CN112265957B - Preparation method of magnesium-based hydrogen storage material with high hydrogen storage density - Google Patents
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Abstract
The invention discloses a preparation method of a magnesium-based hydrogen storage material with high hydrogen storage density, which adopts a temperature-changing mechanical ball milling process to prepare MgH 2 Performing gradual temperature-changing mechanical ball milling with the activated TiFe alloy under different filling gases in different proportions to realize gradual and gradual mild ball milling conditions to obtain MgH 2 -a TiFe nano magnesium based hydrogen storage material. The hydrogen absorption and desorption temperature of the obtained hydrogen storage material is obviously reduced, the initial hydrogen desorption temperature is 466K, and the hydrogen desorption peak temperature is 552K. The preparation process of the nano magnesium hydride is simple and convenient to operate and low in operation temperature, solves the problems of high operation temperature and large hydride crystal grain required by the conventional preparation of the nano magnesium hydride, improves the hydrogen charging and discharging performance of the nano magnesium-based hydrogen storage material, and has good development prospect.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a preparation method of a high hydrogen storage density nano magnesium-based hydrogen storage material, so as to obtain a nano material with good hydrogen storage performance.
Background
The hydrogen energy is an ideal renewable energy source, the hydrogen fuel cell can efficiently convert the hydrogen energy into the electric energy without the restriction of Carnot cycle, and the greenhouse gas emission does not exist, so the hydrogen fuel cell has great development prospect, but the storage and transportation technology of the hydrogen greatly restricts the practical application of the hydrogen fuel cell. Compared with the hydrogen storage in a high-pressure gas cylinder, the solid alloy hydrogen storage has the unique advantage in safety, is widely applied to various hydrogen energy fields, and is a hydrogen storage mode with the greatest development prospect.
The magnesium hydride hydrogen storage material has high hydrogen storage capacity, rich magnesium resource storage on the earth and obvious advantages in use cost, and is taken as one of ideal solid hydrogen storage materials. However, compared with the traditional hydrogen storage alloy, the hydrogen evolution kinetics and the thermodynamic property of the magnesium hydride material are not ideal, the hydrogen evolution temperature usually reaches above 350 ℃ to reach the expected hydrogen storage density, and the overhigh operating temperature severely limits the practical application of the magnesium hydride, so that a method for improving the disadvantages of the kinetics and the thermodynamics is urgently needed, and the advantage of the high hydrogen storage density can be fully utilized.
Disclosure of Invention
In view of the defect that the existing magnesium-based hydrogen storage material generally has higher operation temperature, the invention aims to provide a preparation method of a nano magnesium-based hydrogen storage material with lower operation temperature.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for preparing magnesium-based hydrogen storage material with high hydrogen storage density comprises the following steps
(1) Placing the TiFe alloy packaged and stored in vacuum into a sample chamber of hydrogen absorption reaction equipment, vacuumizing at the high temperature of 600 ℃, and introducing high-pressure hydrogen with the pressure of 4-5 MPa for pressure maintaining;
(2) repeating the step (1) for many times, and cooling the system to room temperature when the hydrogen pressure of the sample chamber is obviously reduced to obtain activated TiFe alloy particles;
(3) Mixing the activated TiFe alloy particles with MgH 2 Mixing the raw materials in a ratio of 1: 10-1: 50, placing the mixture into a ball milling tank, sealing the ball milling tank, and vacuumizing the ball milling tank for 2 to 3 hours at the temperature of 150 ℃ in a variable temperature ball milling device;
(4) and (3) introducing high-purity argon of 0.1-0.5 MPa into the ball milling tank at the temperature of the step (3), wherein the ball-material ratio is 30: 1, ball milling for 2-3 hours;
(5) cooling the device to be below 100 ℃, introducing a hydrogen-argon mixed gas of 0.1-0.5 MPa into the ball milling tank, wherein hydrogen and argon respectively account for half, performing ball milling at 150 ℃ for 2-3 hours, supplementing the hydrogen-argon mixed gas into the ball milling tank to 1-1.5 MPa after stopping ball milling, and performing ball milling for 2-3 hours;
(6) vacuumizing the device at 200 ℃, introducing high-purity hydrogen with the pressure of 0.1-0.5 MPa, ball-milling for 2-3 hours, supplementing the high-purity hydrogen to the ball-milling tank to 1-1.5 MPa after ball-milling is stopped, and ball-milling for 2-3 hours to obtain MgH 2 -a TiFe nano magnesium-based high hydrogen storage density hydrogen storage material.
The preparation method of the magnesium-based hydrogen storage material with high hydrogen storage density comprises the step (1) of vacuumizing for 60 min.
In the preparation method of the magnesium-based hydrogen storage material with high hydrogen storage density, the pressure in the step (2) is obviously reduced by 0.5MPa in 30 minutes.
According to the preparation method of the magnesium-based hydrogen storage material with high hydrogen storage density, the TiFe particles activated in the step (2) are stored in the atmosphere of high-purity hydrogen, so that the TiFe alloy particles are prevented from being poisoned, and the storage time is not longer than 48 hours.
In the preparation method of the magnesium-based hydrogen storage material with high hydrogen storage density, the activated TiFe alloy particles in the step (3) are placed in a ball milling tank in a glove box under argon atmosphere.
According to the preparation method of the magnesium-based hydrogen storage material with high hydrogen storage density, the ball milling speed in the step (4) is 300 rpm, mechanical energy can be converted into partial heat energy in the high-energy ball milling process, and the temperature of the system can be increased, so that the ball milling temperature is controlled by the variable-temperature ball milling device through filling of inert gas.
In the preparation method of the magnesium-based hydrogen storage material with high hydrogen storage density, the hydrogen component of the hydrogen-argon mixed gas in the step (5) is 50%, and the argon component is 50%.
The invention has the beneficial effects that: the invention adopts an in-situ ball milling method of gradually changing the temperature of metal magnesium hydride particles and activated TiFe particles and gradually introducing filling gas, aims to realize gradually mild ball milling conditions, prevents TiFe alloy particles which are easy to be poisoned from being polluted, enables the TiFe alloy and magnesium hydride to be more fully contacted, and obtains the nano magnesium-based hydrogen storage material which has good appearance, small and uniform particle size and obviously improved hydrogen absorption and desorption dynamics and thermodynamic performance.
The hydrogen absorption and desorption temperature of the hydrogen storage material prepared by the method is remarkably reduced, the initial hydrogen desorption temperature is 466K, the hydrogen desorption peak temperature is 552K, the preparation process is simple and convenient to operate, the operation temperature is low, the problems of high operation temperature and large hydride crystal grain size required by the conventional preparation of nano magnesium hydride are solved, the hydrogen absorption and desorption performance of the nano magnesium-based hydrogen storage material is improved, and the method has a good development prospect.
Drawings
FIG. 1 is a Transmission Electron Microscope (TEM) image of the Mg-based hydrogen storage material obtained in examples 1-3 of the present invention;
FIG. 2 is a graph of hydrogen evolution kinetics at 523K for the magnesium-based hydrogen storage materials of examples 1-3 of the present invention;
FIG. 3 is a graph of dehydrogenation Mass Spectra (MS) of magnesium-based hydrogen storage materials of examples 1-3 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples, which are as follows.
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described in detail below with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The TiFe hydrogen storage alloy is a common hydrogen storage material, has the advantages of low price, good cycle performance and the like, can be used as a catalyst in a special scene, but is difficult to be used together with low-melting-point materials such as magnesium hydride and the like due to the characteristics of difficult activation, easy inactivation in air and the like.
The mechanical ball milling method is another common method for synthesizing the nano structure, but magnesium has good ductility, the mechanical ball milling method can reduce the particle size of magnesium to submicron level, prolong the ball milling time and even possibly grow the particles again, the kinetic performance of the prepared nano magnesium hydride can be improved, and the optimization of the thermodynamic performance is not ideal;
in order to improve the kinetic and thermodynamic properties of metal magnesium hydride particles, a certain amount of catalyst is often added, wherein transition metal, carbon material, etc. are widely used catalysts, and in addition, adding other hydrogen storage materials as catalysts is also regarded as a common method for improving kinetic thermodynamics, such as LaNi 5 、LiNH 2 And LiBH 4 The hydrogen storage material can be used for self hydrogen release after being fully activated, and simultaneously can realize synchronous optimization on the thermodynamic kinetics of the magnesium hydride in the reaction process, thereby playing a role similar to a catalyst, and being a more common catalyst.
Example 1
And (3) placing the TiFe alloy in a sample chamber of a hydrogen absorption reaction device, vacuumizing for 60min at a high temperature of 600 ℃, introducing high-pressure hydrogen for pressure maintaining, and cooling the system to room temperature when the hydrogen pressure in the sample chamber is obviously reduced to obtain activated TiFe alloy particles.
Mixing the activated TiFe alloy particles with magnesium hydride and a mixture of the mixture of 1: 50, placing the mixture into a ball milling tank, sealing the ball milling tank, vacuumizing the ball milling tank for 2 hours at the temperature of 150 ℃ in a variable temperature ball milling device, and introducing high-purity argon gas of 0.1MPa into the ball milling tank, wherein the ball material ratio is 30: 1, ball milling for 2 hours at the ball milling rotating speed of 300 rpm.
Cooling the device to be below 100 ℃, introducing 0.1MPa hydrogen and argon mixed gas into the ball milling tank, wherein the hydrogen component is 50 percent, the argon component is 50 percent, performing ball milling for 2 hours at 150 ℃, supplementing the hydrogen and argon mixed gas into the ball milling tank to 1MPa after stopping ball milling, and performing ball milling for 2 hours.
Vacuumizing the device at 200 ℃ after ball milling is stopped, then introducing high-purity hydrogen with the pressure of 0.1MPa, ball milling for 2 hours, supplementing the high-purity hydrogen into the ball milling tank to the pressure of 1MPa after ball milling is stopped, and carrying out ball milling for 2 hours to obtain MgH 2 -a TiFe nano magnesium based hydrogen storage material.
TEM image of sample material obtained in this example is shown in (c) of FIG. 1, MgH alone 2 And TEM images of TiFe are shown in (a) and (b) of fig. 1. As can be seen, MgH was present after ball milling 2 And the particle size of the TiFe remains unchanged with an average dimension of 400 nm. But MgH after ball milling 2 The surface of the sample appeared very rough, indicating that many surface defects were generated during the ball milling process.
FIG. 2 is a graph of hydrogen evolution curves for samples of magnesium-based hydrogen storage materials at 523K. As can be seen from curve (a) in fig. 2, almost no hydrogen gas is released at this temperature without the addition of TiFe alloy particles, which is common for magnesium hydride materials. As can be seen from curve (b) in FIG. 2, about 6 wt% of hydrogen was released within 10min after the addition of 2 wt% TiFe.
FIG. 3 is a DSC hydrogen desorption curve of a sample under Ar atmosphere at a heating speed of 10K/min, FIG. 3 (a) is a hydrogen desorption mass spectrum curve of magnesium hydride alone, and it can be seen from the graph that the hydrogen desorption peak temperature is up to 663K, FIG. 3 (b) is a hydrogen desorption mass spectrum curve of magnesium hydride and 2 wt% of TiFe alloy particles after ball milling, and the hydrogen desorption peak temperature is reduced from 663K to 551K. Illustrating the thermodynamic performance of the sample of this example compared to MgH alone 2 Is greatly improved.
Example 2
And (3) placing the TiFe alloy in a sample chamber of a hydrogen absorption reaction device, vacuumizing for 60min at a high temperature of 600 ℃, introducing high-pressure hydrogen for pressure maintaining, and cooling the system to room temperature when the hydrogen pressure in the sample chamber is obviously reduced to obtain activated TiFe alloy particles.
Mixing activated TiFe alloy particles with magnesium hydride and a mixture of 1: 20, placing the mixture into a ball milling tank, sealing the ball milling tank, vacuumizing the ball milling tank for 2.5 hours at the temperature of 150 ℃ in a variable temperature ball milling device, and introducing high-purity argon gas of 0.25MPa into the ball milling tank, wherein the ball material ratio is 30: 1, the ball milling speed is 300 rpm, and the ball milling is carried out for 2.5 hours.
Cooling the device to be below 100 ℃, introducing 0.25MPa hydrogen and argon mixed gas into the ball milling tank, wherein the hydrogen component is 50 percent, the argon component is 50 percent, performing ball milling for 2.5 hours at 150 ℃, supplementing the hydrogen and argon mixed gas into the ball milling tank to 1.25MPa after stopping ball milling, and performing ball milling for 2 hours.
Vacuumizing the device at 200 ℃ after ball milling is stopped, then introducing high-purity hydrogen with the pressure of 0.25MPa, ball milling for 2.5 hours, supplementing the high-purity hydrogen into the ball milling tank to the pressure of 1.25MPa after ball milling is stopped, and carrying out ball milling for 2.5 hours to obtain MgH 2 -a TiFe nano magnesium based hydrogen storage material.
The TEM image of the sample material obtained in this example is shown in FIG. 1 (d), from which it can be seen that MgH is present after ball milling 2 And the particle size of the TiFe remains unchanged with an average dimension of 400 nm. But MgH after ball milling 2 The surface of the sample appeared very rough, indicating that many surface defects were generated during the ball milling process. Hydrogen evolution curve of ball milled samples under 523K conditions.
As can be seen from fig. 2, almost no hydrogen was released at this temperature without the addition of the TiFe catalyst. As can be seen from the curve (c) in FIG. 2, after addition of 5 wt% TiFe, about 5 wt% of hydrogen was released within 4min, and the improvement in hydrogen release kinetics was significant.
FIG. 3 is a DSC chart of hydrogen evolution of a sample under Ar atmosphere at a heating rate of 10K/min. FIG. 3, curve (c), shows the hydrogen evolution mass spectrum of magnesium hydride after ball milling with 5 wt% TiFe alloy particles, with the peak hydrogen evolution temperature decreasing from 663K to 540K. Illustrating the thermodynamic performance of the sample of this example compared to MgH alone 2 Is greatly improved.
Example 3
And (3) placing the TiFe alloy in a sample chamber of a hydrogen absorption reaction device, vacuumizing for 60min at a high temperature of 600 ℃, introducing high-pressure hydrogen for pressure maintaining, and cooling the system to room temperature when the hydrogen pressure in the sample chamber is obviously reduced to obtain activated TiFe alloy particles.
Mixing activated TiFe alloy particles with magnesium hydride and a mixture of 1: 10, placing the mixture in a ball milling tank, sealing the ball milling tank, vacuumizing the ball milling tank for 3 hours at the temperature of 150 ℃ in a variable temperature ball milling device, and introducing high-purity argon gas of 0.5MPa into the ball milling tank, wherein the ball material ratio is 30: 1, the ball milling speed is 300 rpm, and the ball milling is carried out for 3 hours.
Cooling the device to be below 100 ℃, introducing 0.5MPa hydrogen and argon mixed gas into the ball milling tank, wherein the hydrogen component is 50 percent, the argon component is 50 percent, performing ball milling for 3 hours at 150 ℃, supplementing the hydrogen and argon mixed gas into the ball milling tank to 1.5MPa after stopping ball milling, and performing ball milling for 3 hours.
Vacuumizing the device at 200 ℃ after ball milling is stopped, then introducing high-purity hydrogen with the pressure of 0.5MPa, ball milling for 3 hours, supplementing the high-purity hydrogen into the ball milling tank to the pressure of 1.5MPa after ball milling is stopped, and carrying out ball milling for 3 hours to obtain MgH 2 -a TiFe nano magnesium based hydrogen storage material.
The TEM image of the sample material obtained in this example is shown as (e) in FIG. 1, from which it can be seen that MgH is present after ball milling 2 And the particle size of the TiFe remains unchanged with an average dimension of 400 nm. But MgH after ball milling 2 The surface of the sample appeared rough, indicating that many surface defects were generated during the ball milling process, and (f) in fig. 1 is a TEM image of the magnesium-based hydrogen storage material after increasing the addition amount of the TiFe alloy. As can be seen from the graph, the increase in the addition amount of the TiFe alloy does not decrease MgH 2 The particle size of (1).
FIG. 2 is a graph of hydrogen evolution for a ball milled sample at 523K. As can be seen from fig. 2, almost no hydrogen was released at this temperature without the addition of the TiFe catalyst. It can be seen from the curve (d) in fig. 2 that after 10 wt% of TiFe is added, about 3 wt% of hydrogen is released within 1min, and the hydrogen release kinetics is improved remarkably, but since the hydrogen release amount of the material is already relatively close to the theoretical hydrogen release amount, and TiFe itself belongs to a material with low hydrogen storage density, the addition of too much TiFe will reduce the mass hydrogen storage density of the material, so that the regulation of the kinetic performance cannot provide more hydrogen release amount. FIG. 3 is a DSC chart of hydrogen evolution of a sample under Ar atmosphere at a heating rate of 10K/min.
FIG. 3, curve (d), is the hydrogen evolution mass spectrum curve of magnesium hydride and TiFe alloy particles of 10 wt% after ball milling, the peak temperature of hydrogen evolution decreases from 663K to 525K. The thermodynamic property of the sample is improved after the addition of the TiFe, but the content of the TiFe is increased from 5% to 10%, the hydrogen desorption peak temperature is not greatly reduced, and a curve (e) in FIG. 3 is a hydrogen desorption mass spectrum curve of the magnesium-based hydrogen storage material after the addition of the TiFe alloy is increased, so that the continuous improvement of the content of the TiFe can not greatly reduce the hydrogen desorption peak, and the purpose of further optimizing the hydrogen desorption thermodynamic property of the material can be achieved.
The above-described embodiments are merely illustrative of the principles and effects of the present invention, and some embodiments may be applied, and it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the inventive concept of the present invention, and these embodiments are within the scope of the present invention.
Claims (7)
1. A preparation method of magnesium-based hydrogen storage material with high hydrogen storage density is characterized in that: comprises the following steps
(1) Placing the TiFe alloy in a sample chamber, vacuumizing at the high temperature of 600 ℃, and introducing 4-5 MPa hydrogen for pressure maintaining;
(2) repeating the step (1) for many times, and cooling to room temperature when the hydrogen pressure of the sample chamber is obviously reduced to obtain activated TiFe alloy particles;
(3) Mixing TiFe alloy particles with MgH 2 Mixing the raw materials in a ratio of 1: 10-1: 50, placing the mixture into a ball milling tank, sealing the ball milling tank, and vacuumizing the ball milling tank for 2 to 3 hours at 150 ℃ in a variable temperature ball milling device;
(4) introducing high-purity argon gas of 0.1-0.5 MPa into the ball milling tank, wherein the ball-material ratio is 30: 1, ball milling for 2-3 hours;
(5) cooling to below 100 ℃, introducing 0.1-0.5 MPa hydrogen and argon mixed gas into a ball milling tank, ball milling for 2-3 hours at 150 ℃, supplementing the hydrogen and argon mixed gas to 1-1.5 MPa after ball milling is stopped, and ball milling for 2-3 hours;
(6) vacuumizing at 200 ℃, introducing high-purity hydrogen with the pressure of 0.1-0.5 MPa, ball-milling for 2-3 hours, supplementing the high-purity hydrogen to the pressure of 1-1.5 MPa after ball-milling is stopped, and ball-milling for 2-3 hours to obtain MgH 2 -TiFe nano magnesium base high hydrogen storage density hydrogen storage material。
2. The method for preparing a magnesium-based hydrogen storage material with high hydrogen storage density as claimed in claim 1, wherein the time for evacuating in step (1) is 60 min.
3. The method of claim 1, wherein said substantial pressure drop in step (2) is a pressure drop of 0.5MPa in 30 minutes.
4. The method of claim 1, wherein the activated TiFe particles of step (2) are maintained in an atmosphere of high purity hydrogen for no more than 48 hours.
5. The method as claimed in claim 1, wherein the TiFe alloy particles activated in step (3) are placed in a ball mill pot through a glove box under argon atmosphere.
6. The method for preparing a magnesium-based hydrogen storage material with high hydrogen storage density as claimed in claim 1, wherein the ball milling rotation speed in step (4) is 300 rpm, and the ball milling temperature of the temperature-variable ball milling device is controlled by filling inert gas.
7. The method as claimed in claim 1, wherein the hydrogen-argon mixture in step (5) has a hydrogen content of 50% and an argon content of 50%.
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