CN117000993B - Preparation method of tantalum powder for metal additive manufacturing - Google Patents
Preparation method of tantalum powder for metal additive manufacturing Download PDFInfo
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- CN117000993B CN117000993B CN202310979189.2A CN202310979189A CN117000993B CN 117000993 B CN117000993 B CN 117000993B CN 202310979189 A CN202310979189 A CN 202310979189A CN 117000993 B CN117000993 B CN 117000993B
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 170
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 44
- 239000002184 metal Substances 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 39
- 239000000654 additive Substances 0.000 title claims abstract description 37
- 230000000996 additive effect Effects 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 120
- 239000007789 gas Substances 0.000 claims abstract description 79
- 238000005243 fluidization Methods 0.000 claims abstract description 77
- 239000000843 powder Substances 0.000 claims abstract description 65
- 239000012159 carrier gas Substances 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 238000007873 sieving Methods 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 78
- 229910052786 argon Inorganic materials 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 26
- 239000001307 helium Substances 0.000 claims description 12
- 229910052734 helium Inorganic materials 0.000 claims description 12
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 12
- 230000000052 comparative effect Effects 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 8
- 239000012300 argon atmosphere Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000012216 screening Methods 0.000 description 5
- 229910052715 tantalum Inorganic materials 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000001360 synchronised effect Effects 0.000 description 3
- 238000010146 3D printing Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000003703 image analysis method Methods 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- RHDUVDHGVHBHCL-UHFFFAOYSA-N niobium tantalum Chemical compound [Nb].[Ta] RHDUVDHGVHBHCL-UHFFFAOYSA-N 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
Classifications
-
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- 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
- 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
-
- 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
Abstract
The invention relates to a preparation method of tantalum powder for metal additive manufacturing, which belongs to the technical field of metal powder and comprises the following steps: firstly, carrying out fluidization treatment on raw material tantalum powder, so that most of tantalum powder with the particle size smaller than 5 mu m can be adhered to the surface of large particles, and the fluidization treatment tantalum powder with narrower particle size distribution is obtained; then sieving the fluidization tantalum powder to obtain four fluidization tantalum powder with particle size ranges; finally, setting different powder feeding rates, carrier gas flow rates, plasma power, reaction chamber pressure and plasma working gas flow rates according to the particle size range of the fluidization treatment tantalum powder, and obtaining the tantalum powder for metal additive manufacturing. According to the technical scheme, the preparation method of the tantalum powder for metal additive manufacturing provided by the invention has the advantages that the tantalum powder yield is obviously improved, the spheroidization rate is improved, the generation of oversized particles and satellite balls is avoided, and the fluidity of the tantalum powder is improved.
Description
Technical Field
The invention belongs to the technical field of metal powder, and particularly relates to a preparation method of tantalum powder for metal additive manufacturing.
Background
Compared with the traditional manufacturing technology, the additive manufacturing technology commonly called 3D printing has the advantages of high molding precision, no need of post-treatment, short production period, high material utilization rate, capability of being individually designed and the like, and has important application prospects in the fields of aviation, aerospace, biomedicine and the like. With the development of 3D printing technology, metal powder materials have become important factors restricting the development of the materials, and the requirements on the performance of the metal powder are higher and higher.
The metal tantalum has the advantages of biocompatibility, excellent mechanical property, high corrosion resistance and the like, and has important application in the fields of national defense, military industry, biomedical treatment and the like. The tantalum powder for metal additive manufacturing needs to have the advantages of high spheroidization rate, narrow particle size distribution, low oxygen content and the like. At present, the radio frequency plasma spheroidization technology is often used for preparing various high-performance and high-quality spherical powders, and the metal powder prepared by the radio frequency plasma spheroidization technology has higher spheroidization rate and narrower particle size distribution, but the powder raw material with wider particle size distribution is lower in yield after being subjected to radio frequency plasma spheroidization treatment, so that the method is not beneficial to industrial production.
Disclosure of Invention
The invention aims to provide a preparation method of tantalum powder for metal additive manufacturing, which comprises the steps of firstly carrying out fluidization treatment on raw material tantalum powder, so that most of tantalum powder with the particle size smaller than 5 mu m can be adhered to the surfaces of large particles, and fluidization treatment tantalum powder with narrower particle size distribution is obtained; then sieving the fluidization tantalum powder to obtain four fluidization tantalum powder with particle size ranges; finally, different powder feeding rates, carrier gas flow rates, plasma power, reaction chamber pressure and plasma working gas flow rates are set according to the particle size range of the fluidization tantalum powder, so that the tantalum powder yield is remarkably improved, the spheroidization rate is improved, the generation of oversized particles and satellite balls is avoided, and the fluidity of the tantalum powder is improved.
The invention aims to solve the technical problems: at present, the radio frequency plasma spheroidization technology is often used for preparing various high-performance and high-quality spherical powders, and the metal powder prepared by the radio frequency plasma spheroidization technology has higher spheroidization rate and narrower particle size distribution, but the powder raw material with wider particle size distribution is lower in yield after being subjected to radio frequency plasma spheroidization treatment, so that the method is not beneficial to industrial production.
The aim of the invention can be achieved by the following technical scheme:
a preparation method of tantalum powder for metal additive manufacturing comprises the following steps:
a1, introducing raw material tantalum powder into a fluidized bed reactor, and treating for 8-15min under the inert gas atmosphere and the 390-420 ℃ condition to obtain fluidization treatment tantalum powder;
further, in step A1, the inert gas is argon.
Further, in the step A1, the purity of the raw material tantalum powder is 99.90-99.99%.
Further, in the step A1, the oxygen content of the raw tantalum powder is 500-800ppm.
Further, in the step A1, the grain size of the raw material tantalum powder is in the range of 1-120 μm.
In the operation process, the raw material tantalum powder is subjected to fluidization treatment, collision and friction occur among tantalum particles in the fluidization process, and the impact pressure among the particles in the collision process is far lower than the deformation yield strength of the tantalum powder at 390-420 ℃, so that the tantalum particles hardly deform in the fluidization process, but under the high-temperature condition, the tantalum particles with the particle size smaller than 5 mu m are easier to adhere to the surfaces of large particles along with the occurrence of collision and friction, so that the particle size distribution is narrowed.
A2, sieving the fluidization tantalum powder to obtain four fluidization tantalum powder with particle size ranges;
further, in step A2, the four particle sizes are in the range of 1-5 μm, 6-10 μm, 11-15 μm and more than 15 μm, respectively.
And A3, passing the fluidization tantalum powder into an incident frequency plasma device for plasma spheroidization treatment to obtain the tantalum powder for metal additive manufacturing.
Further, in the step A3, in the stage of plasma spheroidization, different powder feeding rates, carrier gas flows, plasma power, reaction chamber pressures and plasma working gas flows are set according to the particle size range of the fluidized tantalum powder.
Further, in the stage of plasma spheroidizing, the powder feeding rate of the fluidization tantalum powder with the particle size range of 1-5 μm is 55-70g/min, the carrier gas flow is 11-15L/min, the plasma power is 7-11kW, the pressure of the reaction chamber is 95-102kPa, the central gas flow is 12-16L/min, and the sheath gas flow is 90-105L/min.
Further, in the stage of plasma spheroidizing, the powder feeding rate of the fluidization tantalum powder with the particle size ranging from 6 μm to 10 μm is 48g/min to 60g/min, the carrier gas flow is 7L/min to 11L/min, the plasma power is 16kW to 25kW, the pressure of the reaction chamber is 93kPa to 108kPa, the central gas flow is 15L/min to 19L/min, and the sheath gas flow is 100L/min to 110L/min.
Further, in the stage of plasma spheroidizing, the powder feeding rate of the fluidization tantalum powder with the particle size range of 11-15 μm is 29-45g/min, the carrier gas flow is 3-8L/min, the plasma power is 30-40kW, the pressure of the reaction chamber is 85-95kPa, the central gas flow is 20-28L/min, and the sheath gas flow is 115-120L/min.
Further, in the stage of plasma spheroidizing, the powder feeding rate of the fluidization tantalum powder with the particle size range of more than 15 mu m is 10-25g/min, the carrier gas flow is 2-7L/min, the plasma power is 40-55kW, the pressure of the reaction chamber is 75-85kPa, the central gas flow is 10-25L/min, and the sheath gas flow is 80-105L/min.
Further, the carrier gas is argon.
Further, the central gas comprises argon.
Further, the central gas includes argon and hydrogen.
Further, the volume ratio of the argon to the hydrogen is 1-3:1.
further, the sheath gas includes argon.
Further, the sheath gas includes argon and helium.
Further, the volume ratio of the argon to the helium is 2-10:1.
in the operation process, the four kinds of fluidization tantalum powder with particle size ranges are subjected to plasma spheroidization under different technological parameters, so that the tantalum powder yield can be improved. When tantalum powder with wider particle size distribution is directly placed into radio frequency plasma equipment to carry out plasma spheroidization, the heat required by melting tantalum powder with different particle sizes is different, in order to ensure that tantalum powder with larger particle sizes can be fully melted, the powder feeding rate is generally lower, the number of particles entering the plasma torch in unit time is less under the lower powder feeding rate, the heat absorbed by single particles is more, when tantalum powder with different particle sizes carries out plasma spheroidization under the same technological parameters, tantalum powder with smaller particle sizes can be evaporated due to the excessive heat absorbed, so that the powder yield is reduced, meanwhile, the particles with different particle sizes collide, and the small particles can adhere to the surfaces of large particles to form satellite balls. Therefore, the invention creatively divides tantalum powder into four particle size ranges, tantalum powder with the particle size smaller than 5 mu m uses higher powder feeding speed, so that the heat absorbed by single particles is reduced, evaporation is not easy, but the powder is agglomerated due to the higher powder feeding speed, and then larger particles are generated by melting, and the particles are too large and are not suitable for metal additive manufacturing. In the invention, the plasma spheroidizing process of the tantalum powder with the particle size smaller than 5 mu m is not easy to control, so that the raw material tantalum powder is firstly fluidized before plasma spheroidizing, so that most of the tantalum powder with the particle size smaller than 5 mu m can be adsorbed on the surface of large particles, and the tantalum powder adsorbed with small particles is melted into large liquid drops when entering a plasma torch and then is quenched into spherical particles, and in addition, the generation of satellite balls can be reduced.
Corresponding technological parameters are also set for tantalum powder with the particle size ranging from 6 to 10 mu m, 11 to 15 mu m and larger than 15 mu m, and the corresponding powder feeding speed is lower when the particle size is larger, so that the tantalum powder can be fully melted to form particles with high sphericity, the spheroidization rate is improved, meanwhile, the evaporation caused by the absorption of excessive heat by the particles with smaller particle size is avoided, and the powder yield is improved. In addition, because the powder feeding rate of large particles is low, the collision probability can be reduced, the generation of oversized particles is avoided, and the fluidity of tantalum powder is improved.
The invention has the beneficial effects that:
(1) According to the technical scheme, the tantalum powder is creatively divided into four particle size ranges, different powder feeding rates, carrier gas flow rates, plasma power, reaction chamber pressure and plasma working gas flow rates are set according to the particle size ranges of the tantalum powder, the tantalum powder yield is remarkably improved, the spheroidization rate is improved, oversized particles and satellite balls are avoided, and the fluidity of the tantalum powder is improved.
(2) In the technical scheme of the invention, because the tantalum powder with the grain diameter smaller than 5 mu m is not easy to control in the plasma spheroidizing process, the tantalum powder is easy to evaporate or escape from a high-temperature area, so that the powder yield is reduced or the spheroidizing rate is reduced, the tantalum powder is subjected to fluidization treatment before the plasma spheroidizing process, so that most of the tantalum powder with the grain diameter smaller than 5 mu m can be adhered to the surface of large particles, the powder yield is improved, and the grain size distribution of the finally obtained tantalum powder for manufacturing the metal additive is narrowed.
(3) In the technical scheme of the invention, corresponding technological parameters are also arranged for tantalum powder with the particle size ranging from 6 to 10 mu m, from 11 to 15 mu m and larger than 15 mu m, and the corresponding powder feeding speed is lower when the particle size is larger, so that the tantalum powder can be fully melted to form particles with high sphericity, the spheroidization rate is improved, meanwhile, evaporation caused by excessive heat absorption by the particles with smaller particle size is avoided, and the powder yield is improved. In addition, because the powder feeding rate of large particles is low, the collision probability can be reduced, the generation of oversized particles is avoided, and the fluidity of tantalum powder is improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. 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.
Example 1
A preparation method of tantalum powder for metal additive manufacturing comprises the following steps:
a1, introducing raw material tantalum powder with the purity of 99.90% into a fluidized bed reactor, wherein the oxygen content of the raw material tantalum powder is 512ppm, the particle size range is 1-120 mu m, and treating for 8min under the argon atmosphere and the 390 ℃ to obtain fluidization treatment tantalum powder;
a2, screening the fluidization tantalum powder to obtain four fluidization tantalum powder with particle size ranges of 1-5 mu m, 6-10 mu m, 11-15 mu m and more than 15 mu m;
a3, passing the fluidization tantalum powder into an incident frequency plasma device to carry out plasma spheroidization treatment to obtain tantalum powder for metal additive manufacturing;
setting powder feeding speed of fluidization tantalum powder with particle size ranging from 1 μm to 5 μm at 55g/min, carrier gas flow of 11L/min, plasma power of 7kW, reaction chamber pressure of 95kPa, central gas flow of 12L/min and sheath gas flow of 90L/min in a plasma spheroidizing stage;
setting the powder feeding speed of the fluidization treatment tantalum powder with the particle size ranging from 6 mu m to 10 mu m to be 48g/min, the carrier gas flow to be 7L/min, the plasma power to be 16kW, the pressure of the reaction chamber to be 93kPa, the central gas flow to be 15L/min and the sheath gas flow to be 100L/min;
setting the powder feeding speed of the fluidization treatment tantalum powder with the particle size range of 11-15 mu m to be 29g/min, the carrier gas flow to be 3L/min, the plasma power to be 30kW, the pressure of the reaction chamber to be 85kPa, the central gas flow to be 20L/min and the sheath gas flow to be 115L/min;
the powder feeding rate of the fluidization tantalum powder with the particle size range larger than 15 mu m is set to be 10g/min, the carrier gas flow is 2L/min, the plasma power is 40kW, the pressure of the reaction chamber is 75kPa, the central gas flow is 10L/min, and the sheath gas flow is 80L/min.
The carrier gas is argon; the central gas is argon; the sheath gas is argon.
Example 2
A preparation method of tantalum powder for metal additive manufacturing comprises the following steps:
a1, introducing raw material tantalum powder with the purity of 99.92% into a fluidized bed reactor, wherein the oxygen content of the raw material tantalum powder is 591ppm, the particle size range is 1-120 mu m, and treating for 10min under the argon atmosphere and 400 ℃ to obtain fluidization treatment tantalum powder;
a2, screening the fluidization tantalum powder to obtain four fluidization tantalum powder with particle size ranges of 1-5 mu m, 6-10 mu m, 11-15 mu m and more than 15 mu m;
a3, passing the fluidization tantalum powder into an incident frequency plasma device to carry out plasma spheroidization treatment to obtain tantalum powder for metal additive manufacturing;
in the stage of plasma spheroidizing, setting the powder feeding rate of the fluidization treatment tantalum powder with the particle size range of 1-5 mu m to be 60g/min, the carrier gas flow to be 12L/min, the plasma power to be 8kW, the pressure of a reaction chamber to be 98kPa, the central gas flow to be 13L/min and the sheath gas flow to be 92L/min;
setting the powder feeding speed of the fluidization treatment tantalum powder with the particle size ranging from 6 mu m to 10 mu m to be 50g/min, the carrier gas flow to be 8L/min, the plasma power to be 18kW, the pressure of a reaction chamber to be 95kPa, the central gas flow to be 16L/min and the sheath gas flow to be 102L/min;
setting the powder feeding speed of the fluidization treatment tantalum powder with the particle size range of 11-15 mu m to be 31g/min, the carrier gas flow to be 4L/min, the plasma power to be 32kW, the reaction chamber pressure to be 87kPa, the central gas flow to be 22L/min and the sheath gas flow to be 116L/min;
the powder feeding rate of the fluidization tantalum powder with the particle size range larger than 15 μm is set to be 13g/min, the carrier gas flow is 3L/min, the plasma power is 43kW, the pressure of the reaction chamber is 78kPa, the central gas flow is 14L/min, and the sheath gas flow is 87L/min.
The carrier gas is argon; the central gas is argon and hydrogen, and the volume ratio of the argon to the hydrogen is 1:1, a step of; the sheath gas is argon and helium, and the volume ratio of the argon to the helium is 2:1.
example 3
A preparation method of tantalum powder for metal additive manufacturing comprises the following steps:
a1, introducing raw material tantalum powder with the purity of 99.95% into a fluidized bed reactor, wherein the oxygen content of the raw material tantalum powder is 569ppm, the particle size range is 1-120 mu m, and treating for 10min under the argon atmosphere and 400 ℃ to obtain fluidization treatment tantalum powder;
a2, screening the fluidization tantalum powder to obtain four fluidization tantalum powder with particle size ranges of 1-5 mu m, 6-10 mu m, 11-15 mu m and more than 15 mu m;
a3, passing the fluidization tantalum powder into an incident frequency plasma device to carry out plasma spheroidization treatment to obtain tantalum powder for metal additive manufacturing;
in the stage of plasma spheroidizing, setting the powder feeding rate of the fluidization treatment tantalum powder with the particle size range of 1-5 mu m to be 60g/min, the carrier gas flow to be 13L/min, the plasma power to be 9kW, the pressure of a reaction chamber to be 98kPa, the central gas flow to be 14L/min and the sheath gas flow to be 99L/min;
setting the powder feeding speed of the fluidization treatment tantalum powder with the particle size ranging from 6 mu m to 10 mu m to be 55g/min, the carrier gas flow to be 9L/min, the plasma power to be 20kW, the pressure of the reaction chamber to be 100kPa, the central gas flow to be 17L/min and the sheath gas flow to be 105L/min;
setting the powder feeding speed of the fluidization treatment tantalum powder with the particle size range of 11-15 mu m to be 36g/min, the carrier gas flow to be 6L/min, the plasma power to be 35kW, the reaction chamber pressure to be 90kPa, the central gas flow to be 26L/min and the sheath gas flow to be 117L/min;
the powder feeding rate of the fluidization tantalum powder with the particle size range larger than 15 μm is set to be 16g/min, the carrier gas flow is 5L/min, the plasma power is 48kW, the pressure of the reaction chamber is 81kPa, the central gas flow is 18L/min, and the sheath gas flow is 97L/min.
The carrier gas is argon; the central gas is argon and hydrogen, and the volume ratio of the argon to the hydrogen is 2:1, a step of; the sheath gas is argon and helium, and the volume ratio of the argon to the helium is 5:1.
example 4
A preparation method of tantalum powder for metal additive manufacturing comprises the following steps:
a1, introducing raw material tantalum powder with purity of 99.97% into a fluidized bed reactor, wherein the oxygen content of the raw material tantalum powder is 736ppm, the particle size range is 1-120 mu m, and treating for 12min under argon atmosphere and 410 ℃ to obtain fluidization treatment tantalum powder;
a2, screening the fluidization tantalum powder to obtain four fluidization tantalum powder with particle size ranges of 1-5 mu m, 6-10 mu m, 11-15 mu m and more than 15 mu m;
a3, passing the fluidization tantalum powder into an incident frequency plasma device to carry out plasma spheroidization treatment to obtain tantalum powder for metal additive manufacturing;
setting the powder feeding rate of the fluidization tantalum powder with the particle size range of 1-5 mu m to be 67g/min, the carrier gas flow to be 14L/min, the plasma power to be 10kW, the pressure of the reaction chamber to be 100kPa, the central gas flow to be 15L/min and the sheath gas flow to be 102L/min in the plasma spheroidizing stage;
setting the powder feeding speed of the fluidization treatment tantalum powder with the particle size ranging from 6 mu m to 10 mu m to 57g/min, the carrier gas flow rate to 10L/min, the plasma power to 21kW, the reaction chamber pressure to 102kPa, the central gas flow rate to 18L/min and the sheath gas flow rate to 107L/min;
setting the powder feeding speed of the fluidization treatment tantalum powder with the particle size range of 11-15 mu m to be 42g/min, the carrier gas flow to be 7L/min, the plasma power to be 38kW, the reaction chamber pressure to be 92kPa, the central gas flow to be 27L/min and the sheath gas flow to be 118L/min;
the powder feeding rate of the fluidization tantalum powder with the particle size range larger than 15 μm is set to be 22g/min, the carrier gas flow is 6L/min, the plasma power is 51kW, the pressure of the reaction chamber is 83kPa, the central gas flow is 20L/min, and the sheath gas flow is 100L/min.
The carrier gas is argon; the central gas is argon and hydrogen, and the volume ratio of the argon to the hydrogen is 2.5:1, a step of; the sheath gas is argon and helium, and the volume ratio of the argon to the helium is 7:1.
example 5
A preparation method of tantalum powder for metal additive manufacturing comprises the following steps:
a1, introducing raw material tantalum powder with the purity of 99.99% into a fluidized bed reactor, wherein the oxygen content of the raw material tantalum powder is 793ppm, the particle size range is 1-120 mu m, and treating for 15min under the argon atmosphere and 420 ℃ to obtain fluidized tantalum powder;
a2, screening the fluidization tantalum powder to obtain four fluidization tantalum powder with particle size ranges of 1-5 mu m, 6-10 mu m, 11-15 mu m and more than 15 mu m;
a3, passing the fluidization tantalum powder into an incident frequency plasma device to carry out plasma spheroidization treatment to obtain tantalum powder for metal additive manufacturing;
in the stage of plasma spheroidizing, setting the powder feeding rate of the fluidization tantalum powder with the particle size range of 1-5 mu m to be 70g/min, the carrier gas flow to be 15L/min, the plasma power to be 11kW, the pressure of a reaction chamber to be 102kPa, the central gas flow to be 16L/min and the sheath gas flow to be 105L/min;
setting the powder feeding speed of the fluidization treatment tantalum powder with the particle size ranging from 6 mu m to 10 mu m to be 60g/min, the carrier gas flow to be 11L/min, the plasma power to be 25kW, the pressure of the reaction chamber to be 108kPa, the central gas flow to be 19L/min and the sheath gas flow to be 110L/min;
setting the powder feeding rate of the fluidization tantalum powder with the particle size range of 15 mu m to be 45g/min, the carrier gas flow to be 8L/min, the plasma power to be 40kW, the reaction chamber pressure to be 95kPa, the central gas flow to be 28L/min and the sheath gas flow to be 120L/min;
the powder feeding rate of the fluidization tantalum powder with the particle size range larger than 15 μm is set to be 25g/min, the carrier gas flow is 7L/min, the plasma power is 55kW, the pressure of the reaction chamber is 85kPa, the central gas flow is 25L/min, and the sheath gas flow is 105L/min.
The carrier gas is argon; the central gas is argon and hydrogen, and the volume ratio of the argon to the hydrogen is 3:1, a step of; the sheath gas is argon and helium, and the volume ratio of the argon to the helium is 10:1.
comparative example 1
In comparison with example 3, the tantalum powder of comparative example 1 was not subjected to fluidization treatment, and the other steps and raw materials were synchronized with example 3.
Comparative example 2
In comparison with example 3, comparative example 2 was not classified into four kinds of particle size ranges of the fluidization tantalum powder, but the fluidization tantalum powder was directly uniformly placed in a radio frequency plasma apparatus to perform plasma spheroidization, and the process parameters in the plasma spheroidization stage were the same as those of the tantalum powder having a particle size range of 11 to 15 μm, and the other steps and raw materials were synchronized with example 3.
Comparative example 3
In comparison with example 3, in comparative example 3, the fluidization tantalum powder was not classified into four kinds of fluidization tantalum powder having a particle size range, but the fluidization tantalum powder was directly uniformly placed in a radio frequency plasma apparatus to perform plasma spheroidization, and the process parameters in the plasma spheroidization stage were the same as those of tantalum powder having a particle size range of more than 15 μm, and other steps and raw materials were synchronized with example 3.
The tantalum powders for metal additive manufacturing prepared in examples 1 to 5 and comparative examples 1 to 3 were now subjected to performance test, and the results are shown in Table 1.
And (3) performance detection:
(1) Powder yield: weighing (a) raw material tantalum powder, then weighing (b) the finally prepared tantalum powder for metal additive manufacturing, and calculating the yield according to a formula (b is 100%)/a;
(2) Spheroidization rate: measuring the ratio of spherical powder in the prepared tantalum powder for metal additive manufacturing by adopting an image analysis method;
(3) Particle size distribution: according to the standard of GB/T1480-2012 particle size determination by metal powder dry sieving method and GB/T19077-2016 particle size analysis laser diffraction method;
(4) Oxygen content: the detection is carried out according to the standard of GB/T15076.14-2008 'determination of oxygen content of tantalum-niobium chemical analysis method'.
TABLE 1
As can be seen from the data in Table 1, the tantalum powder prepared by the preparation method provided by the invention has high yield, the prepared tantalum powder for metal additive manufacturing has higher spheroidization rate and narrow granularity division, and meanwhile, the oxygen content is obviously reduced, so that the tantalum powder is very suitable for the metal additive manufacturing technology.
As can be seen from the data of comparative example 3 and comparative example 1, the tantalum powder for metal additive manufacturing prepared in comparative example 1 has lower powder yield and spheroidization rate, which should be due to the fact that the tantalum powder having a small particle size evaporates or does not melt during the plasma spheroidization treatment, i.e., escapes from the high temperature zone, resulting in a decrease in powder yield and spheroidization rate.
As can be seen from the data of comparative example 3 and comparative examples 2 and 3, the fluidization tantalum powder was sieved into four particle size ranges and subjected to plasma spheroidization treatment, respectively, so that the powder yield and spheroidization rate were significantly improved, and the particle size distribution was also significantly narrowed, which means that the powder with different particle sizes was treated separately to avoid evaporation of small-sized particles or escape from the high-temperature zone, and at the same time, agglomeration of large particles into oversized particles was also suppressed.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (7)
1. A preparation method of tantalum powder for metal additive manufacturing is characterized by comprising the following steps: the method comprises the following steps:
a1, introducing raw material tantalum powder into a fluidized bed reactor, and treating for 8-15min under the inert gas atmosphere and the 390-420 ℃ condition to obtain fluidization treatment tantalum powder;
a2, sieving the fluidization tantalum powder to obtain four fluidization tantalum powder with particle size ranges;
a3, passing the fluidization tantalum powder into an incident frequency plasma device to carry out plasma spheroidization treatment to obtain tantalum powder for metal additive manufacturing;
in the step A1, the grain size range of the raw material tantalum powder is 1-120 mu m;
in the step A2, the four particle sizes are respectively 1-5 mu m, 6-10 mu m, 11-15 mu m and more than 15 mu m;
in the step A3, in the stage of plasma spheroidizing, different powder feeding rates, carrier gas flow rates, plasma power, reaction chamber pressure and plasma working gas flow rates are set according to the particle size range of the fluidized tantalum powder.
2. The method for preparing tantalum powder for metal additive manufacturing according to claim 1, wherein the method comprises the following steps: in the plasma spheroidizing stage, the powder feeding rate of the fluidization tantalum powder with the particle size range of 1-5 mu m is 55-70g/min, the carrier gas flow is 11-15L/min, the plasma power is 7-11kW, the pressure of a reaction chamber is 95-102kPa, the central gas flow is 12-16L/min, and the sheath gas flow is 90-105L/min.
3. The method for preparing tantalum powder for metal additive manufacturing according to claim 1, wherein the method comprises the following steps: in the plasma spheroidizing stage, the powder feeding rate of the fluidization tantalum powder with the particle size ranging from 6 mu m to 10 mu m is 48g/min to 60g/min, the carrier gas flow is 7L/min to 11L/min, the plasma power is 16kW to 25kW, the pressure of a reaction chamber is 93kPa to 108kPa, the central gas flow is 15L/min to 19L/min, and the sheath gas flow is 100L/min to 110L/min.
4. The method for preparing tantalum powder for metal additive manufacturing according to claim 1, wherein the method comprises the following steps: in the plasma spheroidizing stage, the powder feeding rate of the fluidization tantalum powder with the particle size range of 11-15 mu m is 29-45g/min, the carrier gas flow is 3-8L/min, the plasma power is 30-40kW, the pressure of a reaction chamber is 85-95kPa, the central gas flow is 20-28L/min, and the sheath gas flow is 115-120L/min.
5. The method for preparing tantalum powder for metal additive manufacturing according to claim 1, wherein the method comprises the following steps: in the plasma spheroidizing stage, the powder feeding rate of the fluidization tantalum powder with the particle size range of more than 15 mu m is 10-25g/min, the carrier gas flow is 2-7L/min, the plasma power is 40-55kW, the pressure of a reaction chamber is 75-85kPa, the central gas flow is 10-25L/min, and the sheath gas flow is 80-105L/min.
6. The method for preparing tantalum powder for metal additive manufacturing according to claim 1, wherein the method comprises the following steps: the carrier gas is argon, the central gas is argon, and the sheath gas is argon.
7. The method for preparing tantalum powder for metal additive manufacturing according to claim 1, wherein the method comprises the following steps: the carrier gas is argon; the central gas is argon and hydrogen, and the volume ratio of the argon to the hydrogen is 1-3:1, a step of; the sheath gas is argon and helium, and the volume ratio of the argon to the helium is 2-10:1.
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| CN114289722A (en) * | 2021-12-08 | 2022-04-08 | 北京科技大学 | Preparation method of fine-grained spherical tungsten powder |
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| WO2015023438A1 (en) * | 2013-08-12 | 2015-02-19 | United Technologies Corporation | Powder spheroidizing via fluidized bed |
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| CN107309434A (en) * | 2017-06-06 | 2017-11-03 | 中国航天空气动力技术研究院 | A kind of preparation method and application of the spherical molybdenum powder of high-purity compact |
| CN108907210A (en) * | 2018-07-27 | 2018-11-30 | 中南大学 | A method of increasing material manufacturing is prepared with solid globular metallic powder |
| CN111085690A (en) * | 2020-01-10 | 2020-05-01 | 北京矿冶科技集团有限公司 | Spherical rhenium powder plasma preparation method with high powder feeding rate, spherical rhenium powder and rhenium product |
| CN114289718A (en) * | 2021-12-08 | 2022-04-08 | 北京科技大学 | Method for efficiently preparing nano-pore porous tungsten product with complex shape |
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