CN111283210A - High-purity metal vanadium powder and preparation method thereof - Google Patents
High-purity metal vanadium powder and preparation method thereof Download PDFInfo
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 57
- 239000002184 metal Substances 0.000 title claims abstract description 57
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000012216 screening Methods 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000000889 atomisation Methods 0.000 claims description 6
- 238000010894 electron beam technology Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 229910001338 liquidmetal Inorganic materials 0.000 claims description 4
- 238000003754 machining Methods 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000009751 slip forming Methods 0.000 claims 1
- 238000011068 loading method Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 description 12
- 229910045601 alloy Inorganic materials 0.000 description 11
- 239000007789 gas Substances 0.000 description 10
- 239000002994 raw material Substances 0.000 description 6
- 230000004927 fusion Effects 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229910000756 V alloy Inorganic materials 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007123 defense Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- GVHUQXQVSWGYSH-UHFFFAOYSA-N 4-(3-bromophenyl)-2-methyl-1,3-thiazole Chemical compound S1C(C)=NC(C=2C=C(Br)C=CC=2)=C1 GVHUQXQVSWGYSH-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/10—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying using centrifugal force
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
- C22C27/025—Alloys based on vanadium, niobium, or tantalum alloys based on vanadium
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Mechanical Engineering (AREA)
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- Organic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to high-purity metal vanadium powder and a preparation method thereof. The method comprises the following steps: preparing and processing metal vanadium into an electrode rod, then loading the electrode rod into an atomizing device, atomizing to prepare powder, and screening and grading to obtain high-purity metal vanadium powder with the granularity of less than or equal to 60 meshes. The V content of the high-purity metal vanadium powder is more than or equal to 99.9 percent, the Fe content is less than or equal to 0.02 percent, the Si content is less than or equal to 0.01 percent, the Cr content is less than or equal to 0.03 percent, the Al content is less than or equal to 0.01 percent, and the O content is less than or equal to 0.03 percent (weight percentage). The method has the advantages of simple preparation process, low impurity element content, low gas element content, stable comprehensive performance, high material utilization rate, easy realization of large-scale production, high production efficiency and good effect.
Description
Technical Field
The invention belongs to the technical field of special alloy smelting and atomization powder preparation, and particularly relates to high-purity metal vanadium powder and a preparation method thereof.
Background
Vanadium-containing steel has excellent characteristics of high strength, high toughness, good wear resistance and the like, is widely applied to industries such as automobiles, shipbuilding, railways, aviation, bridges, electronic technology, national defense industry and the like, and accounts for about 85% of vanadium consumption.
The metal pure vanadium has the characteristics of high melting point, corrosion resistance, hydrogen storage, high-temperature superconductivity, strong high-temperature creep resistance, small fast neutron absorption cross section and the like, and is widely applied to the aviation, aerospace, nuclear industry, military industry and new strategic industry of national defense. The pure vanadium metal can be prepared by various methods, such as fused salt electrolysis, vanadium iodide thermal decomposition, active metal reduction, electron beam cold hearth refining, etc. The V-4Cr-4Ti alloy is an important candidate structural material of a fusion reactor, and has excellent properties of low activation property, high-temperature strength, liquid metal corrosion resistance, neutron irradiation swelling resistance and the like. Therefore, the alloy is of great interest in the design of structures such as the primary wall, cladding and divertors of a fusion reactor. In order to further improve the high-temperature strength and the service temperature of the V-4Cr-4Ti alloy, researchers propose that metal oxides are added into the V-4Cr-4Ti alloy through a mechanical alloying method to obtain the V-4Cr-4Ti alloy with a dispersion strengthening effect. The V-4Cr-4Ti alloy introduces a large amount of fine dispersed phases, can pin dislocation in a material matrix, increase rheological stress, and can pin grain boundaries, prevent grain boundary slippage and improve the strength. In addition, a plurality of interfaces are formed between the fine dispersion phase and the matrix, and point defects caused by neutron irradiation in the reactor can be captured, so that the irradiation resistance of the material is enhanced. Meanwhile, the dispersed phase has excellent thermal stability, and is beneficial to further improving the service temperature of the vanadium alloy material.
The preparation of dispersion-strengthened V-4Cr-4Ti alloy by the mechanical alloying method requires high-quality vanadium powder or vanadium alloy powder as a raw material as a premise. At present, methods for preparing metal vanadium powder include a mechanical crushing method and a metal gas-based reduction method. The mechanical crushing method mainly adopts dendritic vanadium metal prepared by a molten salt electrolysis method as a raw material, and then crushes the dendritic vanadium metal by a mechanical ball mill to finally obtain vanadium metal powder. According to the method, a large amount of impurity elements (W, Co, Ni, Fe, Cr and the like) are introduced in the mechanical ball milling process, and meanwhile, vanadium powder is easy to oxidize in the ball milling process, so that the oxygen content of the final metal vanadium powder can exceed 0.5 wt%. The patent (CN 109295310A) of advanced metal material industry and technology research institute Limited company adopts metal gas-based reduction to prepare high-purity metal vanadium powder, and the method adopts vanadium oxide as a raw material and active metal as a reducing agent to obtain the metal vanadium powder with the purity of 98 wt% through the thermal reduction reaction of the raw material and the reducing agent. The purity of the vanadium powder prepared by the two methods can not meet the limit of impurity elements and gas elements of nuclear fusion structural materials, and the types and the quantity of related impurity elements are not restricted
Disclosure of Invention
The invention mainly aims to provide high-purity metal vanadium powder and a preparation method thereof, which are easy to realize large-scale production, high in production efficiency and good in effect.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-purity vanadium metal powder has the following characteristics,
(1) the components: the V content of the high-purity metal vanadium powder is more than or equal to 99.9 percent, the Fe content is less than or equal to 0.02 percent, the Si content is less than or equal to 0.01 percent, the Cr content is less than or equal to 0.03 percent, the Al content is less than or equal to 0.01 percent, and the O content is less than or equal to 0.03 percent (all in weight percentage); (2) granularity: less than or equal to-60 meshes (standard mesh number).
The invention provides a preparation method of high-purity metal vanadium powder, which comprises the following steps:
(1) preparing an electrode bar: preparing metal vanadium round bars with the size meeting the requirement by vacuum electron beam melting, and machining the metal vanadium round bars into electrode bars;
(2) charging an electrode bar: and filling the electrode rod into an atomizing device through a mechanical shaft, extending the electrode rod into an atomizing chamber, vacuumizing the atomizing chamber for three stages, filling high-purity Ar gas (99.99 percent), and ensuring positive pressure in the atomizing chamber.
(3) Atomizing to prepare powder: and starting the electric spindle to control the rotating speed of the electrode rod connected with the mechanical shaft, wherein the specific rotating speed is determined according to the dynamic balance condition of the specific rod material. Starting a plasma gun, loading the melting point of the current view electrode Bar material, and keeping the atmosphere pressure at 1.5 Bar; the micro-area liquid film is formed continuously with the front end surface of the electrode rod being heated, the electrode rod keeps a certain stepping rate while keeping high rotating speed, so that the micro-area liquid film is broken into high-temperature liquid drops under the action of centrifugal force; the high-temperature liquid drops are rapidly cooled to form metal powder in the flying process in the atomizing chamber.
(4) Screening and grading: and finally, the prepared powder falls into a collecting charging barrel at the lowest part, and is screened and classified on a screening machine according to the requirements of customers, so that the high-purity metal vanadium powder is finally obtained.
Further, in the step (1), the content of impurity elements in the metal vanadium round rod is required to be as follows: fe content is less than or equal to 0.02%, Si content is less than or equal to 0.01%, Cr content is less than or equal to 0.03%, Al content is less than or equal to 0.01%, and O content is less than or equal to 0.025%.
Further, in the step (1), the electrode rod has the following size requirements: the diameter of the electrode rod is phi 40 mm-75 mm, and the length of the electrode rod is 300mm-1000 mm.
Further, in the step (3), the rotating speed of the electrode bar is 10000r/min-18000 r/min; the current of the plasma gun is 1800A-2800A; the electrode bar stepping rate is 1.0mm/s-2.0 mm/s.
Further, in the step (4), screening and grading are carried out on a screening machine to obtain the high-purity metal vanadium powder with-60 meshes (standard mesh number).
The preparation method of the invention adopts the metal vanadium as the raw material, the electrode rod is manufactured by machining after vacuum electron beam melting, and the high-purity metal vanadium powder with low impurity content and low gas element content is obtained by the atomization process.
The high-purity metal vanadium powder with low impurity content and low gas element content, prepared by the invention, provides raw material guarantee for preparing vanadium-based alloy by a powder metallurgy method, further improves the dispersion of the V-4Cr-4Ti alloy for nuclear fusion and strengthens the comprehensive performance of the V-4Cr-4Ti alloy, and promotes the development of structural components for nuclear fusion in China.
Drawings
FIG. 1 is a process flow chart of the preparation method of high-purity metal vanadium powder.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples, but the present invention is not limited thereto, and can be implemented by appropriately modifying the present invention within the scope not changing the claims of the present invention.
Example 1
The high-purity metal vanadium powder comprises the following components in parts by weight:
(1) the components: fe content: 0.017%, Si content: 0.01%, Cr content: 0.026%, Al content: less than or equal to 0.01 percent, and the content of O is as follows: less than or equal to 0.026%, and V content: the balance (weight percent);
(2) granularity: 100 mesh (standard mesh count).
The preparation process of the high-purity metal vanadium powder comprises the following steps:
(1) preparing an electrode bar: metal vanadium prepared by a molten salt electrolysis method is prepared into metal vanadium round bar materials with the diameter phi of 50mm through vacuum electron beam melting, and the metal vanadium round bar materials are machined into electrode bars with the diameter phi of 40mm multiplied by 300 mm;
(2) charging an electrode bar: the electrode rod is filled into an atomizing chamber of the atomizing device through a mechanical shaft, the electrode rod extends into the atomizing chamber, the length of the electrode rod is about one third of the length of the whole electrode rod when the electrode rod is lifted into the atomizing chamber, then the atomizing chamber is vacuumized in three stages and filled with high-purity Ar gas (99.99%), and positive pressure of the atomizing chamber is guaranteed.
(3) Atomizing to prepare powder: and starting the electric spindle, controlling the rotating speed of the electrode rod connected with the mechanical shaft, and adjusting the rotating speed of the electrode rod to 10000r/min, wherein the specific rotating speed is determined according to the dynamic balance condition of the specific bar. Starting a plasma gun, loading current to 1800A by an electrode Bar, and keeping the atmosphere pressure at 1.5 Bar; the micro-area liquid film is formed continuously with the front end surface of the electrode rod being heated, the electrode rod keeps the stepping rate of 1.0mm/s while keeping high rotating speed, and the liquid metal is subjected to centrifugal force and rapid cooling action to form metal powder.
(4) Screening and grading: finally, the prepared powder falls into a collecting charging barrel at the lowest part, and is screened and graded on a screening machine to finally obtain the high-purity metal vanadium powder with the particle size of-100 meshes.
The high-purity vanadium powder with low impurity content and low gas element content is prepared by the embodiment, the powder yield is high, and the main indexes are as follows: (1) the components: fe content: 0.017%, Si content: 0.01%, Cr content: 0.026%, Al content: less than or equal to 0.01 percent, and the content of O is as follows: less than or equal to 0.026%, and V content: the balance (weight percent); (2) granularity: 100 mesh (standard mesh count).
Example 2
The high-purity metal vanadium powder comprises the following components in parts by weight:
(1) the components: fe content: 0.016%, Si content: less than or equal to 0.01 percent, Cr content: 0.018%, Al content: less than or equal to 0.01 percent, and the content of O is as follows: less than or equal to 0.023 percent, and the content of V is as follows: the balance, (weight percent);
(2) granularity: 60 mesh (standard mesh count).
The preparation process of the high-purity metal vanadium powder comprises the following steps:
(1) preparing an electrode bar: metal vanadium prepared by a molten salt electrolysis method is prepared into a metal vanadium round bar with the diameter phi of 75mm through vacuum electron beam melting, and is machined into an electrode bar with the diameter phi of 70mm multiplied by 1000 mm;
(2) charging an electrode bar: the electrode rod is filled into an atomizing chamber of the atomizing device through a mechanical shaft, the electrode rod extends into the atomizing chamber, the length of the electrode rod is about one third of the length of the whole electrode rod when the electrode rod is lifted into the atomizing chamber, then the atomizing chamber is vacuumized in three stages and filled with high-purity Ar gas (99.99%), and positive pressure of the atomizing chamber is guaranteed.
(3) Atomizing to prepare powder: and starting the electric spindle, controlling the rotating speed of the electrode rod connected with the mechanical shaft, and adjusting the rotating speed of the electrode rod to 18000r/min, wherein the specific rotating speed is determined according to the dynamic balance condition of the specific rod. Starting a plasma gun, loading current to 2800A on an electrode Bar, and keeping the atmosphere pressure at 1.5 Bar; the micro-area liquid film is formed continuously with the front end face of the electrode rod being heated, the electrode rod keeps the step rate of 2.0mm/s while keeping high rotation speed, and the liquid metal is subjected to centrifugal force and rapid cooling action to form metal powder.
(4) Screening and grading: finally, the prepared powder falls into a collecting charging barrel at the lowest part, and is screened and graded on a screening machine to finally obtain the high-purity metal vanadium powder with 60 meshes.
The high-purity vanadium powder with low impurity content and low gas element content is prepared by the embodiment, the powder yield is high, the product granularity distribution is uniform, and the main indexes are as follows: (1) the components: fe content: 0.016%, Si content: less than or equal to 0.01 percent, Cr content: 0.018%, Al content: less than or equal to 0.01 percent, and the content of O is as follows: less than or equal to 0.023 percent, and the content of V is as follows: the balance, (weight percent); (2) granularity: 100 mesh (standard mesh count).
The above embodiments describe the technical solutions of the present invention in detail. It will be clear that the invention is not limited to the described embodiments. Based on the embodiments of the present invention, those skilled in the art can make various changes, but any changes equivalent or similar to the present invention are within the protection scope of the present invention.
Claims (7)
1. A high-purity metal vanadium powder is characterized in that,
(1) the components: the V content of the high-purity metal vanadium powder is more than or equal to 99.9 percent, the Fe content is less than or equal to 0.02 percent, the Si content is less than or equal to 0.01 percent, the Cr content is less than or equal to 0.03 percent, the Al content is less than or equal to 0.01 percent, and the O content is less than or equal to 0.03 percent (weight percentage);
(2) granularity: 60 mesh (standard mesh count).
2. The preparation method of the high-purity metal vanadium powder is characterized by comprising the following steps:
(1) preparing an electrode bar: preparing metal vanadium round bar materials by melting metal vanadium through vacuum electron beams, and preparing electrode bars by machining;
(2) charging an electrode bar: filling an electrode rod into an atomization device through a mechanical shaft, extending the electrode rod into an atomization chamber, vacuumizing the atomization chamber in three stages, filling high-purity Ar gas, and ensuring positive pressure of the atomization chamber;
(3) atomizing to prepare powder: starting an electric spindle, controlling the rotating speed of an electrode rod connected with a mechanical shaft, and starting a plasma gun, wherein the atmosphere pressure is 1.5 Bar; the micro-area liquid film is continuously formed along with the heating of the front end surface of the electrode rod, the electrode rod keeps a certain stepping rate while keeping high rotating speed, so that the micro-area liquid film is broken into high-temperature liquid drops under the action of centrifugal force on the liquid metal; the high-temperature liquid drops are rapidly cooled to form metal powder in the flying process in the atomizing chamber;
(4) screening and grading: and (4) screening and grading the metal powder prepared in the step (3) to finally obtain the high-purity metal vanadium powder.
3. The method according to claim 2, wherein the content of impurity elements in the metal vanadium round rod in the step (1) requires that: fe content is less than or equal to 0.02%, Si content is less than or equal to 0.01%, Cr content is less than or equal to 0.03%, Al content is less than or equal to 0.01%, and O content is less than or equal to 0.025%.
4. The method of claim 2, wherein the electrode rod size requirement of step (1) is: the diameter of the electrode rod is phi 40 mm-75 mm, and the length of the electrode rod is 300mm-1000 mm.
5. The method according to claim 2, wherein the concentration of the high purity Ar gas in step (2) is 99.99%.
6. The method according to claim 2, wherein the rotation speed of the electrode rod in the step (3) is 10000r/min-18000 r/min; the current of the plasma gun is 1800A-2800A; the electrode rod stepping rate is 1.0mm/s-2.0 mm/s.
7. The method as claimed in claim 2, wherein the screening in the step (4) is carried out on a screening machine for screening and grading to obtain the high-purity metal vanadium powder with the number of minus 60 meshes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112024900A (en) * | 2020-08-24 | 2020-12-04 | 四川容克斯科技有限公司 | Spherical metal vanadium powder and preparation method and application thereof |
| CN113770349A (en) * | 2021-09-14 | 2021-12-10 | 有研工程技术研究院有限公司 | High-purity spherical metal vanadium powder and preparation method and application thereof |
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2020
- 2020-02-27 CN CN202010123861.4A patent/CN111283210A/en active Pending
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| CN113770349A (en) * | 2021-09-14 | 2021-12-10 | 有研工程技术研究院有限公司 | High-purity spherical metal vanadium powder and preparation method and application thereof |
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Application publication date: 20200616 |