt.%, in this stage, along with the rising and the MgH of temperature
2The further acceleration of decomposing, the alloy hydrogen discharging speed tends towards stability gradually, up to putting hydrogen near finishing.
Claims (3)
1. the method for a preparing magnesium-based composite hydrogen storage material in magnetic field is characterized in that this method has following processing step:
1) take by weighing each component according to Mg base hydrogen bearing alloy with catalysis stoichiometric mutually, described Mg base hydrogen bearing alloy matrix is La
2Mg
17Alloy, catalysis are Fe mutually
3O
4, Nb
2O
5Or a kind of in the Ni powder, the amount of wherein catalysis phase accounts for 5～15wt.% of gross weight, utilizes agate mortar to grind 10～20min in glove box, makes its thorough mixing;
2) be placed in stainless steel crucible with nickel sheet parcel said mixture and put into autoclave, vacuumize repeatedly 3～5 times, feed the hydrogen of purity 〉=99.999% subsequently, pressure leaves standstill 10～30min after reaching 1.0～5.0MPa;
3) autoclave is placed the steady strong magnetic field of 6～12T, the tubular oven of making by a weak magnetic material heats material, temperature rise rate is 3～10 ℃/min, be incubated 100～300min after being warming up to 350 ℃, be chilled to after the room temperature with stove material is taken out, will obtain Mg-based composite hydrogen storage material after its vacuum packaging.
2. the method for preparing Mg-based composite hydrogen storage material according to claim 1 is characterized in that in the steady strong magnetic field of 5MPa hydrogen atmosphere and 6～12T, is heated to 350 ℃ and be incubated 180min by the temperature rise rate of 5 ℃/min.
3. the method for preparing Mg-based composite hydrogen storage material according to claim 1 is characterized in that employed autoclave and tubular oven device make by the stainless material of weak magnetic.
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| CN108188406A (en) * | 2017-12-21 | 2018-06-22 | 陕西科技大学 | A kind of magnesium-base nanometer composite hydrogen-storing material and preparation method |
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|---|---|---|---|---|
| US4126242A (en) * | 1974-07-16 | 1978-11-21 | The Research Institute For Iron, Steel And Other Metals Of The Tohoku University | Hydrogen-occluding alloy |
| CN1478055A (en) * | 2000-11-07 | 2004-02-25 | �������繫˾ | Method of rapidly carrying out hydrogenation of hydrogen storage material |
| CN1896289A (en) * | 2006-06-27 | 2007-01-17 | 上海大学 | Production of magnesium-based hydrogen-storage material under equalized strong magnetic field and its producer |
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2008
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4126242A (en) * | 1974-07-16 | 1978-11-21 | The Research Institute For Iron, Steel And Other Metals Of The Tohoku University | Hydrogen-occluding alloy |
| CN1478055A (en) * | 2000-11-07 | 2004-02-25 | �������繫˾ | Method of rapidly carrying out hydrogenation of hydrogen storage material |
| CN1896289A (en) * | 2006-06-27 | 2007-01-17 | 上海大学 | Production of magnesium-based hydrogen-storage material under equalized strong magnetic field and its producer |
Non-Patent Citations (5)
| Title |
|---|
| JP特开2003-277001A 2003.10.02 |
| Qian Li et al..Feasibility study on the controlled hydriding combustionsynthesis of Mg-La-Ni ternary hydrogen storage composite.International Journal of Hydrogen Energy32.2006,321875-1884. * |
| Qian Li et al..Synthesis and hydrogenation properties of Mg-3mol%LaNi3composite prepared under an external magnetic field.Intermetallics15.2006,1561-68. * |
| 唐有根 等.磁场凝固处理对稀土贮氢合金结构和电化学性能的影响.稀有金属材料与工程36 11.2007,36(11),1971-1974. |
| 唐有根等.磁场凝固处理对稀土贮氢合金结构和电化学性能的影响.稀有金属材料与工程36 11.2007,36(11),1971-1974. * |
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