Integrated device for preparing magnesium hydride powder and method for preparing magnesium hydride powder

Abstract

Provided is an integrated device for preparing magnesium hydride powder and a method for preparing magnesium hydride powder. The device comprises a heating chamber for heating a magnesium-based metal material to produce metal droplets; a powder-making chamber comprising an atomizing means used for atomizing the metal droplets which are then cooled to form a metal powder; and a reaction chamber used for performing a hydrogenation reaction on the metal powder to form the magnesium hydride powder. The device is an integrated structure monolithic with a simple structure and a convenient operation; and the entire process of preparing magnesium hydride powder can be completed in this single device and can realize automated control. The preparation method is simple and easy to operate and produces a product that has a moderate size, uniform particles, and excellent performance.

Claims

1. An integrated device for preparing magnesium hydride powder, characterized in that the device comprises: a heating chamber used for heating a magnesium-based metal material to produce metal droplets; a powder-making chamber comprising an atomizer used for atomizing the metal droplets which are then cooled to form a metal powder; and a reaction chamber used for performing a hydrogenation reaction on the metal powder to form the magnesium hydride powder; wherein the device further comprises a collection chamber between the powder-making chamber and the reaction chamber, and the collection chamber is used for collecting and screening the metal powder; a vibratile sieve is provided inside the collection chamber, wherein the sieve has a mesh aperture of 100-1000 mesh and vibrates for speeding up the screening of the metal powder by vibration of the sieve.

2. The device according to claim 1, characterized in that the heating chamber comprises a hatch cover, wherein when the hatch cover is opened, the heating chamber is in communication with the external environment, and the heating chamber can be charged from the external environment; and when the hatch cover is closed, the heating chamber is not in communication with the external environment.

3. The device according to claim 1, characterized in that the heating chamber is connected to a vacuum pump for evacuating the heating chamber.

4. The device of claim 3, characterized in that the heating chamber is further connected to an inert gas pipeline for charging the heating chamber with an inert gas.

5. The device of claim 4, characterized in that the inert gas is selected from one of or a combination of some of helium, neon, argon, krypton, and xenon.

6. The device according to claim 1, characterized in that the magnesium-based metal material is selected from one of or a combination of some of pure magnesium, a magnesium-nickel alloy, a magnesium-aluminum alloy, and a magnesium-rare earth alloy.

7. The device of claim 6, characterized in that the magnesium-nickel alloy, the magnesium-aluminum alloy, or the magnesium-rare earth alloy has a magnesium content between 60 wt % and 99.9 wt % and a content of other elements between 0.1 wt % and 40 wt %.

8. The device according to claim 1, characterized in that the heating chamber comprises a first container for containing the magnesium-based metal material.

9. The device of claim 8, characterized in that a heater is provided around and/or under the first container.

10. The device of claim 8, characterized in that the first container is connected to a droplet forming member for forming the metal droplets from the magnesium-based metal material melted or molten in the first container.

11. The device of claim 10, characterized in that the droplet forming member is connected to the bottom of the first container and has a tip with a diameter of 2-5 mm.

12. The device of claim 11, characterized in that the droplet forming member is a tip nozzle formed at the bottom of the first container.

13. The device according to claim 1, characterized in that the powder-making chamber further comprises a cooling system, and the atomizer atomizes the metal droplets by a high-pressure inert gas and the cooling system cools the metal droplets into the metal powder.

14. The device of claim 13, characterized in that the powder-making chamber is connected to a first duct, wherein one end of the first duct is disposed inside a cavity of the powder-making chamber and provided with the atomizer.

15. The device of claim 14, characterized in that the other end of the first duct is disposed outside the cavity of the powder-making chamber and connected to a gas outlet of a compressor, with the compressor being used for compressing the inert gas to form the high-pressure inert gas.

16. The device of claim 13, characterized in that the cooling system is a cooling water system sleeved around the cavity of the powder-making chamber, and the cooling water system has a cooling water inlet and a cooling water outlet which are arranged one above the other.

17. The device of claim 1, characterized in that the collection chamber comprises a first valve arranged between the powder-making chamber and the collection chamber, wherein when the first valve is opened, the collection chamber is in communication with the powder-making chamber; and when the first valve is closed, the collection chamber is isolated from the powder-making chamber.

18. The device of claim 17, characterized in that the first valve is located at the bottom of the powder-making chamber and the top of the collection chamber.

19. The device of claim 15, characterized in that a second duct is connected between the collection chamber and the compressor, a filter screen is provided on the second duct, and the filter screen is of at least 1600 mesh.

20. The device of claim 1, characterized in that the reaction chamber comprises a second valve arranged between the collection chamber and the reaction chamber, wherein when the second valve is opened, the collection chamber is in communication with the reaction chamber; and when the second valve is closed, the collection chamber is isolated from the reaction chamber.

21. The device of claim 20, characterized in that the reaction chamber comprises a hydrogen gas inlet that is connected to a hydrogen source.

22. The device of claim 1, characterized in that a thermal insulator is provided around the cavity of the reaction chamber, the thermal insulator comprises a heating resistance wire.

23. The device of claim 9, characterized in that the device further comprises a first control power supply that is connected to the heater.

24. The device of claim 22, characterized in that the device further comprises a second control power supply that is connected to the thermal insulator.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) FIG. 1 is a schematic structural view of an integrated device for preparing magnesium hydride powder according to a preferred embodiment of the present invention;

(2) FIG. 2 is an XRD chart of magnesium hydride powder prepared in a preferred embodiment of the present invention;

(3) FIG. 3 is a particle size distribution diagram of a sample powder prepared in a preferred embodiment of the present invention;

(4) FIG. 4 is an SEM photograph of a sample powder prepared in a preferred embodiment of the present invention;

(5) FIG. 5 is an SEM photograph of a sample powder prepared in a preferred embodiment of the present invention; and

(6) FIG. 6 is an SEM photograph of a sample powder prepared in a preferred embodiment of the present invention.

(7) In the drawings, 1—heating chamber, 11—hatch cover, 12—vacuum pump, 13—first container, 14—heating means, and 15—droplet forming member; 2—powder-making chamber, 21—first duct, 22—compressor, 23—cooling system, 24—cooling water outlet, 25—cooling water inlet, and 26—atomizing means; 3—collection chamber, 31—first valve, 32—sieve, 33—filter screen, and 34—second duct; and 4—reaction chamber, 41—second valve, 42—hydrogen gas inlet, and 43—thermal insulation means.

DETAILED DESCRIPTION OF EMBODIMENTS

(8) The embodiments of the present invention are described in detail below. The following embodiments are implemented on the premise of the technical solutions of the present invention, and detailed embodiments and specific operation procedures are given; however, the scope of protection of the present invention is not limited to the following embodiments.

(9) FIG. 1 is a schematic structural view of an integrated device for preparing magnesium hydride powder according to a preferred embodiment of the present invention, the device comprising a heating chamber 1, a powder-making chamber 2, a collection chamber 3, and a reaction chamber 4.

(10) In the device, the heating chamber 1 is used for heating a magnesium-based metal material to produce metal droplets of the magnesium-based metal material. The heating chamber comprises a hatch cover 11 arranged on the top of the heating chamber 1. The heating chamber 1 is connected to a vacuum pump 12 for evacuating the heating chamber 1. The heating chamber 1 is further connected to an inert gas pipeline (not shown in the figure) for charging the heating chamber 1 with an inert gas. The heating chamber 1 further comprises a first container 13, wherein the first container 13 is a crucible for containing the magnesium-based metal material. A heating means 14 is provided around the first container 13, and the heating means 14 is an induction or resistance heating coil used for heating the magnesium-based metal material. The first container 13 is further connected to a droplet forming member 15 for forming the metal droplets from the magnesium-based metal material melted or molten in the first container 13. The droplet forming member 15 is a tip nozzle formed at the bottom of the first container 13, that is, the first container 13 is a crucible with a tip nozzle at the bottom.

(11) The powder-making chamber 2 is used for forming the metal droplets of the magnesium-based metal material into a metal powder. The powder-making chamber 2 is connected to a first duct 21, with one end of the first duct 21 being located inside a cavity of the powder-making chamber 2, and is provided with an atomizing means 26, which is a tip nozzle, wherein the atomizing means 26 is arranged near, and below and on one side of, the droplet forming member 15, so that the high-pressure inert gas blown out therefrom atomizes the metal droplets dripping from the tip of the droplet forming member 15. The direction pointed by the tip nozzle of the first duct 21 and the direction pointed by the tip of the droplet forming member 15 are perpendicular to each other. The other end of the first duct 21 is disposed outside the cavity of the powder-making chamber 2 and connected to a gas outlet of a compressor 22, with the compressor 22 being used for compressing the inert gas to form the high-pressure inert gas. Where the inert gas is argon, the compressor 22 is an argon compressor. A cooling system 23 is comprised around the cavity of the powder-making chamber 2 to condense the atomized metal droplets into a metal powder. The cooling system 23 is a cooling water system sleeved around the cavity of the powder-making chamber 2, and the cooling water system 23 has a cooling water outlet 24 and a cooling water inlet 25, wherein the cooling water outlet 24 is above and the cooling water inlet 25 is below.

(12) The collection chamber 3 is used for screening and collecting the metal powder formed in the powder-making chamber 2 so as to obtain a metal powder within a specified particle size range, thereby making the particle size of the prepared magnesium hydride powder more uniform. The collection chamber 3 comprises a first valve 31, wherein the first valve 31 is arranged between the powder-making chamber 2 and the collection chamber 3 and is located at the bottom of the powder-making chamber 2 and the top of the collection chamber 3. A vibratile sieve 32 is provided inside the collection chamber 3 for screening the metal powder obtained in the powder-making chamber in order to obtain magnesium powder within a specified particle size range. The sieve 32 divides the collection chamber 3 into upper and lower parts, wherein powder with a particle size larger than the mesh aperture is left in the upper part of the sieve 32, while powder with a particle size smaller than the mesh aperture can fall through the sieve aperture to the lower part of the sieve 32. The sieve 32 is provided with a vibrating means, which can speed up the screening of the powder by vibrating the sieve 32. A second duct 34 is connected between the collection chamber 3 and the compressor 22 for recovering and recycling the inert gas. Therefore, the inert gas can form a cycle of “the gas outlet of the compressor 22—the first duct 21—the powder-making chamber 2—the collection chamber 3—the second duct 34—the gas inlet of the compressor 22”, so that the pressure of the inert gas in the powder-making chamber 2 and the collection chamber 3 can be adjusted by adjusting the gas inlet and outlet of the compressor 22. The second duct 34 is provided with a filter screen 33 for filtering out the metal powder from the inert gas before entering the gas inlet of the compressor 22. The filter screen 33 is installed at an end of the second duct 34, which is connected to the collection chamber 3, and is located on a side of the collection chamber 3.

(13) The reaction chamber 4 is used for hydrogenating the metal powder within the specified particle size range obtained in the collection chamber 3 to form magnesium hydride powder. The reaction chamber 4 comprises a second valve 41, wherein the second valve 41 is arranged between the collection chamber 3 and the reaction chamber 4 and is located at the bottom of the collection chamber 3 and the top of the reaction chamber 4. The reaction chamber 4 comprises a hydrogen gas inlet 42, wherein the hydrogen gas inlet 42 is connected to a hydrogen source (not shown in the figure) used for supplying hydrogen required for the reaction of hydrogenating the magnesium powder into magnesium hydride to the reaction chamber 4 and forming a hydrogen pressure. The hydrogen gas inlet 42 is arranged on a side wall of a cavity of the reaction chamber 4. A thermal insulation means 43 is further provided around the cavity of the reaction chamber 4, and the thermal insulation means comprises a heating resistance wire used for providing the temperature required for the reaction of hydrogenating the magnesium powder into magnesium hydride.

(14) The structure of an integrated device for preparing magnesium hydride powder according to a preferred embodiment of the present invention has been described above. Based on this device, the method for preparing magnesium hydride powder of the present invention will be illustrated below in detail using different embodiments.

Embodiment 1

(15) In this embodiment, the method for preparing magnesium hydride powder using the above-mentioned integrated device involves:

(16) (a) opening the hatch cover 11 on the top of the heating chamber 1, putting a magnesium-nickel alloy raw material block (in which the content of nickel is 5 wt %) into the graphite crucible of the first container 13, and closing the hatch cover 11; evacuating the heating chamber 1, charging same with argon, and repeating once; and evacuating same again to a vacuum of 10.sup.−3 Pa, then charging the heating chamber 1 with 0.06 MPa argon, and heating the graphite crucible to 800° C. by controlling the heating means 14 so that the magnesium-nickel alloy raw material in the crucible is melted to form a molten metal;

(17) (b) allowing the molten metal to flow out through the tip nozzle at the bottom of the crucible into the powder-making chamber 2 in which the molten metal is atomized into powder droplets by a 5 MPa high-pressure argon gas and cooled into a metal powder under the action of 2 MPa circulating cooling water at 20° C.;

(18) (c) allowing the metal powder to fall through the bottom of the powder-making chamber 2 on the 400 mesh vibratile sieve 32 in the collection chamber 3; and

(19) (d) after the sieved powder falls into the reaction chamber 4, closing the second valve 41, maintaining the reaction chamber 4 at 360° C., and introducing 3 MPa hydrogen to start hydrogenation; and after the hydrogenation is completed over 10 h, collecting the product magnesium hydride powder from the reaction chamber 4.

(20) An XRD test is carried out on the powder prepared in this embodiment, and as shown in FIG. 2, there are clear and complete MgH.sub.2 crystal surface characteristic peaks and a small number of Mg characteristic peaks, indicating that only a small amount of Mg is not hydrogenated and the prepared magnesium hydride powder has a higher purity, that is, the MgH.sub.2 content thereof is high.

(21) A nano-particle size test is carried out on the powder prepared in this embodiment, and as shown in FIG. 3, the yield of powder with a particle size of 11.25 μm or less reaches 94%, the volume average particle size of the particles is 7.87 μm, and the particle size consistency is relatively high.

(22) In addition, the morphology of the powder prepared in this embodiment is observed using SEM, and as shown in FIGS. 4 and 5, the powder is shown to be more uniform and have a good sphericity.

Embodiment 2

(23) The method for preparing magnesium hydride powder in this embodiment is basically the same as that in Embodiment 1, only except that:

(24) the raw material block placed in step (a) is a magnesium-aluminum alloy (in which the content of aluminum is 3 wt %), and the heating temperature is 650° C.;

(25) the inert gases used in step (a) and step (b) are helium, the pressure of the heating chamber 1 is 0.05 MPa, and the pressure of the high-pressure helium is 1 MPa;

(26) the circulating cooling water in step (b) has a temperature of 50° C. and a pressure of 0.5 MPa; and

(27) in step (d), the hydrogen pressure is 1 MPa, the hydrogenation temperature is 400° C., and the hydrogenation time is 20 h.

(28) Compared with Embodiment 1, the powder prepared in this embodiment is all spherical magnesium hydride powder with a uniform size and a complete morphology, as shown in FIG. 6.

Embodiment 3

(29) The method for preparing magnesium hydride powder in this embodiment is basically the same as that in Embodiment 1, only except that:

(30) the raw material block placed in step (a) is pure magnesium metal, and the heating temperature is 1100° C.;

(31) the inert gases used in step (a) and step (b) are argon, the pressure of the heating chamber 1 is 0.15 MPa, and the pressure of the high-pressure argon is 15 MPa;

(32) the sieve in step (c) is of 200 mesh; and

(33) in step (d), the hydrogen pressure is 5 MPa, the hydrogenation temperature is 200° C., and the hydrogenation time is 40 h.

(34) By comparing the powder prepared in this embodiment with that of Embodiment 1, the prepared magnesium hydride powder also has a higher level of purity, that is, the content of MgH.sub.2 in the product is high, a higher particle diameter consistency, a rational size distribution, and a complete spherical morphology.

(35) The preferred embodiments of the present invention have been described in detail above. It should be understood that a person of ordinary skill in the art would be able to make various modifications and variations according to the concept of the present invention without involving any inventive effort. Therefore, any technical solutions that can be obtained by a person skilled in the art based on the prior art according to the concept of the present invention through logical analysis, reasoning, or limited trials should all be within the scope of protection determined by the claims.