CN114309629A - Gas-solid two-phase atomization method for superfine spherical hydrogen storage metal or alloy powder thereof - Google Patents
Gas-solid two-phase atomization method for superfine spherical hydrogen storage metal or alloy powder thereof Download PDFInfo
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Abstract
The invention discloses a gas-solid two-phase atomization method of micro spherical hydrogen storage metal or alloy powder thereof, which comprises the following steps: s1, fluidizing the hydrogen-absorbed hydrogen storage metal or alloy particles thereof, and then forming a gas-solid two-phase flow with inert gas; s2, the formed gas-solid two-phase flow is used for impacting and atomizing the hydrogen storage metal solution or the alloy solution thereof, and the solid phase in the gas-solid two-phase flow is rushed into the hydrogen storage metal solution or the alloy solution thereof for dehydrogenation and explosion; s3, cooling the fine molten drops after dehydrogenation and explosion in inert gas to obtain fine spherical powder of hydrogen storage metal or alloy thereof; and the solid phase component in the gas-solid two-phase flow is the same as the hydrogen storage metal solution or the alloy solution component thereof; compared with the prior art, the obtained spherical powder has fine granularity, high nodularity and no dirtying powder, and the process flow is simplified.
Description
Technical Field
The invention relates to the technical field of powder material preparation, in particular to a gas-solid two-phase atomization method of superfine spherical hydrogen storage metal or alloy powder thereof.
Background
As one of the marking technologies of the third industrial revolution, additive manufacturing technology has had a great impact in the global manufacturing field. The fine metal spherical powder is a material basis of a metal additive manufacturing industry chain and also has the greatest value, and the cost and the performance of the fine metal spherical powder become one of bottlenecks which restrict the rapid and healthy development of the industry. The metal powder for additive manufacturing needs to meet the requirements of high purity, high sphericity, fine particle size, narrow particle size distribution and the like. Therefore, the innovation of the preparation technology and the process of the fine spherical metal powder becomes a hot point of domestic and foreign research.
The atomization method is the most mature and widely applied method for preparing spherical metal powder. The method is a preparation method which uses a fast moving fluid (atomizing medium) to impact a metal melt, so that the kinetic energy of the fluid is converted into melt surface energy, the metal or alloy melt is crushed into fine liquid drops, and the liquid drops are rapidly condensed into solid powder. The metal powder prepared by the atomization method achieves good effects in the aspects of sphericity and fluidity, and is widely applied to the field of preparation of active material powder such as titanium alloy and the like. However, in the actual production process, the main disadvantage of the atomization method is that the yield of fine powder of 15-53 μm is low, especially in the aspect of titanium alloy powder preparation, the yield of fine powder generally does not exceed 25%, and the productivity needs to be further improved.
In order to solve this problem and improve the yield of fine powder, some researchers have proposed a new atomization technique, such as a gas-solid two-phase atomization technique, by considering improvement in the selection of the atomization medium. The gas-solid two-phase atomization technology is a novel atomization mode which changes the composition of an atomization medium in the atomization process, namely solid particles are added into atomization gas to form solid-gas two-phase flow, and the melt is fully crushed to obtain fine metal powder.
For example: patent document No. cn01106868.x discloses a solid atomization method of liquid metal and alloy, which atomizes the liquid metal or alloy by high-speed airflow containing high-concentration soluble solid medium particles, and separates the solid particles from metal powder by water washing, filtering and drying. The invention particularly teaches that the solid phase medium should be a solid medium which is easily separable from and non-fouling of the powder, solid particles having relatively high thermal capacity and thermal conductivity, such as NaCl, KCl, urea and other water soluble organic or inorganic substances, and compressed air or a high pressure inert gas, such as nitrogen, as the carrier gas stream for the solid atomized medium particles. However, the gas-solid two-phase flow adopted by the method is not suitable for atomization of high-activity hydrogen storage metal and alloy (such as titanium, zirconium and alloys thereof) powder, whether the gas-solid two-phase flow is a solid phase (such as NaCl, KCl, urea and other organic or inorganic substances capable of being dissolved in water) or a gas phase (compressed air or high-pressure nitrogen), and has the problem of dirtying the powder.
In addition, in the research on the process for preparing fine stainless steel powder by atomizing solid-gas two-phase flow of su bin, the same atomizing technology is adopted, that is, powder with the same component as the atomized alloy is used as a solid medium to crush the molten metal under the action of the solid-gas two-phase flow. The method has the advantages that the solid medium with the same components does not dirty powder, and the solid medium for atomization can be recycled. The method has the defects that compared with solid salt atomized powder, the powder obtained by the same atomization technology has larger particle size, and the prepared stainless steel powder body needs to be subjected to secondary screening separation on coarse particles, so that the workload is increased. Finally, there is no example of the same atomization technique being applied to the field of high-activity hydrogen storage metals or alloys thereof.
In summary, the existing gas-solid two-phase atomization method cannot be applied to the preparation of high-activity metal and alloy spherical powder represented by titanium and titanium alloy, the yield of fine powder cannot be remarkably improved, and the process flow is more complicated compared with the traditional gas atomization.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a gas-solid two-phase atomization method of superfine spherical hydrogen storage metal or alloy powder thereof, and aims to solve the problems that the existing gas-solid two-phase atomization method cannot be applied to the preparation of high-activity metal represented by titanium and titanium alloy and alloy spherical powder thereof, the yield of fine powder cannot be remarkably improved, and the process flow is relatively complicated in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: a gas-solid two-phase atomization method of superfine spherical hydrogen storage metal or alloy powder thereof comprises the following steps:
s1, fluidizing the hydrogen-absorbed hydrogen storage metal or alloy particles thereof, and then forming a gas-solid two-phase flow with inert gas;
s2, the formed gas-solid two-phase flow is used for impacting and atomizing the hydrogen storage metal solution or the alloy solution thereof, and the solid phase in the gas-solid two-phase flow is rushed into the hydrogen storage metal solution or the alloy solution thereof for dehydrogenation and explosion;
s3, cooling the fine molten drops after dehydrogenation and explosion in inert gas to obtain fine spherical powder of hydrogen storage metal or alloy thereof;
and the solid phase component in the gas-solid two-phase flow is the same as the hydrogen storage metal solution or the alloy solution component thereof.
Furthermore, the solid phase in the gas-solid two-phase flow is prepared by hydrogenation and crushing, and the particle size range of the solid phase is 10-1000 μm.
Further, the solid phase particle size range in the gas-solid two-phase flow is 100-300 μm.
Further, the hydrogen storage metal is a metal simple substance capable of forming metal coordination hydride, and the metal simple substance comprises titanium, vanadium, niobium or zirconium.
Further, the hydrogen storage metal alloy is AxByThe hydrogen storage alloy includes titanium-based hydrogen storage alloy, zirconium-based hydrogen storage alloy, iron-based hydrogen storage alloy or rare earth-based hydrogen storage alloy.
Furthermore, the superheat degree of the hydrogen storage metal melt is 150K-200K above the melting point of the corresponding metal, and the superheat degree of the hydrogen storage metal alloy melt is 100K-120K above the melting point of the corresponding metal alloy.
Further, the inert gas is nitrogen, argon or helium.
Further, the inert gas is argon.
Further, the temperature of the gas-solid two-phase flow is 100-150 ℃.
Further, in the step S2, the mass ratio of the falling melt liquid flow in unit time to the solid phase particles in the gas-solid two-phase flow is 1: 0.1-3.
Compared with the prior art, the invention has the following beneficial effects:
(1) compared with the traditional gas atomization technology, the gas-solid two-phase flow has higher kinetic energy, the energy conversion rate and the atomization crushing efficiency are improved, the granularity of the prepared spherical powder is finer, and the yield of fine powder with the granularity range of 15-53 mu m reaches more than 80%;
(2) in the invention, the gas phase in the gas-solid two-phase flow is inert gas, and the solid phase has the same components as the atomized hydrogen storage metal solution or the atomized hydrogen storage metal solution, so the defect of dirtying the final product is avoided;
(3) the hydrogen-absorbing and storing metal or alloy particles thereof can be broken and refined under the action of high temperature of the melt, and the obtained product powder does not need to be screened again for separation, thereby simplifying the powder-making operation process;
(4) the solid phase in the gas-solid two-phase flow can be heated, decomposed and exploded and simultaneously releases gas in the process of impacting the melt, and the explosion phenomenon can reduce the particle size of solid phase particles in the gas-solid two-phase flow on one hand and promote the melt to be further atomized and crushed on the other hand, so that finer molten drops can be obtained. Both factors contribute to the improvement of the proportion of fine powder.
Drawings
FIG. 1 is a gas-solid two-phase atomization diagram of hydrogen absorption and storage metal or alloy thereof in the invention;
FIG. 2 is a schematic view of a fine spherical Ti powder prepared in example 1 of the present invention;
FIG. 3 is a schematic view of a fine spherical Ti-6Al-4V powder prepared in example 2 of the present invention.
Detailed Description
The present invention will be described in further detail below by way of specific embodiments:
a gas-solid two-phase atomization method of superfine spherical hydrogen storage metal or alloy powder thereof comprises the following steps:
1. selecting high-purity hydrogen storage metal or alloy thereof (the alloy is referred to as hydrogen storage metal alloy in the application) as a raw material, wherein the hydrogen storage metal is a metal simple substance such as titanium, vanadium, niobium, zirconium and the like capable of forming metal coordination hydride; the hydrogen storage metal alloy is AxByThe hydrogen storage alloy can be AB5Type AB, type AB2Form A or2The B-type hydrogen-absorbing alloy may specifically beIs a titanium-based hydrogen storage alloy, a zirconium-based hydrogen storage alloy, an iron-based hydrogen storage alloy or a rare earth-based hydrogen storage alloy. The purity of the hydrogen storage metal or the alloy thereof is more than or equal to 99.99 percent in mass fraction;
2. carrying out high-temperature hydrogenation on the hydrogen storage metal or the alloy thereof in the atmosphere of high-purity hydrogen to obtain hydrogen absorption and storage metal or the alloy thereof;
3. crushing the hydrogenated hydrogen storage metal or alloy thereof in a high-purity argon atmosphere, wherein the particle size range of the crushed hydrogen storage metal or alloy is 10-1000 microns, and preferably 100-300 microns;
4. high-temperature inert gas is adopted, and can be nitrogen, argon or helium, and argon is preferred; fluidizing the crushed hydrogen storage metal or alloy particles thereof to form a gas-solid two-phase flow with the temperature of 100-150 ℃;
5. melting the hydrogen storage metal or the alloy thereof by adopting an arc melting or induction melting method to form a melt, wherein the superheat degree of the hydrogen storage metal melt is 120-150K above the melting point of the corresponding metal, and the superheat degree of the hydrogen storage metal alloy melt is 100-120K above the melting point of the corresponding metal alloy;
6. injecting the hydrogen storage metal melt or the metal alloy melt into an atomizing chamber, and impacting a melt liquid flow by using high-temperature gas-solid two-phase flow, wherein the dynamic pressure of the gas-solid two-phase flow is 0.5-3.0 MPa, and the mass ratio of the atomized melt liquid flow in unit time to solid phase particles in the gas-solid two-phase flow is 1: 0.1-3;
7. the melt liquid flow is broken under the common impact action of inert gas and hydrogen-absorbing solid-phase particles, the gas-solid two-phase flow atomizes the melt by means of the kinetic energy of the gas-solid two-phase flow, the hydrogen-absorbing solid-phase particles are directly flushed into the melt under the drive of the gas flow, the hydrogen is rapidly removed and exploded under the action of high temperature of the melt, the melt wrapped or attached on the particles is further torn, and finer molten drops are formed. Hydrogen-absorbing solid-phase particles are exploded and hydrogen elements contained in the hydrogen-absorbing solid-phase particles are removed at the same time, so that finer powder is formed and is wrapped by melt adhered to the hydrogen-absorbing solid-phase particles to form a sphere;
8. the atomized and exploded spherical molten drops are cooled in inert atmosphere to form fine spherical hydrogen storage metal or alloy powder thereof, and the yield of fine powder of the fine spherical powder in the range of 15-53 mu m can reach more than 80%.
The invention takes hydrogen storage metal or alloy thereof as raw material, and utilizes the mixing acceleration of hydrogen absorption and storage metal or alloy particles thereof and high-temperature inert gas to form high-temperature gas-solid two-phase flow to impact the hydrogen storage metal or alloy melt thereof, thereby not only realizing the high-efficiency atomization of the melt, but also realizing the dehydrogenation and refinement of the hydrogen absorption and storage metal or alloy thereof, and the yield of the collected fine powder of the final product reaches more than 80 percent, and the problem of dirtying the final product does not exist.
Example 1
The gas-solid two-phase atomization method is adopted to prepare pure titanium spherical powder
(1) The sponge titanium with the purity of more than or equal to 99.99 (wt%) is taken as a raw material, hydrogen with the purity of more than or equal to 99.995 (wt%) is used for carrying out hydrogen permeation on the sponge titanium to obtain titanium hydride, and the titanium hydride is crushed to the granularity of 50-200 mu m in the argon atmosphere;
(2) sponge titanium with the purity of more than or equal to 99.99 (wt%) is used as a raw material, the sponge titanium is melted into a titanium melt by adopting an electric arc melting method, and the melt temperature is 1810 +/-10 ℃;
(3) fluidizing titanium hydride particles by using high-temperature argon gas to obtain a gas-solid two-phase flow containing the titanium hydride particles, wherein the temperature of the gas-solid two-phase flow is 120 ℃;
(4) pressurizing the gas-solid two-phase flow to 1.2MPa, atomizing the titanium melt, wherein the mass ratio of the liquid flow mass of the titanium melt falling into the atomizing chamber in unit time to solid phase particles (titanium hydride) in the gas-solid two-phase flow is 1: 1;
(5) the titanium melt liquid flow is broken under the common impact action of argon and titanium hydride particles, while the two-phase flow consisting of argon and titanium hydride atomizes the melt by means of the self kinetic energy, the titanium hydride solid phase particles can be directly flushed into the titanium melt under the drive of the argon flow, and are rapidly dehydrogenated and exploded under the high-temperature action of the titanium melt, so that the titanium melt wrapped or attached on the titanium hydride particles is further torn to form finer titanium melt drops; the titanium hydride particles are also exploded and simultaneously remove hydrogen elements contained in the titanium hydride particles to form finer titanium powder, and the titanium powder is wrapped by the titanium melt adhered on the titanium powder to form a spherical shape;
(6) cooling the atomized and exploded spherical titanium molten drops in an argon inert atmosphere to form fine spherical titanium powder, wherein the yield of fine powder of the fine spherical powder in the range of 15-53 mu m is 83 percent.
Example 2
The gas-solid two-phase atomization method is adopted to prepare Ti-6Al-4V spherical powder
(1) Using Ti-6Al-4V with the purity of more than or equal to 99.99 (wt%) as a raw material, carrying out hydrogen permeation on the Ti-6Al-4V by using hydrogen with the purity of more than or equal to 99.995 (wt%) to obtain hydrogenated Ti-6Al-4V, and crushing the hydrogenated Ti-6Al-4V to the particle size of 150-500 mu m under the argon atmosphere;
(2) taking a Ti-6Al-4V bar with the purity of more than or equal to 99.99 (wt%) as a raw material, melting Ti-6Al-4V into a melt by an induction melting method, wherein the melt temperature is 1780 +/-10 ℃;
(3) fluidizing the hydrogenated Ti-6Al-4V particles by using high-temperature argon to obtain a gas-solid two-phase flow containing the hydrogenated Ti-6Al-4V particles, wherein the temperature of the gas-solid two-phase flow is 125 ℃;
(4) pressurizing the gas-solid two-phase flow to 1.5MPa, atomizing the Ti-6Al-4V melt, wherein the mass ratio of the liquid flow quality of the Ti-6Al-4V melt falling into an atomizing chamber in unit time to solid phase particles (Ti-6Al-4V titanium) in the gas-solid two-phase flow is 1: 1.5;
(5) the Ti-6Al-4V melt flow is crushed under the common impact action of argon and hydrogenated Ti-6Al-4V particles, two-phase flow consisting of the argon and the hydrogenated Ti-6Al-4V atomizes the melt by means of self kinetic energy, the hydrogenated Ti-6Al-4V solid-phase particles are directly flushed into the Ti-6Al-4V melt under the driving of argon flow, and are rapidly dehydrogenated and exploded under the action of high temperature of the Ti-6Al-4V melt, and the Ti-6Al-4V melt wrapped or attached on the hydrogenated Ti-6Al-4V particles is further torn to form finer Ti-6Al-4V melt drops; the hydrogenated Ti-6Al-4V particles are also exploded and simultaneously remove hydrogen elements contained in the particles to form finer Ti-6Al-4V powder which is wrapped by the Ti-6Al-4V melt adhered on the powder to form a sphere;
(6) cooling the atomized and exploded spherical Ti-6Al-4V molten drops in an argon inert atmosphere to form fine spherical Ti-6Al-4V powder, wherein the yield of fine powder of the fine spherical powder in the range of 15-53 mu m reaches 85%.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (10)
1. A gas-solid two-phase atomization method of superfine spherical hydrogen storage metal or alloy powder thereof is characterized by comprising the following steps:
s1, fluidizing the hydrogen-absorbed hydrogen storage metal or alloy particles thereof, and then forming a gas-solid two-phase flow with inert gas;
s2, the formed gas-solid two-phase flow is used for impacting and atomizing the hydrogen storage metal solution or the alloy solution thereof, and the solid phase in the gas-solid two-phase flow is rushed into the hydrogen storage metal solution or the alloy solution thereof for dehydrogenation and explosion;
s3, cooling the fine molten drops after dehydrogenation and explosion in inert gas to obtain fine spherical powder of hydrogen storage metal or alloy thereof;
and the solid phase component in the gas-solid two-phase flow is the same as the hydrogen storage metal solution or the alloy solution component thereof.
2. The gas-solid two-phase atomization method of the fine spherical hydrogen storage metal or alloy powder thereof according to claim 1, characterized in that: the solid phase in the gas-solid two-phase flow is prepared by hydrogenation and crushing, and the particle size range is 10-1000 mu m.
3. The gas-solid two-phase atomization method of the fine spherical hydrogen storage metal or alloy powder thereof according to claim 2, characterized in that: the solid phase particle size range in the gas-solid two-phase flow is 100-300 mu m.
4. The gas-solid two-phase atomization method of the fine spherical hydrogen storage metal or alloy powder thereof according to claim 1, characterized in that: the hydrogen storage metal is a metal simple substance capable of forming metal coordination hydride, and the metal simple substance comprises titanium, vanadium, niobium or zirconium.
5. The gas-solid two-phase atomization method of the fine spherical hydrogen storage metal or alloy powder thereof according to claim 1, characterized in that: the hydrogen storage metal alloy is AxByThe hydrogen storage alloy includes titanium-based hydrogen storage alloy, zirconium-based hydrogen storage alloy, iron-based hydrogen storage alloy or rare earth-based hydrogen storage alloy.
6. The gas-solid two-phase atomization method of the fine spherical hydrogen storage metal or alloy powder thereof according to claim 1, characterized in that: the superheat degree of the hydrogen storage metal melt is 150-200K above the melting point of the corresponding metal, and the superheat degree of the hydrogen storage metal alloy melt is 100-120K above the melting point of the corresponding metal alloy.
7. The gas-solid two-phase atomization method of the fine spherical hydrogen storage metal or alloy powder thereof according to claim 1, characterized in that: the inert gas is nitrogen, argon or helium.
8. The gas-solid two-phase atomization method of the fine spherical hydrogen storage metal or alloy powder thereof according to claim 7, characterized in that: the inert gas is argon.
9. The gas-solid two-phase atomization method of the fine spherical hydrogen storage metal or alloy powder thereof according to claim 1, characterized in that: the temperature of the gas-solid two-phase flow is 100-150 ℃.
10. The gas-solid two-phase atomization method of the fine spherical hydrogen storage metal or alloy powder thereof according to claim 1, characterized in that: in the step S2, the mass ratio of the falling melt liquid flow in unit time to the solid phase particles in the gas-solid two-phase flow is 1: 0.1-3.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5147448A (en) * | 1990-10-01 | 1992-09-15 | Nuclear Metals, Inc. | Techniques for producing fine metal powder |
| JPH08120365A (en) * | 1994-10-19 | 1996-05-14 | Sanyo Electric Co Ltd | Hydrogen storage alloy and its production |
| US6398125B1 (en) * | 2001-02-10 | 2002-06-04 | Nanotek Instruments, Inc. | Process and apparatus for the production of nanometer-sized powders |
| CN1369339A (en) * | 2001-02-13 | 2002-09-18 | 中南大学 | Solid atomizing process for molten metal and alloy |
| CN108015295A (en) * | 2017-12-29 | 2018-05-11 | 北京康普锡威科技有限公司 | A kind of preparation method of increasing material manufacturing metal-based nano composite powder material |
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- 2021-12-28 CN CN202111626013.6A patent/CN114309629A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5147448A (en) * | 1990-10-01 | 1992-09-15 | Nuclear Metals, Inc. | Techniques for producing fine metal powder |
| JPH08120365A (en) * | 1994-10-19 | 1996-05-14 | Sanyo Electric Co Ltd | Hydrogen storage alloy and its production |
| US6398125B1 (en) * | 2001-02-10 | 2002-06-04 | Nanotek Instruments, Inc. | Process and apparatus for the production of nanometer-sized powders |
| CN1369339A (en) * | 2001-02-13 | 2002-09-18 | 中南大学 | Solid atomizing process for molten metal and alloy |
| CN108015295A (en) * | 2017-12-29 | 2018-05-11 | 北京康普锡威科技有限公司 | A kind of preparation method of increasing material manufacturing metal-based nano composite powder material |
Non-Patent Citations (1)
| Title |
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| 陈刚, 苏斌, 陈鼎, 张福全, 陈振华: "气固两相流雾化法制备微细不锈钢粉末", 中国有色金属学报, no. 04, pages 584 - 589 * |
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