CN115974133A - High-purity beta gallium oxide nano-microspheres and preparation method thereof - Google Patents
High-purity beta gallium oxide nano-microspheres and preparation method thereof Download PDFInfo
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- 229910001195 gallium oxide Inorganic materials 0.000 title claims abstract description 54
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000004005 microsphere Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 43
- 239000000725 suspension Substances 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 238000001556 precipitation Methods 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 14
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 12
- 239000012498 ultrapure water Substances 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- 239000002244 precipitate Substances 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 239000002077 nanosphere Substances 0.000 claims 9
- 239000000843 powder Substances 0.000 description 17
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- -1 oxygen ions Chemical class 0.000 description 6
- 238000005118 spray pyrolysis Methods 0.000 description 6
- 239000013077 target material Substances 0.000 description 6
- 238000000889 atomisation Methods 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 241001089723 Metaphycus omega Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(iii) oxide Chemical compound O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The invention discloses a high-purity beta gallium oxide nano microsphere and a preparation method thereof, wherein metal Ga and ultrapure water are mixed to obtain a mixed solution, a hydrothermal reaction is carried out to obtain a gallium oxyhydroxide precipitation suspension A, the solid-to-liquid ratio of the gallium oxyhydroxide precipitation suspension A is adjusted to obtain a gallium oxyhydroxide precipitation suspension B, the gallium oxyhydroxide precipitation suspension B is conveyed into an atomizing nozzle under continuous stirring, atomized gas medium is atomized into liquid drops, and the liquid drops are spheroidized by plasma to obtain the high-purity beta gallium oxide nano microsphere. The high-purity beta gallium oxide nano-microspheres prepared by the preparation method provided by the invention have the purity of more than or equal to 5N, narrow particle size distribution, high sphericity and excellent fluidity and dispersibility.
Description
Technical Field
The invention relates to a high-purity beta gallium oxide nano microsphere and a preparation method thereof, belonging to the technical field of semiconductor material preparation.
Background
Gallium oxide (Ga) 2 O 3 ) Is an important wide bandgap semiconductor material, which has five crystal structures: alpha-Ga 2 O 3 、β-Ga 2 O 3 、γ-Ga 2 O 3 、ε-Ga 2 O 3 And delta-Ga 2 O 3 And can be mutually converted under certain conditions. Wherein beta-Ga 2 O 3 Is most stable, has a monoclinic structure at room temperature, has a spatial structure of C2/m,
β＝103.83°。Ga 2 O 3 has the characteristics of excellent photoluminescence performance, chemical and thermal stability and the like,it can be widely used in the fields of sensitive materials, catalysts, photoelectronic materials, fluorescent powder, etc.
In recent years, IGZO (indium gallium zinc oxide) is applied to the field of TFT-LCD displays, so that the number of transistors is reduced, the light transmittance of each pixel is improved, and the display has a higher energy efficiency level and higher efficiency. At present, a radio frequency/direct current (RF/DC) sputtering system is the mainstream film growth equipment, and factors influencing the quality of the sputtered transparent conductive film play a crucial role in the density, conductivity, grain size, microstructure and purity of the target besides the film deposition process. For example, the density of the target material is low, that is, micropores are formed on the surface or inside of the target material, and protrusions are formed on the surface of the target material in the coating process, which causes the local energy of the target material to be too high, and oxygen ions are impacted into a free state to form a high-resistance region, so that some microparticles enter the film, the quality of the film is reduced, and the stability of the coating is affected.
Currently, IGZO sputtering target materials sold In commercial markets are mainly sintered by solid-phase reaction hot pressing, and In is prepared by 2 O 3 ZnO and Ga 2 O 3 Mixing the three kinds of powder according to a certain proportion, ball-milling and homogenizing, hot-pressing and sintering and the like to prepare the IGZO target material for sputtering. The preparation method is simple to operate, but the uniformity of mechanical ball milling mixing is influenced by the granularity and the morphology of each powder. In 2 O 3 ZnO and Ga 2 O 3 The granularity, the shape, the fluidity and the dispersity of the powder play a decisive role in the homogenizing effect and the hot pressing process.
Chinese patent application CN107010654B discloses a method for preparing monodisperse gallium oxide powder and a high-density ceramic target thereof. The invention uses more than 99.99% of metal gallium to dissolve in acid, then ammonia water is added for precipitation and aging to obtain white precipitate, and the product is obtained by washing, filtering, drying, calcining and other working procedures. However, the method has high calcination temperature, the obtained product microscopic particles are easy to agglomerate, and the product uniformity is reduced.
Chinese patent application CN106744730A discloses a two-step method for preparing gallium oxide and gallium nitride nano powder by using metal gallium as raw material, adopting metal Ga and water according to the mass ratio of 1: 2-10, making them produce reaction in high-pressure reaction still at 180-280 deg.C to obtain hydroxyl gallium oxide, then heating and decomposing hydroxyl gallium oxide in the air at 400-800 deg.C so as to obtain gallium oxide nano powder whose grain size is 10-20 nm.
However, the nano-sized gallium oxide particles prepared by the prior art are not spherical, and the obtained gallium oxide particles can not meet the requirements of fluidity and dispersibility.
Disclosure of Invention
Aiming at the defects of the prior art, the first purpose of the invention is to provide a preparation method of high-purity beta gallium oxide nano microspheres.
The second purpose of the invention is to provide the high-purity beta gallium oxide nano-microsphere prepared by the preparation method.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a preparation method of high-purity beta gallium oxide nano microspheres, which comprises the steps of mixing metal Ga with ultrapure water to obtain a mixed solution, carrying out hydrothermal reaction to obtain a gallium oxyhydroxide precipitation suspension A, adjusting the solid-to-liquid ratio of the gallium oxyhydroxide precipitation suspension A to obtain a gallium oxyhydroxide precipitation suspension B, conveying the gallium oxyhydroxide precipitation suspension B into an atomizing nozzle under continuous stirring, atomizing into liquid drops by an atomizing gas medium, and spheroidizing the liquid drops by plasma to obtain the high-purity beta gallium oxide nano microspheres.
The preparation method provided by the invention comprises the steps of firstly carrying out hydrothermal reaction on metal Ga and ultrapure water to obtain a gallium oxyhydroxide precipitate suspension A, adjusting the solid-to-liquid ratio, atomizing, obtaining small droplets through atomization, feeding the small droplets into plasma flame flow for high-temperature spray pyrolysis, wherein the moisture of the suspended droplets can be quickly volatilized under the ultrahigh-temperature high-speed environment, the gallium oxyhydroxide is pyrolyzed into beta gallium oxide at high temperature, the surface of the beta gallium oxyhydroxide is melted under the high-temperature action of plasma, spherical droplets are formed due to the action of surface tension, and spherical micro powder is formed after cooling.
In a preferred embodiment, the purity of the metal Ga is not less than 5N.
Preferably, the ultrapure water has a resistivity of not less than 18 M.OMEGA.cm (25 ℃).
In the invention, to obtain beta gallium oxide nano-microspheres with more than 5N, firstly, the purity of raw material gallium is ensured to be not less than 5N and the resistivity of pure water is ensured to be not less than 18 MOmega-cm (25 ℃).
Preferably, the mass ratio of the metal Ga to the ultrapure water is 1: 2-10.
Preferably, the temperature of the hydrothermal reaction is 180-280 ℃, and the time of the hydrothermal reaction is 5-8h.
In the actual operation process, metal Ga and ultrapure water are mixed and then placed in a high-pressure reaction kettle for reaction.
In a preferable scheme, in the gallium oxyhydroxide precipitate suspension B, the mass ratio of the gallium oxyhydroxide precipitate to water is 10-15: 90-85.
The inventor finds that the solid-liquid mass ratio of the gallium oxyhydroxide precipitate to water in the gallium oxyhydroxide precipitate suspension B is controlled in the above range, which is crucial, if the liquid phase is too much, the spheroidization efficiency is low, and the preparation amount is small; too little liquid phase results in low spheroidization ratio, and partial hydroxyl gallium oxide is converted into beta-Ga 2 O 3 And no balls are formed after the process.
In the actual operation process, the gallium oxyhydroxide precipitation suspension liquid B is conveyed to an atomizing nozzle by a straight-flow pump while being continuously stirred.
In a preferable scheme, the atomizing gas medium is selected from argon with the purity of more than or equal to 5N.
Preferably, the pressure of the atomized gas medium is 1.6-2.2MPa.
The inventors found that the final spheroidization rate is highest when the pressure of the atomized gas medium is controlled within the above range, and that when the atomization pressure is low, the gallium oxyhydroxide suspension is insufficiently atomized, and when the pressure is too high, the plasma flame stabilization is affected, and the direct current plasma flame is stabilized, the decomposition and spheroidization stability of the atomized gallium oxyhydroxide can be ensured, so that when the pressure of the atomized gas medium is too high or too low, the final spheroidization effect is affected.
In a preferred scheme, the flow rate of the atomizing gas medium is 0.5L/min-2.5L/min.
In a preferable scheme, when the plasma is spheroidized, the power of the plasma is 9.75 KW-12.8 KW.
The inventor finds that when the spheroidization power of the plasma is controlled within the range, the spheroidization rate is high, the dispersity is good, and if the spheroidization rate of the gallium oxyhydroxide is low, the gallium oxyhydroxide can be converted into beta gallium oxide to be fused and agglomerated due to too high power.
The invention also provides the high-purity beta gallium oxide nano-microsphere prepared by the preparation method.
The purity of the high-purity beta gallium oxide nano-microspheres is more than or equal to 5N, and the particle size of the high-purity beta gallium oxide nano-microspheres is 100-500 nm.
Principles and advantages
The invention provides a preparation method of high-purity beta gallium oxide nano microspheres, which comprises the steps of carrying out hydrothermal reaction on metal Ga and ultrapure water to obtain a gallium oxyhydroxide precipitate suspension A, adjusting the solid-liquid ratio, atomizing to obtain small droplets, sending the small droplets into a plasma flame flow for high-temperature spray pyrolysis, wherein the water in the suspended droplets can be rapidly volatilized in an ultrahigh-temperature and high-speed environment, the gallium oxyhydroxide is pyrolyzed at high temperature to form beta gallium oxide, the surface of the beta gallium oxyhydroxide is melted under the high-temperature action of plasma, spherical droplets are formed under the action of surface tension, and spherical micro powder is formed after cooling.
The invention provides a novel preparation method of high-purity gallium oxide nano microspheres, which can overcome the defects of large grain size, complex process and difficult process control of gallium oxide prepared by the prior art. Simple process and is beneficial to industrial production.
Drawings
FIG. 1 is a scanning electron micrograph of spherical fine particles of high purity beta gallium oxide obtained in example 1.
FIG. 2 is a scanning electron micrograph of the spherical fine powder of high purity beta gallium oxide obtained in example 2.
FIG. 3 is a scanning electron micrograph of the spherical fine powder of high purity beta gallium oxide obtained in comparative example 1.
Detailed Description
The present invention and its embodiments are described in further detail below with reference to examples.
The invention is characterized by the following steps:
A. 5N metal Ga and ultrapure water with the resistivity not lower than 18M omega cm (25 ℃) react in a high-pressure reaction kettle at the temperature of 180-280 ℃ according to the mass ratio of 1: 2-10 to obtain gallium oxyhydroxide precipitate suspension.
B. And C, adjusting the mass ratio of the hydroxyl gallium oxide precipitate suspension obtained in the step A to be 10-15: 90-85, continuously stirring and simultaneously conveying the suspension into an atomizing nozzle by using a direct current pump, and atomizing the suspension by using 5N argon gas with the pressure of 1.6-2.2MPa and the flow of 0.5-2.5L/min to form liquid drops with the particle size as small as possible.
C. And C, feeding the atomized liquid drops obtained in the step B into a plasma flame flow, carrying out high-temperature spray pyrolysis, controlling the power of the plasma to be 9.75-12.8 KW, rapidly volatilizing the moisture of the suspended liquid drops under an ultrahigh-temperature high-speed environment, pyrolyzing the hydroxyl gallium oxide into gallium oxide, melting the surface under the high-temperature action of the plasma, forming spherical liquid drops under the action of surface tension, and cooling to form spherical micro powder.
The raw materials of the gallium oxyhydroxide precipitation suspension liquid are 5N metal gallium and ultrapure water with the resistivity of not less than 18M omega cm (25 ℃).
Examples of the invention are given below:
example 1
10 g of gallium metal and 50g of water are reacted in a high-pressure reaction kettle at the reaction temperature of 250 ℃ for 5 hours to obtain gallium oxyhydroxide precipitate suspension. Adjusting the solid-liquid mass ratio in the gallium oxyhydroxide precipitation suspension to be 10: 90, continuously stirring and simultaneously conveying the suspension to an atomizing nozzle by a direct current pump, and atomizing the suspension by 5N argon gas with the pressure of 1.6MPa to form liquid drops with the particle size as small as possible. And (3) feeding the liquid drops obtained after atomization into plasma flame flow with the power of 9.75KW for high-temperature spray pyrolysis, and cooling to form spherical gallium oxide micro powder. FIG. 1 is a scanning electron micrograph of the high-purity spherical micro-powder of beta-gallium oxide obtained in example 1, from which it can be seen that the sphericity is high, the particle diameter D50 is 220nm, and the purity is not less than 99.999%. The results of the impurity content measurement are shown in table 1.
Example 2
Reacting 20 g of gallium metal and 150g of water in a high-pressure reaction kettle at the reaction temperature of 250 ℃ for 5 hours to obtain gallium oxyhydroxide precipitate suspension. Adjusting the mass ratio of solid to liquid in the gallium oxyhydroxide precipitation suspension to 15: 85, continuously stirring, conveying the suspension to an atomizing nozzle by a direct-current pump, and atomizing the suspension by 5N argon with the pressure of 2.2MPa to form liquid drops with the smallest particle size. And (3) feeding the liquid drops obtained after atomization into plasma flame flow with the power of 12.8KW for high-temperature spray pyrolysis, and cooling to form spherical gallium oxide micro powder. FIG. 2 is a scanning electron micrograph of the spherical fine powder of high-purity beta gallium oxide obtained in example 2, wherein the particle diameter D50 is 490nm, and the purity is not less than 99.999%. The results of the impurity content measurement are shown in table 1.
Comparative example 1
Otherwise, the mixture was atomized with 5N argon gas under a pressure of 1.8MPa to form droplets having as small a particle size as possible, in accordance with example 2. And (3) feeding the liquid drops obtained after atomization into plasma flame flow with the power of 19.5KW for high-temperature spray pyrolysis, and cooling to form large-particle spherical gallium oxide micro powder after agglomeration. Fig. 3 is a scanning electron microscope photograph of the spherical fine powder of high purity beta gallium oxide of comparative example 3, from which it can be found that the particle size of the fine powder is larger and D50 reaches 35 μm due to the fusion and agglomeration after the gallium oxyhydroxide is converted into the beta gallium oxide because the plasma power is too high. The results of the impurity content measurement are shown in Table 1.
TABLE 1
Claims (10)
1. A preparation method of high-purity beta gallium oxide nano microspheres is characterized by mixing metal Ga and ultrapure water to obtain a mixed solution, carrying out hydrothermal reaction to obtain a gallium oxyhydroxide precipitation suspension A, adjusting the solid-to-liquid ratio of the gallium oxyhydroxide precipitation suspension A to obtain a gallium oxyhydroxide precipitation suspension B, conveying the gallium oxyhydroxide precipitation suspension B into an atomizing nozzle under continuous stirring, atomizing into liquid drops by using an atomizing gas medium, and carrying out plasma spheroidization on the liquid drops to obtain the high-purity beta gallium oxide nano microspheres.
2. The preparation method of the high-purity beta gallium oxide nanospheres according to claim 1, wherein the purity of the metal Ga is not less than 5N;
the resistivity of the ultrapure water is not lower than 18M omega cm (25 ℃).
3. The method for preparing high-purity beta gallium oxide nanospheres according to claim 1 or 2, wherein the mass ratio of metal Ga to ultrapure water is 1: 2-10.
4. The preparation method of the high-purity beta gallium oxide nanospheres according to claim 1 or 2, wherein the temperature of the hydrothermal reaction is 180-280 ℃ and the time of the hydrothermal reaction is 5-8h.
5. The method for preparing high-purity beta gallium oxide nanospheres according to claim 1 or 2, wherein the mass ratio of gallium oxyhydroxide precipitate to water in the gallium oxyhydroxide precipitate suspension B is 10-15: 90-85.
6. The preparation method of the high-purity beta gallium oxide nanospheres according to claim 1 or 2, wherein the atomizing gas medium is selected from argon with purity of not less than 5N.
7. The method for preparing high-purity beta gallium oxide nanospheres according to claim 1 or 2, wherein the pressure of the atomizing gas medium is 1.6-2.2MPa; the flow rate of the atomized gas medium is 0.5L/min-2.5L/min.
8. The preparation method of the high-purity beta gallium oxide nanospheres according to claim 1 or 2, characterized in that the power of the plasma during plasma spheroidization is 9.75 KW-12.8 KW.
9. A high purity beta gallium oxide nanosphere prepared by the method of any of claims 1-8.
10. The high-purity beta gallium oxide nanosphere according to claim 9, wherein: the purity of the high-purity beta gallium oxide nano-microspheres is more than or equal to 5N, and the particle size of the high-purity beta gallium oxide nano-microspheres is 100-500 nm.
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|---|---|---|---|---|
| KR101473716B1 (en) * | 2013-08-23 | 2014-12-26 | (주)티에스엠 | Manufacturing method of gallium oxide of high purity spherical for minimalize of loss of gallium and high purity spherical gallium oxide therefrom |
| CN106744730A (en) * | 2015-11-19 | 2017-05-31 | 上饶师范学院 | Gallium oxide, gallium nitride nano-powder are prepared by raw material two-step method of gallium |
| CN113371682A (en) * | 2021-05-13 | 2021-09-10 | 中国恩菲工程技术有限公司 | Nano-micron spherical powder and preparation method and equipment thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101473716B1 (en) * | 2013-08-23 | 2014-12-26 | (주)티에스엠 | Manufacturing method of gallium oxide of high purity spherical for minimalize of loss of gallium and high purity spherical gallium oxide therefrom |
| CN106744730A (en) * | 2015-11-19 | 2017-05-31 | 上饶师范学院 | Gallium oxide, gallium nitride nano-powder are prepared by raw material two-step method of gallium |
| CN113371682A (en) * | 2021-05-13 | 2021-09-10 | 中国恩菲工程技术有限公司 | Nano-micron spherical powder and preparation method and equipment thereof |
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