CN113843415A - Tantalum-niobium alloy powder and preparation method thereof - Google Patents
Tantalum-niobium alloy powder and preparation method thereof Download PDFInfo
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- CN113843415A CN113843415A CN202111146735.1A CN202111146735A CN113843415A CN 113843415 A CN113843415 A CN 113843415A CN 202111146735 A CN202111146735 A CN 202111146735A CN 113843415 A CN113843415 A CN 113843415A
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- 239000000843 powder Substances 0.000 title claims abstract description 131
- 229910001257 Nb alloy Inorganic materials 0.000 title claims abstract description 82
- RHDUVDHGVHBHCL-UHFFFAOYSA-N niobium tantalum Chemical compound [Nb].[Ta] RHDUVDHGVHBHCL-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000010955 niobium Substances 0.000 claims abstract description 18
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 15
- 239000000956 alloy Substances 0.000 claims description 33
- 229910045601 alloy Inorganic materials 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 11
- -1 tantalum-niobium hydride Chemical compound 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 239000000654 additive Substances 0.000 abstract description 30
- 230000000996 additive effect Effects 0.000 abstract description 30
- 238000004519 manufacturing process Methods 0.000 abstract description 30
- 229910052758 niobium Inorganic materials 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 10
- 238000013461 design Methods 0.000 abstract description 3
- 238000005457 optimization Methods 0.000 abstract 2
- 239000001257 hydrogen Substances 0.000 description 38
- 229910052739 hydrogen Inorganic materials 0.000 description 38
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 24
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 16
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 16
- 229910052786 argon Inorganic materials 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000007789 gas Substances 0.000 description 12
- 238000002844 melting Methods 0.000 description 12
- 230000008018 melting Effects 0.000 description 12
- 229910052715 tantalum Inorganic materials 0.000 description 11
- 239000003870 refractory metal Substances 0.000 description 10
- 238000005086 pumping Methods 0.000 description 8
- 238000009832 plasma treatment Methods 0.000 description 7
- 238000012216 screening Methods 0.000 description 7
- 238000003723 Smelting Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000010894 electron beam technology Methods 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000006356 dehydrogenation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007943 implant Substances 0.000 description 3
- 238000010902 jet-milling Methods 0.000 description 3
- 229910001092 metal group alloy Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 229910001080 W alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000021164 cell adhesion Effects 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000004845 hydriding Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 229910000753 refractory alloy Inorganic materials 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000126 substance 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/023—Hydrogen absorption
-
- 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
-
- 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
According to the invention, aiming at the requirements of laser additive manufacturing, through component design optimization and preparation process optimization, hydrogenation treatment and plasma spheroidization technologies are organically combined, and Ta-Nb alloy with the mass percentage of 40-80% and Nb with the mass percentage of 20-60% is selected to prepare spherical tantalum-niobium alloy powder with the sphericity of more than or equal to 90%, so that the requirements of laser additive manufacturing can be met.
Description
Technical Field
The invention relates to the field of tantalum-niobium alloy, in particular to a tantalum-niobium alloy powder material for laser additive manufacturing and a preparation method thereof.
Technical Field
The additive manufacturing technology is one of rapid prototyping technologies, and is a technology for constructing a three-dimensional part by using materials such as metal powder or plastic and the like and by using a three-dimensional model as a basis and by means of scanning layer by layer and stacking layer by layer. The technology combines various disciplines such as CAD/CAM, optics, numerical control, material science and the like, has very wide application fields, has application prospects in jewelry, medical treatment, shoes, industrial design, construction, aerospace, automobiles, education and the like, and the main heat sources of common metal additive manufacturing equipment are laser and electron beams.
In the modern day of the increasingly developed material science, higher requirements are put forward on high-end metal materials, such as ultrahigh-speed aircrafts, nuclear industry heat conduction parts, high-temperature engines, gas turbines and the like, and the working temperature needs to be increased for improving the working efficiency and the stability. The traditional high-temperature resistant alloys such as cobalt-based alloys and nickel-based alloys almost reach the performance limit and are difficult to meet the use requirement at higher temperature. The refractory metal and the alloy thereof have the characteristics of high strength, high melting point, high temperature oxidation resistance and the like, and particularly maintain excellent performances of high strength, corrosion resistance and the like in a high-temperature environment of more than 1500 ℃, so that the refractory metal becomes a novel metal material for the high-temperature environment with the highest potential.
The refractory metals and the refractory metal alloys mainly refer to tungsten, molybdenum, tantalum, niobium and the refractory metal alloy materials, the melting point is above 2000 ℃, and the refractory metals and the refractory metal alloys have better high-temperature oxidation resistance and high-temperature corrosion resistance, and currently, most of the refractory metal materials are tungsten, molybdenum, tantalum, niobium and other simple substances and tungsten alloy materials. However, the refractory metal material is not easily machined and welded to be spliced in application due to its high melting point and high strength, so that the practical application of the refractory metal material is always limited, and with the development and popularization of additive manufacturing technology, the additive manufacturing technology can be used for forming complex metal components, thereby providing a brand new idea for the application of tantalum-niobium alloy, and the additive manufacturing technology has high requirements on the performance of raw materials and additive process parameters.
Because tantalum metal is a material with good biocompatibility and is commonly used for manufacturing artificial implants such as artificial bones and teeth, research on tantalum-niobium alloy is basically focused on the medical industry at present. The patent CN108500281A mainly utilizes the inlet plasma spheroidization to prepare the spherical powder of tantalum, niobium and tantalum-niobium alloy with the particle size of 25-180 mu m and is used for preparing medical instruments by 3D printing. In the scheme, the used powder is mainly spherical powder with large particle size and used for electron beam additive manufacturing, the powder has large particle size and cannot be used for a laser additive manufacturing technology, the electron beam additive manufacturing technology has poor forming precision, and part of fine structures cannot be formed.
Some manufacturers use easily prepared shaped powders for spherical powder replacement. Patent CN105855566A utilizes the methods of crushing, ball milling and later stage shaping to prepare polyhedral powder with certain regularity, which is used for additive manufacturing of medical implants. According to the technical scheme, when the part is manufactured in an additive manufacturing mode, due to the fact that the powder is polyhedral, defects such as cavities and fine cracks are prone to occurring on the surface of the formed part, but the requirement of the medical implant on the density of the formed part is not high, even the porous part is more suitable for cell adhesion and growth, and when the conventional part is manufactured, the part needs to be high in density and smooth in surface, and therefore the part is not suitable for conventional metal laser additive manufacturing.
The laser additive manufacturing has the advantages of high energy density and high processing precision, and the laser additive manufacturing method is the focus of current research on how to break through the difficult problem of laser additive manufacturing of tantalum-niobium alloy.
Disclosure of Invention
In view of the above, the invention prepares the spherical tantalum-niobium alloy powder with the sphericity of more than or equal to 90% by optimizing the component design and the preparation process according to the requirements of laser additive manufacturing. Can meet the requirements of laser additive manufacturing.
The invention provides tantalum-niobium alloy powder which comprises 40-80% of Ta and 20-60% of Nb in percentage by mass, wherein the particle size is 15-53 microns, the powder particle size D10-12-17 microns, D50-35 microns, D90-50-55 microns and the sphericity is more than or equal to 90% according to the requirements of conventional metal additive manufacturing equipment.
According to the tantalum-niobium alloy powder provided by the invention, the tantalum-niobium alloy powder further preferably comprises 55-65% of Ta and 45-35% of Nb by mass.
Because pure tantalum has high cost, in practical application, a certain amount of niobium is added into tantalum as an alloy element in consideration of cost, and because the two elements of tantalum and niobium belong to mutual infinite solid solution elements, the material cost can be reduced by increasing the content of niobium element on the premise of ensuring that the material performance meets the requirements. However, it has been found that too high a niobium content can seriously affect the workability and the balance of properties of the alloy product. The research shows that the components are between Ta40Nb60 and Ta80Nb20, and more preferably between Ta55Nb45 and Ta65N35, which is most beneficial to preparing the powder material with excellent performance by the method.
The invention also provides a preparation method of the tantalum-niobium alloy powder, which comprises the following steps:
s1, selecting a tantalum-niobium alloy containing 40-80% of Ta and 20-60% of Nb by mass, and hydrogenating the tantalum-niobium alloy to obtain a hydrogenated tantalum-niobium alloy;
s2, crushing the hydrogenated tantalum-niobium alloy to prepare hydrogenated tantalum-niobium alloy powder;
and S3, carrying out plasma treatment on the hydrogenated tantalum-niobium alloy powder to obtain the dehydrogenated tantalum-niobium alloy powder.
The method for preparing tantalum-niobium alloy powder according to the present invention further comprises a tantalum-niobium alloy preparation step before step S1.
According to the preparation method of the tantalum-niobium alloy powder, the melting points of the tantalum and the niobium are higher, so that the alloy ingot is preferably smelted by adopting an electric arc or electron beam smelting mode, and the tantalum-niobium alloy ingot is prepared after smelting. And then carrying out hydrogenation treatment on the tantalum-niobium alloy ingot.
According to the preparation method of the tantalum-niobium alloy powder, the hydrogenation method in the step S1 is as follows: and (3) carrying out hydrogenation treatment on the ingot by using high-temperature hydrogen atmosphere, and pressurizing and heating to hydrogenate the tantalum-niobium alloy ingot.
According to the preparation method of the tantalum-niobium alloy powder, the high-temperature hydrogen atmosphere refers to a hydrogen atmosphere with the temperature higher than 300 ℃. Further preferably, the high-temperature hydrogen atmosphere refers to a hydrogen atmosphere with a temperature higher than 340 ℃.
According to the method for preparing tantalum-niobium alloy powder, the pressure of hydrogen for hydrogenation in step S1 is more than 1.0 MPa.
It is understood that the purpose of step S1 is to hydrogenate the tantalum-niobium alloy, and that high temperature and low pressure methods may also be used for the hydriding. Researches show that the mode of using high temperature and high pressure has better technical effect.
According to the preparation method of the tantalum-niobium alloy powder, the crushing method in the step S2 is preferably implemented by physical crushing to obtain the primarily crushed tantalum-niobium hydride alloy powder, and then implemented by fluid milling to prepare the further crushed tantalum-niobium hydride alloy powder.
According to the preparation method of the tantalum-niobium alloy powder, the particle size of the tantalum-niobium alloy powder finally obtained in the step S2 is 10-60 microns.
According to the preparation method of the tantalum-niobium alloy powder, the hydrogenated tantalum-niobium alloy powder is subjected to plasma treatment in a mode that powder raw powder is put into direct-current plasma spheroidizing equipment, the hydrogenated powder is subjected to dehydrogenation and spheroidizing treatment by using direct-current plasma at high temperature, the powder is remelted, and the powder is made into a spherical shape when solidified by using the surface tension of a melt.
The processing environment of the powder in the plasma can be adjusted by further adjusting the material conveying speed and the length of the material feeding pipe, so that the powder with better sphericity can be obtained.
According to the preparation method of the tantalum-niobium alloy powder, the plasma treatment is carried out by combining direct-current level plasma spheroidization with high-pressure gas quenching. The plasma with high temperature is combined with the inert gas at normal temperature to cool, so that the nodularity of the powder is ensured to a greater degree, meanwhile, the nanometer micro powder generated by vaporization in the nodularization process of the powder is reduced, and the quality of the product is improved.
In a preferred embodiment, the feeding rate (powder feeding rate) of the tantalum-niobium alloy powder is preferably 50-100g/min, and more preferably 80 g/min.
According to the preparation method of the tantalum-niobium alloy powder, the length of the feeding pipe is 400-500 mm.
According to the preparation method of the tantalum-niobium alloy powder, the hydrogenated tantalum-niobium alloy powder is subjected to plasma treatment by adopting 45-60kW plasma power.
According to the preparation method of the tantalum-niobium alloy powder, the gas circulation cooling temperature of the hydrogenated tantalum-niobium alloy powder is lower than 45 ℃ in the step of plasma treatment.
In the plasma treatment process, not only the spheroidization of the powder is completed, but also the dehydrogenation step is realized. The invention skillfully combines the modes of hydrogenation treatment, crushing and plasma treatment, thereby not only solving the problem of preparing the spheroidized tantalum-niobium alloy, but also solving the problems of controllable cost and complex flow of a new preparation method.
According to the preparation method of the tantalum-niobium alloy powder, after the step S3, the tantalum-niobium alloy spherical powder with the diameter of 15-53 microns is obtained through screening.
The invention also provides the tantalum-niobium alloy powder prepared by the method, which has excellent performance and can be applied to additive manufacturing.
The invention also provides a part prepared from the tantalum-niobium alloy powder by an additive manufacturing processing mode.
Advantageous effects
Because the plasma spheroidizing process used in the scheme has higher temperature, the effect of dehydrogenating the hydrogenated powder of the tantalum-niobium alloy can be realized, and compared with the traditional refractory alloy powder preparation mode, the high-temperature dehydrogenation treatment process is reduced. After spheroidizing, the tantalum-niobium alloy spherical powder with the diameter of 15-53 microns is obtained, and a required additive manufacturing sample piece is prepared by a metal laser additive manufacturing device and an independently developed additive manufacturing process, so that the sample piece has high density and excellent mechanical property.
The invention ensures the nodularity of the powder to a greater extent by cooling the powder by combining the high-temperature plasma with the normal-temperature inert gas, reduces the nanometer micropowder generated by vaporization in the nodularization process of the powder, and improves the product quality.
Detailed Description
The present invention is described below based on examples, and it will be understood by those of ordinary skill in the art that, unless explicitly required by the context, the words "comprise", "comprising", and the like throughout the specification and claims are to be construed in an inclusive sense as opposed to an exclusive or exhaustive sense; that is, what is meant is "including, but not limited to".
Example 1
The invention will be further described below by taking the preparation of Ta60Nb40 alloy powder as an example.
The preparation process comprises the following steps:
1) preparing materials: smelting by using a master alloy, preparing mixed powder of tantalum 60% and niobium 40% according to the alloy proportion by using high-purity tantalum powder and niobium powder as raw materials, and melting the powder by using an arc melting furnace to prepare a Ta60Nb40 tantalum-niobium alloy ingot; and (5) standby.
2) Carrying out hydrogenation crushing and plasma spheroidizing to prepare powder: placing Ta60Nb40 alloy ingot into a hydrogenation reaction kettle, pumping the reaction kettle to below 1pa by a gas replacement mode, introducing argon, and repeating the steps for more than three times. And finally, pumping out argon, opening a hydrogen valve, heating the reaction kettle, introducing hydrogen, starting hydrogen absorption reaction at the temperature of 340 ℃ and the hydrogen pressure of about 1.0MPa, continuously introducing the hydrogen to fully react the inside, controlling the reaction time according to the cast ingot input quantity, and finishing the reaction when the gas pressure is not reduced any more after the hydrogen valve is closed. And (3) cooling, introducing argon to dilute hydrogen atmosphere, taking out the tantalum-niobium alloy ingot with hydrogen embrittlement, and crushing the powder to below 60 micrometers in a ball milling or jet milling mode. And (3) screening to obtain raw powder of 15-53 microns, adding into direct-current plasma spheroidizing equipment, carrying out plasma spheroidizing treatment on the raw powder by a spheroidizing process at the plasma power of 50kW, the powder feeding speed of 80g/min and the gas circulating cooling temperature of 40 ℃ to prepare the spherical tantalum-niobium alloy powder material.
3) Powder classification: and classifying the powder material according to the additive manufacturing powder requirement, wherein the upper limit and the lower limit are respectively 15 micrometers and 53 micrometers, and obtaining a Ta60Nb40 alloy powder finished product after the screening is finished.
The observation of a scanning electron microscope shows that the product has less nano-grade powder content.
Example 2
The invention will be further described below by taking the preparation of Ta60Nb40 alloy powder as an example.
The preparation process comprises the following steps:
1) preparing materials: smelting by using a master alloy, preparing mixed powder of tantalum 60% and niobium 40% according to the alloy proportion by using high-purity tantalum powder and niobium powder as raw materials, and melting the powder by using an arc melting furnace to prepare a Ta60Nb40 tantalum-niobium alloy ingot; and (5) standby.
2) Carrying out hydrogenation crushing and plasma spheroidizing to prepare powder: placing Ta60Nb40 alloy ingot into a hydrogenation reaction kettle, pumping the reaction kettle to below 1pa by a gas replacement mode, introducing argon, and repeating the steps for more than three times. And finally, pumping out argon, opening a hydrogen valve, heating the reaction kettle, introducing hydrogen, starting hydrogen absorption reaction at the temperature of 340 ℃ and the hydrogen pressure of about 1MPa, continuously introducing the hydrogen to fully react the inside, controlling the reaction time according to the input quantity of the cast ingots, and finishing the reaction when the pressure is not reduced any more after the hydrogen valve is closed. And (3) cooling, introducing argon to dilute hydrogen atmosphere, taking out the tantalum-niobium alloy ingot with hydrogen embrittlement, and crushing the powder to below 60 micrometers in a ball milling or jet milling mode. And (3) screening to obtain raw powder of 15-53 microns, adding into direct-current plasma spheroidizing equipment, carrying out plasma spheroidizing treatment on the raw powder by a spheroidizing process at the plasma power of 45kW, the powder feeding speed of 50g/min and the gas circulating cooling temperature of 30 ℃ to prepare the spherical tantalum-niobium alloy powder material.
3) Powder classification: and classifying the powder material according to the additive manufacturing powder requirement, wherein the upper limit and the lower limit are respectively 15 micrometers and 53 micrometers, and obtaining a Ta60Nb40 alloy powder finished product after the screening is finished.
The observation of a scanning electron microscope shows that the product has less nano-grade powder content.
Example 3
The invention will be further described below by taking the preparation of Ta65Nb35 alloy powder as an example.
The preparation process comprises the following steps:
1) preparing materials: smelting by using a master alloy, preparing mixed powder of 65% of tantalum and 35% of niobium by using high-purity tantalum powder and niobium powder as raw materials according to an alloy proportion, and melting the powder by using an arc melting furnace to prepare a Ta65Nb35 tantalum-niobium alloy ingot; and (5) standby.
2) Carrying out hydrogenation crushing and plasma spheroidizing to prepare powder: placing Ta65Nb35 alloy ingot into a hydrogenation reaction kettle, pumping the reaction kettle to below 1pa by a gas replacement mode, introducing argon, and repeating the steps for more than three times. And finally, pumping out argon, opening a hydrogen valve, heating the reaction kettle, introducing hydrogen, starting hydrogen absorption reaction at the hydrogen pressure of about 1.0MPa at 340 ℃, continuously introducing the hydrogen to fully react, controlling the reaction time according to the input quantity of the cast ingots, finishing the reaction when the pressure is not reduced after closing the hydrogen valve, cooling, introducing argon to dilute hydrogen atmosphere, taking out tantalum-niobium alloy ingots with hydrogen embrittlement, crushing the powder to be below 60 micrometers in a ball milling or jet milling mode, sieving to obtain raw powder of 15-53 micrometers, adding direct-current plasma spheroidizing equipment, carrying out plasma spheroidizing treatment with the plasma power of 65kW, the powder feeding rate of 100g/min and the gas circulation cooling temperature of 35 ℃ to obtain the spherical tantalum-niobium alloy powder material.
3) Powder classification: and classifying the powder material according to the additive manufacturing powder requirement, wherein the upper limit and the lower limit are respectively 15 micrometers and 53 micrometers, and obtaining a Ta65Nb35 alloy powder finished product after the screening is finished.
The observation of a scanning electron microscope shows that the product has less nano-grade powder content.
Comparative example 1
The invention will be further described below by taking the preparation of Ta90Nb10 alloy powder as an example.
The preparation process comprises the following steps:
1) preparing materials: smelting by using a master alloy, preparing mixed powder of 90% of tantalum and 10% of niobium by using high-purity tantalum powder and niobium powder as raw materials according to an alloy proportion, and melting the powder by using an arc melting furnace to prepare a Ta90Nb10 tantalum-niobium alloy ingot; and (5) standby.
2) Carrying out hydrogenation crushing and plasma spheroidizing to prepare powder: placing Ta90Nb10 alloy ingot into a hydrogenation reaction kettle, pumping the reaction kettle to below 1pa by a gas replacement mode, introducing argon, and repeating the steps for more than three times. And finally, pumping out argon, opening a hydrogen valve, heating the reaction kettle, introducing hydrogen, starting hydrogen absorption reaction at about 240 ℃ and hydrogen pressure of 0.80MPa, continuously introducing the hydrogen to fully react, controlling reaction time according to the input quantity of the cast ingots, after closing the hydrogen valve, finishing the reaction if the air pressure is not reduced, cooling, introducing argon to dilute hydrogen atmosphere, taking out tantalum-niobium alloy ingots with hydrogen embrittlement, crushing the powder to be below 60 micrometers in a ball milling or airflow milling mode, sieving to obtain raw powder of 15-53 micrometers, adding direct-current plasma spheroidizing equipment, carrying out plasma spheroidizing treatment with plasma power of 30kW, powder feeding rate of 110g/min and gas circulation cooling temperature of 55 ℃, and preparing the spherical tantalum-niobium alloy powder material.
3) Powder classification: and classifying the powder material according to the additive manufacturing powder requirement, wherein the upper limit and the lower limit are respectively 15 micrometers and 53 micrometers, and obtaining a Ta90Nb10 alloy powder finished product after the screening is finished.
The observation of a scanning electron microscope shows that the content of the nano-grade powder in the product is obviously increased.
Those skilled in the art will readily appreciate that the above-described preferred embodiments may be freely combined, superimposed, without conflict.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A tantalum-niobium alloy powder, characterized by: comprises 40-80% of Ta and 20-60% of Nb by mass, the grain diameter is 15-53 microns, and the sphericity is more than or equal to 90%.
2. The tantalum-niobium alloy powder of claim 1, wherein: the alloy comprises 55-65% of Ta and 45-35% of Nb by mass.
3. The preparation method of the tantalum-niobium alloy powder is characterized by comprising the following steps:
s1, selecting a tantalum-niobium alloy containing 40-80% of Ta and 20-60% of Nb by mass, and hydrogenating the tantalum-niobium alloy to obtain a hydrogenated tantalum-niobium alloy;
s2, crushing the hydrogenated tantalum-niobium alloy to prepare hydrogenated tantalum-niobium alloy powder;
and S3, carrying out plasma spheroidizing on the hydrogenated tantalum-niobium alloy powder to obtain the dehydrogenated tantalum-niobium alloy powder.
4. The method of producing tantalum-niobium alloy powder according to claim 3, wherein: in step S1, the hydrogenation treatment is carried out at a temperature higher than 300 ℃ and a pressure higher than 1.0 MPa.
5. The method of producing tantalum-niobium alloy powder according to claim 3, wherein: in step S2, the tantalum-niobium hydride alloy powder is first obtained by physical crushing, and then further crushed tantalum-niobium hydride alloy powder is prepared by flow milling.
6. The method of producing tantalum-niobium alloy powder according to claim 3, wherein: the granularity of the tantalum-niobium alloy powder obtained in the step S2 is 10-60 microns.
7. The method of producing tantalum-niobium alloy powder according to claim 3, wherein: the material conveying speed in the plasma spheroidizing step is selected to be 50-100 g/min.
8. The method of producing tantalum-niobium alloy powder according to claim 3, wherein: the plasma power of the plasma spheroidizing step is 45-60 kW.
9. The method of producing tantalum-niobium alloy powder according to claim 3, wherein: the gas circulation cooling temperature of the plasma spheroidizing step is lower than 45 ℃.
10. The method of producing tantalum-niobium alloy powder according to claim 3, wherein: after step S3, the method further includes the step of obtaining tantalum-niobium alloy spherical powder of 15-53 microns by sieving.
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