CN116652198A - Method for preparing tantalum powder by gas atomization of plasma rotary electrode - Google Patents
Method for preparing tantalum powder by gas atomization of plasma rotary electrode Download PDFInfo
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- CN116652198A CN116652198A CN202310634590.2A CN202310634590A CN116652198A CN 116652198 A CN116652198 A CN 116652198A CN 202310634590 A CN202310634590 A CN 202310634590A CN 116652198 A CN116652198 A CN 116652198A
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000009689 gas atomisation Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 59
- 229910052751 metal Inorganic materials 0.000 claims abstract description 31
- 239000002184 metal Substances 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 22
- 238000000889 atomisation Methods 0.000 claims abstract description 16
- 230000001681 protective effect Effects 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000003723 Smelting Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 230000006698 induction Effects 0.000 claims description 6
- 238000009489 vacuum treatment Methods 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 230000003746 surface roughness Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 239000000654 additive Substances 0.000 abstract description 10
- 230000000996 additive effect Effects 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 10
- 238000010894 electron beam technology Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 238000005266 casting Methods 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 229910052715 tantalum Inorganic materials 0.000 description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 239000011261 inert gas Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 5
- 238000012216 screening Methods 0.000 description 5
- 239000000110 cooling liquid Substances 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- 239000012798 spherical particle Substances 0.000 description 4
- 238000009461 vacuum packaging Methods 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000004075 alteration Effects 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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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
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
-
- 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
- B22F12/00—Apparatus or devices specially adapted for additive manufacturing; Auxiliary means for additive manufacturing; Combinations of additive manufacturing apparatus or devices with other processing apparatus or devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/10—Pre-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Chemical & Material Sciences (AREA)
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- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a method for preparing tantalum powder by gas atomization of a plasma rotary electrode, and belongs to the technical field of tantalum metal processing technology. The method comprises the following steps: s1, casting ingot and processing to prepare a tantalum metal bar according to the component proportion of the tantalum metal bar; s2, placing the tantalum metal bar in a plasma rotary electrode atomization powder making device, sealing, vacuumizing, introducing protective gas, adding the end part of the tantalum metal bar by using a plasma gun, uniformly melting the tantalum metal bar, rotating to generate centrifugal force to throw out liquid drop-shaped metal, condensing and spheroidizing to obtain particle powder to obtain tantalum powder; the end part of the electrode rod is attached with a liquid film layer, and the liquid film is arranged on the end part of the electrode rod. The method adopts the high-speed plasma rotary electrode process to prepare the tantalum powder, and the prepared tantalum powder has the advantages of high sphericity, no high-temperature oxidation, narrow particle size range, high powder quality, excellent physical, chemical and comprehensive mechanical properties, and is suitable for being used in the electron beam powder-laying type additive manufacturing process.
Description
Technical Field
The invention relates to the technical field of tantalum metal processing technology, in particular to a method for preparing tantalum powder by gas atomization of a plasma rotary electrode.
Background
The additive manufacturing is based on a digital model, materials are manufactured into solid articles in a layer-by-layer stacking mode, the process of producing complex parts is greatly simplified, the concept and mode of traditional manufacturing are subverted, and the transition from the traditional manufacturing industry to the modern manufacturing industry is deeply influenced.
Electron beam and laser additive manufacturing are the main stream of the powder-laying type additive manufacturing, but the requirement on powder laying is extremely high, such as the chemical and physical property stability of powder is a precondition, and the electron beam and laser additive manufacturing comprises reasonable fluidity, particle size and morphology of powder, uniform components and the like.
Tantalum powder is a powdery substance of metallic tantalum and has many important uses. Tantalum powder is one of the important raw materials for manufacturing tantalum electrolytic capacitors. The capacitor has the advantages of high capacitance density, low resistance, high temperature stability, long service life and the like, and is widely applied to consumer electronic products such as mobile phones, notebook computers, tablet computers and the like in the electronic industry. The tantalum powder can be used as an additive for manufacturing high-temperature alloy, and can improve the oxidation resistance, corrosion resistance, high-temperature resistance and the like of the alloy. The alloy is widely used in the fields of aerospace, petrochemical industry, nuclear engineering and the like. The tantalum powder can be made into materials of corrosion-resistant equipment, such as tantalum pipes, tantalum plates and the like, and has the characteristics of strong corrosion resistance, high temperature resistance, good corrosion resistance and the like. These devices are widely used in chemical, electronic, medical, etc. industries. At present, most of the powder is prepared by adopting an air atomization powder preparation technology, and the obtained powder has low sphericity, more satellite powder and poor fluidity.
Disclosure of Invention
Aiming at the problems of insufficient stability, low sphericity and poor fluidity of the components in the existing traditional preparation of tantalum powder by gas atomization, the invention provides a method for preparing tantalum powder by gas atomization of a plasma rotary electrode, which adopts a high-speed plasma rotary electrode process to prepare tantalum (Ta) powder, and the prepared tantalum (Ta) powder has the advantages of high sphericity, no high-temperature oxidation, narrow particle size range, less hollow powder and satellite powder, less gas inclusion, high powder quality, excellent physical, chemical and comprehensive mechanical properties and is suitable for being used in an electron beam powder-laying type additive manufacturing process.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the invention aims to provide a method for preparing tantalum powder by gas atomization of a plasma rotary electrode, which comprises the following steps:
s1, smelting by using a vacuum induction furnace according to the component proportion of the tantalum metal bar to obtain an ingot, and then processing to prepare the tantalum metal bar;
s2, placing the tantalum metal bar in a plasma rotary electrode atomization powder making device, sealing, vacuumizing, introducing protective gas, adding the end part of the tantalum metal bar by using a plasma gun, uniformly melting the tantalum metal bar, simultaneously rotating at a high speed to generate centrifugal force to throw out liquid drop-shaped metal, condensing and spheroidizing the tantalum metal bar in the protective gas at the rotating speed of 30000-42000 r/min to obtain granular powder, and screening the dried tantalum powder to obtain the tantalum powder.
Preferably, in S1, the tantalum metal bar has a composition of C:0.01 to 0.02, O:0.01 to 0.02, N: less than or equal to 0.01, H: less than or equal to 0.01, and the balance of Ta.
Preferably, in S1, the diameter of the tantalum metal bar is 30-50 mm, the length is 160-200 mm, the surface roughness is less than or equal to 1 mu m, the roundness deflection angle of the tantalum metal bar is not more than 0.05mm, the linear deflection is not more than 0.01mm, and the relative density is not less than 99%.
Preferably, in S2, when the vacuum degree of the vacuum treatment is 3 to 10X 10 -3 After Pa, the pressure after the protective gas is introduced is 0.1 to 1 multiplied by 10 -5 Pa; the shielding gas is argon.
Preferably, in S2, the oxygen content in the environment after the protective gas is introduced is less than 0.1wt%.
Preferably, in S2, the current of the plasma gun is 800-1000A, and the voltage is 80V.
Preferably, in S2, the distance between the atomizing electrode rod and the plasma gun is 10mm, the feeding speed is 1.2mm/S, and the working gas flow rate of the plasma is 120m 3 /h。
Preferably, in S2, the particle size of the tantalum powder after sieving is 10-90 μm, the fluidity is (5-7)/50 g, and the apparent density is 10.58-10.63g/cm 3 Tap density of 10.5-10.8g/cm 3 。
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention adopts the high-speed plasma rotating electrode process to prepare the tantalum (Ta) powder, and the prepared tantalum (Ta) powder has high sphericity, no high-temperature oxidation, narrow particle size range, less hollow powder and satellite powder, less gas inclusion, high powder quality and excellent physical and chemical properties. Under the action of plasma, the tantalum powder can be melted, flowed and solidified on the surface, so that relatively uniform spherical powder is formed, and the tantalum powder is particularly suitable for being used in an electron beam powder-laying type additive manufacturing process.
(2) The invention can control the granularity of the powder by controlling the parameters of rotation speed, current and voltage, and the like, has high yield and production efficiency of the Ta powder, and has good technological properties of the prepared Ta powder such as fluidity, bulk density, tap density, and the like.
Drawings
FIG. 1 is a flow chart of a tantalum powder process prepared by the invention;
FIG. 2 is a scanning electron microscope image of the tantalum powder prepared in example 1 of the present invention;
fig. 3 is a high power scan of tantalum powder prepared in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available unless otherwise specified.
Example 1
A method for preparing tantalum powder by gas atomization of a plasma rotary electrode is shown in a process flow chart of the tantalum powder prepared by the method as shown in figure 1, and comprises the following steps:
s1, according to mass percent, according to C:0.015, O:0.01, N: less than or equal to 0.01, H: less than or equal to 0.01, the balance being Ta, the sum of the mass percentages of all the groups being 100 percent, carrying out batching, smelting by using a vacuum induction furnace and electroslag remelting to obtain cast ingots, and rolling into tantalum metal bars, wherein the tantalum metal bars conform to the current tantalum (Ta) metal standard: GB/T14841-2008 requirements; carrying out finish turning on the smelted tantalum (Ta) metal rod to obtain a tantalum (Ta) metal electrode rod, removing iron scales to obtain a metal electrode rod meeting the requirements of a plasma rotary electrode atomization powder process, wherein the density of the metal electrode rod is 99%, casting defects such as obvious looseness and shrinkage cavity do not exist, the diameter of the processed tantalum metal electrode rod is 30mm, the degree is 160mm, the roundness deviation is 0.05mm, the straightness deviation is 0.01mm, and the roughness is 1 mu m;
s2, placing the tantalum metal bar in a plasma rotary electrode atomization powder making device, holding the tantalum metal bar on a bar selecting and loading and axial moving mechanical device to form a novel dynamic sealing structure, and after the pre-vacuumizing treatment is carried out on the whole set of powder making equipment, when the vacuum degree of the vacuum treatment is lower than 3 multiplied by 10 -3 Pa, introducing protective gas which is mixed gas of helium and argon to ensure that the pressure in the chamber reaches 0.1 multiplied by 10 -5 Pa, ensuring that the oxygen content in the atmosphere is less than 0.1wt%;
setting the working voltage to 80V, setting the melting current to 1000A, adjusting the rotating speed of the bar to 36000r/min, starting an atomization function and igniting a plasma generator, heating the end face of the high-speed rotating tantalum metal electrode bar by a plasma gun, uniformly melting the electrode bar and throwing out the electrode bar at a high speed by virtue of centrifugal force generated by rotation, rapidly cooling liquid into spherical particles in an inert gas environment, classifying and collecting the condensed powder particles under the protection of inert gas, vacuum packaging after screening, and finally collecting the spherical powder of tantalum Ta metal.
The particle size of the Ta metal powder is 20-90 mu m, and the specific particle size distribution is as follows: fluidity of 35 μm to 65 μm: 5.63/50g, bulk density 10.63g/cm 3 Tap density of 10.50g/cm 3 。
Example 2
A method for preparing tantalum powder by gas atomization of a plasma rotary electrode comprises the following steps:
s1, according to mass percent, according to C:0.016, O:0.015, n: less than or equal to 0.01, H: less than or equal to 0.01, the balance being Ta, the sum of the mass percentages of all the groups being 100 percent, carrying out batching, smelting by using a vacuum induction furnace and electroslag remelting to obtain cast ingots, and rolling into tantalum metal bars, wherein the tantalum metal bars conform to the current tantalum (Ta) metal standard: GB/T14841-2008 requirements; carrying out finish turning on the smelted tantalum metal rod to obtain a tantalum metal electrode rod, removing iron scales to obtain a metal electrode rod meeting the requirements of a plasma rotary electrode atomization powder process, wherein the density of the metal electrode rod is 99%, no obvious casting defects such as loosening and shrinkage cavity exist, the diameter of the processed tantalum metal electrode rod is 30mm, the degree is 160mm, the roundness deviation is 0.05mm, the straightness deviation is 0.01mm and the roughness is 1 mu m;
s2, placing the tantalum metal bar in a plasma rotary electrode atomization powder making device, holding the tantalum metal bar on a bar selecting and loading and axial moving mechanical device to form a novel dynamic sealing structure, and after the pre-vacuumizing treatment is carried out on the whole set of powder making equipment, when the vacuum degree of the vacuum treatment is 3 multiplied by 10 -3 After Pa, introducing a protective gas which is a mixed gas of helium and argon to ensure that the pressure in the chamber reaches 0.1X10 -5 Pa, ensuring that the oxygen content in the atmosphere is less than 0.1wt%;
setting the working voltage to 80V, setting the melting current to 1000A, adjusting the rotating speed of the bar to 42000r/min, starting an atomization function and igniting a plasma generator, heating the end face of the high-speed rotating tantalum metal electrode bar by a plasma gun to uniformly melt the bar and throwing out the bar at a high speed by virtue of centrifugal force generated by rotation, rapidly cooling liquid into spherical particles in an inert gas environment, classifying and collecting the condensed powder particles under the protection of inert gas, vacuum packaging after screening, and finally collecting the spherical powder of tantalum Ta metal.
The particle size of the Ta metal powder is between 12 and 88 mu m, and the specific particle size distribution is as follows: 28 μm to 55 μm, fluidity: 5.53/50g, bulk density 10.58g/cm 3 Tap density 10.80g/cm 3 。
Example 3
A method for preparing tantalum powder by gas atomization of a plasma rotary electrode comprises the following steps:
s1, according to mass percent, according to C:0.017, O:0.016, N: less than or equal to 0.01, H: less than or equal to 0.01, the balance being Ta, the sum of the mass percentages of all the groups being 100 percent, carrying out batching, smelting by using a vacuum induction furnace and electroslag remelting to obtain cast ingots, and rolling into tantalum metal bars, wherein the tantalum metal bars conform to the current tantalum (Ta) metal standard: GB/T14841-2008 requirements; carrying out finish turning on the smelted tantalum (Ta) metal rod to obtain a tantalum (Ta) metal electrode rod, removing iron scales to obtain a metal electrode rod meeting the requirements of a plasma rotary electrode atomization powder process, wherein the density of the metal electrode rod is 99%, casting defects such as obvious looseness and shrinkage cavity do not exist, the diameter of the processed tantalum metal electrode rod is 30mm, the degree is 160mm, the roundness deviation is 0.05mm, the straightness deviation is 0.01mm, and the roughness is 1 mu m;
s2, placing the tantalum metal bar in a plasma rotary electrode atomization powder making device, holding the tantalum metal bar on a bar selecting and loading and axial moving mechanical device to form a novel dynamic sealing structure, and after the pre-vacuumizing treatment is carried out on the whole set of powder making equipment, when the vacuum degree of the vacuum treatment is 3 multiplied by 10 -3 After Pa, introducing a protective gas which is a mixed gas of helium and argon to ensure that the pressure in the chamber reaches 0.1X10 -5 Pa, ensuring that the oxygen content in the atmosphere is less than0.1wt％；
Setting the working voltage to 80V, setting the melting current to 800A, adjusting the rotating speed of the bar to 30000r/min, starting an atomization function and igniting a plasma generator, heating the end face of the high-speed rotating tantalum metal electrode bar by a plasma gun to uniformly melt the bar and throwing out the bar at a high speed by virtue of centrifugal force generated by rotation, rapidly cooling liquid into spherical particles in an inert gas environment, classifying and collecting the condensed powder particles under the protection of inert gas, vacuum packaging after screening, and finally collecting the spherical powder of tantalum Ta metal.
The particle size of the Ta metal powder is 20-100 mu m, and the specific particle size distribution is as follows: fluidity of 35 μm to 75 μm: 5.76/50g, bulk density 10.69g/cm 3 Tap density 10.390g/cm 3 。
Example 4
A method for preparing tantalum powder by gas atomization of a plasma rotary electrode comprises the following steps:
s1, according to mass percent, according to C:0.015, O:0.01, N: less than or equal to 0.01, H: less than or equal to 0.01, the balance being Ta, the sum of the mass percentages of all the groups being 100 percent, carrying out batching, smelting by using a vacuum induction furnace and electroslag remelting to obtain cast ingots, and rolling into tantalum metal bars, wherein the tantalum metal bars conform to the current tantalum (Ta) metal standard: GB/T14841-2008 requirements; carrying out finish turning on the smelted tantalum (Ta) metal rod to obtain a tantalum (Ta) metal electrode rod, removing iron scales to obtain a metal electrode rod meeting the requirements of a plasma rotary electrode atomization powder process, wherein the density of the metal electrode rod is 99%, casting defects such as obvious looseness and shrinkage cavity do not exist, the diameter of the processed tantalum metal electrode rod is 30mm, the degree is 160mm, the roundness deviation is 0.05mm, the straightness deviation is 0.01mm, and the roughness is 1 mu m;
s2, placing the tantalum metal bar in a plasma rotary electrode atomization powder making device, holding the tantalum metal bar on a bar selecting and loading and axial moving mechanical device to form a novel dynamic sealing structure, and after the pre-vacuumizing treatment is carried out on the whole set of powder making equipment, when the vacuum degree of the vacuum treatment is 3 multiplied by 10 -3 After Pa, introducing a protective gas which is a mixed gas of helium and argon to ensure that the pressure in the chamber reaches 0.1X10 -5 Pa, ensure gasOxygen content in the atmosphere is less than 0.1wt%;
setting the working voltage to 80V, setting the melting current to 1000A, adjusting the rotating speed of the bar to 32000r/min, starting an atomization function and igniting a plasma generator, heating the end face of the high-speed rotating tantalum metal electrode bar by a plasma gun to uniformly melt the electrode bar and throwing out the electrode bar at a high speed by virtue of centrifugal force generated by rotation, rapidly cooling liquid into spherical particles in an inert gas environment, classifying and collecting the condensed powder particles under the protection of inert gas, vacuum packaging after screening, and finally collecting the spherical powder of Ta metal.
The particle size of the Ta metal powder is 20-95 mu m, and the specific particle size distribution is as follows: fluidity of 35 μm to 70 μm: 5.63/50g, bulk density 10.63g/cm 3 Tap density 10.32g/cm 3 。
Examination of the microstructure of the tantalum metal prepared in examples 1-3 was performed and FIG. 2 is a scanning electron microscope image of the tantalum powder prepared in example 1 of the present invention. As shown in FIG. 2, the tantalum metal has high sphericity, the powder particle size distribution is relatively uniform, and the particle size is mainly 35-65 μm.
Compared with the prior art of Ta metal spherical powder such as Yang Kun, etc., the research progress of additive manufacturing tantalum and porous tantalum, the bulk density of the Ta metal spherical powder is generally 4.23g/cm 3 The sphericity of the powder is 89%, fig. 3 is a high-power scanning diagram of the tantalum powder prepared in the embodiment 1 of the invention, and as shown in fig. 3, the sphericity of the tantalum metal of the tantalum powder prepared in the embodiment 1 of the invention is high and reaches more than 98%, satellite powder and hollow powder are not seen, and the loose density and tap density are good, so that the tantalum powder is suitable for being used in an electron beam powder spreading type additive manufacturing process.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (8)
1. The method for preparing tantalum powder by gas atomization of the plasma rotary electrode is characterized by comprising the following steps of:
s1, smelting by using a vacuum induction furnace according to the component proportion of the tantalum metal bar to obtain an ingot, and then processing to prepare the tantalum metal bar;
s2, placing the tantalum metal bar in a plasma rotary electrode atomization powder making device, sealing, vacuumizing, introducing protective gas, adding the end part of the tantalum metal bar by using a plasma gun, uniformly melting the tantalum metal bar, rotating to generate centrifugal force to throw out liquid drop-shaped metal, condensing and spheroidizing the tantalum metal bar in the protective gas at the rotating speed of 30000-42000 r/min to obtain particle powder, and drying and sieving to obtain the tantalum powder.
2. The method for preparing tantalum powder by gas atomization of a plasma rotary electrode according to claim 1, wherein in S1, the tantalum metal bar has a composition of C:0.01 to 0.02, O:0.01 to 0.02, N: less than or equal to 0.01, H: less than or equal to 0.01, and the balance of Ta.
3. The method for preparing tantalum powder by gas atomization of a plasma rotary electrode according to claim 1, wherein in S1, the diameter of the tantalum metal bar is 30-50 mm, the length is 160-200 mm, the surface roughness is less than or equal to 1 μm, the roundness deflection angle of the tantalum metal bar is not more than 0.05mm, the linear deflection is not more than 0.01mm, and the relative density is not less than 99%.
4. The method for preparing tantalum powder by gas atomization of a plasma rotary electrode according to claim 1, wherein in S2, when the vacuum degree of the vacuum treatment is 3 to 10X 10 -3 After Pa, the pressure after the protective gas is introduced is 0.1 to 1 multiplied by 10 -5 Pa; the shielding gas is argon.
5. The method for preparing tantalum powder by gas atomization of a plasma rotary electrode according to claim 1, wherein in S2, the oxygen content in the environment after the shielding gas is introduced is less than 0.1wt%.
6. The method for preparing tantalum powder by gas atomization of a plasma rotary electrode according to claim 1, wherein in S2, the current of the plasma gun is 800-1000A and the voltage is 80V.
7. The method for preparing tantalum powder by gas atomization of a plasma rotary electrode according to claim 1, wherein in S2, the distance between the atomizing electrode rod and the plasma gun is 10mm, the feeding speed is 1.2mm/S, and the working gas flow rate of the plasma is 120m 3 /h。
8. The method for preparing tantalum powder by gas atomization of a plasma rotary electrode according to claim 1, wherein in S2, the particle size of said tantalum powder after sieving is 10-90 μm, the fluidity is (5-7)/50 g, and the bulk density is 10.58-10.63g/cm 3 Tap density of 10.5-10.8g/cm 3 。
Priority Applications (1)
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| US4474604A (en) * | 1982-04-30 | 1984-10-02 | Hitachi Metals, Ltd. | Method of producing high-grade metal or alloy powder |
| US20080118391A1 (en) * | 2006-10-30 | 2008-05-22 | Niotan, Inc. | Method and an Apparatus of Plasma Processing of Tantalum Particles |
| CN106735280A (en) * | 2016-11-23 | 2017-05-31 | 西北有色金属研究院 | A kind of preparation method of spherical TiTa alloy powders |
| CN107876794A (en) * | 2017-12-21 | 2018-04-06 | 西安欧中材料科技有限公司 | The Mo powder of increasing material manufacturing, the preparation method of Mo alloy spherical powder |
| CN108620598A (en) * | 2018-06-26 | 2018-10-09 | 西安赛隆金属材料有限责任公司 | A kind of preparation method of tantalum powder |
| WO2023272871A1 (en) * | 2021-06-30 | 2023-01-05 | 宁夏东方钽业股份有限公司 | Tantalum-tungsten alloy powder and preparation method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4474604A (en) * | 1982-04-30 | 1984-10-02 | Hitachi Metals, Ltd. | Method of producing high-grade metal or alloy powder |
| US20080118391A1 (en) * | 2006-10-30 | 2008-05-22 | Niotan, Inc. | Method and an Apparatus of Plasma Processing of Tantalum Particles |
| CN106735280A (en) * | 2016-11-23 | 2017-05-31 | 西北有色金属研究院 | A kind of preparation method of spherical TiTa alloy powders |
| CN107876794A (en) * | 2017-12-21 | 2018-04-06 | 西安欧中材料科技有限公司 | The Mo powder of increasing material manufacturing, the preparation method of Mo alloy spherical powder |
| CN108620598A (en) * | 2018-06-26 | 2018-10-09 | 西安赛隆金属材料有限责任公司 | A kind of preparation method of tantalum powder |
| WO2023272871A1 (en) * | 2021-06-30 | 2023-01-05 | 宁夏东方钽业股份有限公司 | Tantalum-tungsten alloy powder and preparation method therefor |
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