CN111618310A - Spherical vanadium alloy powder and preparation method and application thereof - Google Patents

Spherical vanadium alloy powder and preparation method and application thereof Download PDF

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CN111618310A
CN111618310A CN202010500957.8A CN202010500957A CN111618310A CN 111618310 A CN111618310 A CN 111618310A CN 202010500957 A CN202010500957 A CN 202010500957A CN 111618310 A CN111618310 A CN 111618310A
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vanadium alloy
alloy powder
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何安西
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Sichuan Junkesi Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/14Making metallic powder or suspensions thereof using physical processes using electric discharge
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06Metallic powder characterised by the shape of the particles
    • B22F1/065Spherical particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y70/00Materials specially adapted for additive manufacturing
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00Coating starting from inorganic powder
    • C23C24/08Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/10Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
    • C23C24/103Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

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Abstract

The invention provides spherical vanadium alloy powder and a preparation method and application thereof. The preparation method can comprise the following steps: placing the vanadium alloy rod in a vacuum environment; introducing inert gas into the vacuum environment to replace air, wherein the oxygen content in the vacuum environment after replacement is less than 5 ppm; melting the end face of the vanadium alloy rod to obtain a liquid film by using an electric arc; rotating the vanadium alloy rod, and breaking a liquid film into fine liquid drops under the action of centrifugal force; and cooling to obtain spherical vanadium alloy powder. The spherical vanadium alloy powder can comprise the powder prepared by the preparation method of the spherical vanadium alloy powder. The application may comprise an application in the field of laser or electron beam additive manufacturing, and/or an application in the field of laser or electron beam cladding, for example an application in electron beam 3D printing. The beneficial effects of the invention can include: the preparation efficiency is high, the cost is low, and the safety is high; the problem of poor sphericity of the powder in the traditional production method can be effectively solved.

Description

Spherical vanadium alloy powder and preparation method and application thereof
Technical Field
The invention relates to the field of preparation of vanadium alloy powder, in particular to spherical vanadium alloy powder and a preparation method and application thereof.
Background
Vanadium alloys are internationally recognized as ideal candidate materials for certain key structural components of fusion reactors, and the most remarkable advantages are low activation characteristics and excellent high-temperature strength performance under neutron irradiation conditions. In addition, the vanadium and vanadium alloy also have the advantages of good radiation induced expansion and damage resistance, good dimensional stability, good heat conduction performance, lower thermal expansion coefficient and elastic modulus, low biohazard safety and environmental protection characteristics, good creep resistance, good processability, good corrosion resistance to liquid lithium and the like. In particular vanadium alloys: the V-Cr-Ti system and the V-W-Ti system are more important candidate structural materials of the nuclear fusion reactor, so the alloy has wide application prospect in structural designs of a first wall, a cladding, a divertor and the like of the fusion reactor, aerospace and high temperature fields.
In the application of vanadium alloy, various structural components, such as a space curved shell and the like, are generally required to be manufactured. V is generated at high temperature due to vanadium alloy2O5The material is a highly toxic substance, so that a vacuum sheath forging method is generally adopted in the preparation process of the material, such as ingot cogging, extrusion and the like, and if the method is also adopted in the shell forming process, the risk of releasing toxic substances due to sheath rupture exists because the deformation amount is large, the process is complex, and the problems of large allowance, high cost and the like are caused.
At present, the main production method of vanadium alloy powder comprises the following steps: reduction method, fused salt electrolysis method, gas atomization method, mechanical alloying method, crushing method, inert gas atomization method and the like. The powder produced by the inert gas atomization method has more satellite powder on the particles, also has some hollow powder, and the size interval of the particle size distribution of the powder particles is wider, so that the powder particles in the size interval suitable for 3D printing are lower in occupied ratio.
The method is characterized in that high-purity vanadium powder, chromium powder and titanium powder are used as raw materials by China institute of engineering and physics, the average particle size of the three powders is about 35 microns, the vanadium alloy powder is prepared by a method of mixing the powders and grinding to realize mechanical alloying, acetone is used as a process control agent during wet grinding, the process control agent is not added during dry grinding, and a mechanical alloying method under the protection of inert atmosphere is adopted to efficiently prepare the fine vanadium alloy powder, but the prepared powder has poor sphericity and high oxygen content.
CN201811156064.5 discloses a method for preparing metal vanadium powder by metal gas-based reduction, which comprises the following steps: vanadium oxide is used as a raw material, active metal is used as a reducing agent, the active metal contacts the raw material in a gas form to generate a thermal reduction reaction, and a reaction product is subjected to acid washing, filtering and drying to obtain metal vanadium powder.
CN201811222443.X discloses a preparation method of high-purity vanadium powder, mixing vanadium-containing material with alkali metal or alkaline earth metal chloride salt, mixing with calcium hydride, and performing vacuum thermal reduction to obtain a reduction product; and washing with an ammonium chloride solution, an alkali liquor and an acid liquor in sequence, and finally carrying out dehydrogenation treatment to obtain the high-purity metal vanadium powder.
CN201410335895.4 discloses a preparation method of titanium-aluminum-vanadium alloy powder, which comprises the following steps: a. preparing an electrode: adding TiO into the mixture2、Al2O3、V2O5Mixing the powder, pressing and molding, and sintering at high temperature to obtain the titanium-aluminum-vanadium electrode; b. molten salt electrolysis reaction: and (3) carrying out molten salt electrolysis reaction by taking the prepared titanium-aluminum-vanadium electrode as a cathode, a graphite rod as an anode and NaCl-CaCl2 as molten salt electrolyte, wherein the powder obtained in the cathode frame is the titanium-aluminum-vanadium alloy powder.
CN109628731A discloses a method for preparing vanadium and alloy powder by processing vanadium-containing raw materials in a short process, firstly oxidizing and roasting the vanadium-containing raw materials and alkaline compounds to generate vanadate which is easy to dissolve in water, removing impurities and precipitating vanadium to form a high-purity intermediate product CaV2O6, dissolving the intermediate product CaV2O6 and other raw materials in a molten salt medium to form a uniform reaction system, then adding a reducing agent for reduction, and separating, washing and drying to obtain vanadium or vanadium alloy powder with the particle size of 50-800 nm and the purity of more than or equal to 99.0 wt.%.
The sphericity and cleanliness of the vanadium alloy powder prepared by the method are low.
Disclosure of Invention
In view of the deficiencies in the prior art, it is an object of the present invention to address one or more of the problems in the prior art as set forth above. For example, one of the objectives of the present invention is to produce vanadium alloy powders that meet the requirements of additive manufacturing techniques.
In order to achieve the above object, an aspect of the present invention provides a method for preparing spherical vanadium alloy powder.
The preparation method can comprise the following steps: placing the vanadium alloy rod in a vacuum environment; introducing inert gas into the vacuum environment to replace air, wherein the oxygen content in the vacuum environment after replacement is less than 5 ppm; melting the end face of the vanadium alloy rod to obtain a liquid film by using an electric arc; rotating the vanadium alloy rod, and breaking a liquid film into fine liquid drops under the action of centrifugal force; and cooling to obtain spherical vanadium alloy powder.
According to one or more exemplary embodiments of the present invention, the mass fraction of vanadium in the vanadium alloy rod may be 89 to 92%.
According to one or more exemplary embodiments of the present invention, in the initial stage of melting the end face of the vanadium alloy rod out of the liquid film by using the arc, the vacuum degree of the vacuum environment is controlled to be 7 × 10-3Pa or less.
According to one or more exemplary embodiments of the present invention, the vanadium alloy rod may be rotated at a rotation speed of 2000 to 26000 rpm.
According to one or more exemplary embodiments of the present invention, the arc may be output by an arc melting system, and an operating current output of the arc melting system may be 1500-4000A.
According to one or more exemplary embodiments of the present invention, the inert gas may include a mixed gas composed of argon and helium, and the volume ratio of helium in the mixed gas is 10 to 90%; alternatively, the inert gas may comprise argon.
According to one or more exemplary embodiments of the present invention, the step of placing the vanadium alloy rod in a vacuum environment may include: putting the vanadium alloy rod into an arc melting rotary atomization device, extracting vacuum and controlling the vacuum degree in the deviceAt 7 × 10-3Pa or less.
According to one or more exemplary embodiments of the present invention, the method may further include the steps of: and screening the cooled vanadium alloy powder by using an ultrasonic vibration screen or a standard screen under a protective atmosphere, and grading according to the granularity to obtain vanadium alloy powder of different grades.
In another aspect, the invention provides spherical vanadium alloy powder. The spherical vanadium alloy powder can comprise the powder prepared by the preparation method of the spherical vanadium alloy powder.
In yet another aspect, the present invention provides an application of spherical vanadium alloy powder, which may include: application in the field of laser or electron beam additive manufacturing, application in the field of laser or electron beam cladding, for example application in electron beam 3D printing.
Compared with the prior art, the beneficial effects of the invention can include: the preparation efficiency is high, the cost is low, and the safety is high; the problem of poor sphericity of the powder in the traditional production method can be effectively solved; the produced vanadium alloy powder is basically free of hollow powder and satellite powder, and has the advantages of narrow particle size distribution range, high sphericity, good fluidity, few impurities and the like.
Drawings
The above and other objects and features of the present invention will become more apparent from the following description taken in conjunction with the accompanying drawings, in which:
FIG. 1 shows a morphology of vanadium alloy powder prepared in example 1;
FIG. 2 shows a morphology of vanadium alloy powder prepared in example 2;
fig. 3 shows a schematic diagram of the particle size distribution of the vanadium alloy powder prepared in example 2.
Detailed Description
Hereinafter, spherical vanadium alloy powder (may also be referred to as vanadium alloy powder) of the present invention, and a preparation method and application thereof will be described in detail with reference to the accompanying drawings and exemplary embodiments.
The selective laser melting forming additive manufacturing technology provides a brand new thought and method for integration of vanadium alloy material preparation and part accurate forming, and is expected to greatly improve the material utilization rate and greatly reduce the overall manufacturing cost on the premise of ensuring the quality and performance of parts. However, the metal powder for the additive manufacturing technology needs to have accurate chemical composition and low oxygen content, and must also meet the physical properties required by the additive manufacturing technology for the metal powder: fine powder grain diameter, narrow grain diameter distribution interval, high powder grain sphericity, good fluidity, large apparent density, high tap density, few impurities and other special requirements.
Therefore, the inventor provides spherical vanadium alloy powder suitable for the field of additive manufacturing and a preparation method thereof.
The invention provides a preparation method of spherical vanadium alloy powder.
In an exemplary embodiment of the present invention, the method for preparing the spherical vanadium alloy powder may include the steps of:
processing the vanadium alloy rod subjected to vacuum melting or a vanadium alloy bar (also called vanadium alloy bar) prepared by a powder metallurgy method into a raw material rod (also called vanadium alloy rod, vanadium alloy raw material rod and the like).
The raw material rod is put into an arc melting centrifugal atomization device (also called an arc melting rotary atomization device), vacuum is pumped, and then inert gas or mixed inert gas is introduced into the device.
Starting an equipment arc under the protection of inert gas to melt the front end of the vanadium alloy raw material rod into a liquid film, controlling the rotating speed of the rotating vanadium alloy raw material rod, crushing the liquid film melted at the front end of the raw material rod into fine liquid drops under the action of centrifugal force, controlling the cooling speed of the fine liquid drops crushed by the vanadium alloy liquid by adjusting the proportion and the flow rate of mixed inert gas, realizing the sphericization of the vanadium alloy powder under the action of surface tension, and obtaining the spherical vanadium alloy powder capable of meeting the technical requirements of additive manufacturing.
In another exemplary embodiment of the present invention, the method for preparing the spherical vanadium alloy powder may include the steps of:
putting a vanadium alloy raw material rod into an electric arc melting and rotary atomizing deviceIn the device, vacuum was drawn and the degree of vacuum in the device was controlled to 7 × 10-3Pa or less, and further, may be 3 × 10-3Pa~6×10-3Pa. Too high vacuum degree in the pumping device prolongs the production preparation time of equipment and reduces the working efficiency, and too low vacuum degree in the pumping device needs to be filled with more inert gas to replace and remove oxygen, which is not economical.
Then introducing inert gas into the device to ensure that the oxygen content in the centrifugal atomizing chamber of the device is less than or equal to 5ppm, and starting the arc melting centrifugal atomizing device under the protection of the inert gas. The inert gas can be argon or a mixed gas composed of argon and helium. Wherein, the purity of argon can be above 99.995%, and the purity of helium can be above 99.995%. Further, the purity of argon and helium may be 99.999%.
Controlling the rotation speed of the vanadium alloy raw material rod to be 2000-26000 rpm, such as 5000rpm, 12000rpm, 18000rpm and the like, melting the vanadium alloy rod through an arc melting system to generate a liquid film, crushing the liquid film into fine droplets under the action of centrifugal force, controlling the cooling speed of the fine droplets of the vanadium alloy through adjusting the proportion of mixed inert gas, and cooling and solidifying under the action of surface tension to realize the spheroidization of the vanadium alloy powder. And simultaneously continuously feeding a vanadium alloy bar, supplementing a melted and separated liquid film, wherein the feeding speed of the raw material bar is 6-240 mm/min and continuously adjustable, so as to obtain the continuous production of the spherical vanadium alloy powder, wherein the feeding speed can be 60mm/min, 70mm/min, 100mm/min, 120mm/min, 170mm/min, 210mm/min, 230mm/min and the like.
In this embodiment, the arc melting rotary atomizing device mainly includes:
(1) an arc melting system: the arc melting system may melt the feedstock bar into a liquid film.
(2) Rotating centrifugal atomization system (rotating system for short): the rotary centrifugal atomizing system can be provided with a centrifugal atomizing chamber, the raw material rod is placed into the rotary centrifugal atomizing chamber, the rotary system can control the rotating speed of the raw material rod, the rotary system can enable the raw material rod to generate centrifugal force, and a liquid film melted at the front end of the raw material rod is atomized into liquid drops to be cooled into powder under the action of the centrifugal force.
(3) A feeding system: the feed system may be connected to one end of the feedstock bar. The feeding system can supplement the liquid film which is melted and separated by continuously feeding the bar stock (namely the raw material bar), and the feeding speed can be continuously adjusted at 60-240 mm/min.
In this embodiment, the working current output of the arc melting system in the arc melting rotary atomizer can be 1500-4000A, such as 2000 + -800A, the arc length can be 35-80 mm, such as 55 + -10 mm, and the arc column diameter can be 40-55 mm, such as 47 + -3 mm.
In this embodiment, the vanadium alloy rod may comprise a vanadium alloy rod produced by vacuum melting or powder metallurgy.
In this embodiment, at the beginning of the preparation, the raw material rod can be completely put into the vacuum chamber of the device, the raw material rod is fed while rotating, and when the distance reaches the requirement of 35-80 mm of arc length, the arc is turned on. Wherein, one end of the raw material rod can be connected with the feeding system, and the other end can be connected with the plasma gun through the electric arc.
In this embodiment, the vanadium alloy rod may include the following components in mass percent:
89-92% of vanadium, e.g. 90%, 91%, etc
7.7-10.7% of one or more of titanium, chromium and tungsten elements, and less than or equal to 0.3% of other elements.
The relative density of the vanadium alloy rods may be above 98%, e.g., 98.5%, 99%, etc.
The diameter of the vanadium alloy rod can be 50-90 mm, and the length can be 250-550 mm.
In this embodiment, before the vanadium alloy rod is placed in the arc melting rotary atomizing device, the method may further include the steps of: and processing the vanadium alloy rod into a proper size according to the requirement of a rotary atomizing device.
In this embodiment, the total flow rate of the inert gas entering the arc melting rotary atomizer with the argon or the mixed gas may be 300 to 900L/min, such as 600 + -200L/min, and the pressure thereof may be 0.3 to 0.8MPa, such as 0.6 + -0.1 MPa.
The volume ratio of the helium in the mixed gas can be 10-90%, for example 50 +/-20%, and the ratio of the helium can be changed according to the requirement of the particle size of the vanadium alloy powder product.
In the embodiment, when the oxygen content in the atomizing cavity is less than or equal to 5ppm, the working current output of the arc melting system is 1500-4000A, the arc length is 35-80 mm, and the diameter of the arc column is 40-55 mm.
In the process of metal powder, the viscosity of the metal liquid is different due to different metal properties and different melting points, and the thickness of a liquid film layer on the melting end face of the raw material rod is determined by the energy density of the melting arc, so that the particle size of the powder and the smooth proceeding of the atomization process are influenced. The energy density of the electric arc is too low, so that the time for finishing the melting of the raw material rod is prolonged, a large amount of heat is transferred to a motor shaft and a bearing, and the motor cannot work normally. The energy density of the electric arc is too high, and the liquid film layer on the melting end surface of the raw material rod is too thick, so that the powder is thickened, the flash is easy to generate, the vibration of the raw material rod is increased, and the atomization process cannot be carried out. The operating current determines the magnitude of the arc energy density. The rotation speed of the raw material rod, the magnitude of the working current, the length of the arc distance and the feeding speed of the raw material rod are important process parameters of the invention, and the atomization process can be smoothly realized only through the combination and cooperation of the process parameters.
By adopting the preparation method of the vanadium alloy powder, the spherical vanadium alloy powder which can meet the technical requirements of additive manufacturing can be prepared in batch. The chemical composition of the prepared vanadium alloy powder is basically equivalent to that of the raw material rod.
The vanadium alloy powder has a particle size of 2000 μm or less, for example, 15 μm, 20 μm, 50 μm, 100 μm, 500 μm, 1100 μm, 1900 μm, or the like. The sphericity of the powder particle morphology to the standard circle may be above 90%, further above 92%, for example 93%.
Oxygen increment in the powder preparation production process: 100ppm or less, nitrogen increment: less than or equal to 30 ppm.
In order that the above-described exemplary embodiments of the invention may be better understood, further description thereof with reference to specific examples is provided below.
Example 1
The V-6W-2.5Ti vanadium alloy bar is used as a raw material, the main chemical element content of the vanadium alloy bar is shown in Table 1, the relative density of the vanadium alloy bar is more than 98%, the vanadium alloy bar is processed into a vanadium alloy raw material bar with the diameter of phi 50 multiplied by 550mm, and surface oxides and impurities are removed.
Putting the vanadium alloy raw material rod with the surface oxides and impurities removed into an arc centrifugal atomization device (namely an arc melting rotary atomization device), and vacuumizing to 6 × 10-3Pa, then introducing mixed inert gas into the device to ensure that the oxygen content in the atomizing chamber is less than or equal to 5 ppm.
Starting an arc melting centrifugal atomization device under the protection of inert gas, controlling power by controlling the working current of arc melting, and further controlling the melting speed of the vanadium alloy rod, wherein the working current is output by 2400A, the arc length is 60mm, and the rotating speed of the raw material vanadium rod is 2600 rpm; the front end of a vanadium alloy raw material rod is melted into a liquid film by electric arc, the liquid film is crushed into fine vanadium alloy liquid drops through rotary centrifugation, the fine vanadium alloy liquid drops are cooled and solidified in a mixed inert gas environment, and the feeding speed of the vanadium alloy raw material rod is 180 mm/min.
And taking out the prepared vanadium alloy powder after cooling to room temperature, sieving by using an ultrasonic vibration sieve under the protection of argon, grading according to the granularity to obtain spherical vanadium alloy powder of different grades, and performing vacuum packaging by using a plastic film to obtain the product.
Wherein, the volume of argon with the purity of 99.995 percent accounts for 10 percent, and the volume of helium with the purity of 99.995 percent accounts for 90 percent in the mixed inert gas. The flow rate of the mixed inert gas is 890L/min, and the pressure is 0.6 +/-0.05 MPa.
The prepared spherical vanadium alloy powder product has a spherical or sphere-like particle shape as shown in figure 1, the main chemical element content of the vanadium alloy powder product is shown in table 2, the particle size of the vanadium alloy powder is 1200-1500 microns, the oxygen content of the powder particles is 471ppm, the oxygen increment in the preparation process is 59ppm, the nitrogen content is 113ppm, the nitrogen increment is 18ppm, and the sphericity is 92%.
TABLE 1 main chemical composition (mass fraction, wt%) of V-6W-2.5 Ti-based vanadium alloy rods
Element(s) W Ti O N Impurity element V
Content (wt.) 5.98 2.47 0.0412 0.0095 ≤0.25 Balance of
TABLE 2 EXAMPLE 1 main chemical composition (mass fraction, wt%) of the vanadium alloy powder obtained
Element(s) W Ti O N Impurity element V
Content (wt.) 5.98 2.47 0.0471 0.0113 ≤0.25 Balance of
Example 2
V-5Cr-5Ti series vanadium alloy bars are used as raw materials, the contents of main chemical elements are shown in Table 3, and the relative density is more than 99%. The rod material is processed into vanadium alloy raw material rod with the diameter of phi 80 multiplied by 350mm, and surface oxides and impurities are removed.
Putting the vanadium alloy raw material rod with the surface oxides and impurities removed into an arc centrifugal atomization device, and pumping the vacuum degree to 6 × 10-3Pa, then introducing mixed inert gas into the device to ensure that the oxygen content in the atomizing chamber is 3 ppm.
Starting an arc melting centrifugal atomization device under the protection of inert gas, controlling the melting speed of the vanadium alloy rod by controlling the working current of arc melting, wherein the working current outputs 2800A, the arc length is 45mm, and the rotating speed of the raw material vanadium alloy rod is 23000 rpm; the front end of the vanadium alloy raw material rod is melted into a liquid film by electric arc, the liquid film is crushed into fine vanadium alloy liquid drops through rotary centrifugation, the fine vanadium alloy liquid drops are cooled and solidified in a mixed inert gas environment, and the feeding speed of the vanadium alloy raw material rod is 96 mm/min.
And taking out the prepared vanadium alloy powder after cooling to room temperature, sieving by using an ultrasonic vibration sieve under the protection of argon, grading according to granularity to obtain spherical vanadium alloy powder of different grades, and performing vacuum packaging by using a plastic film to obtain the product.
Wherein, the volume percentage of argon with the purity of 99.995 percent in the mixed inert gas is 90 percent, and the volume percentage of helium with the purity of 99.995 percent is 10 percent; the flow rate of the mixed inert gas was 690L/min, and the pressure thereof was 0.4 MPa.
The particle shape of the prepared spherical vanadium alloy powder product is spherical or sphere-like as shown in figure 2, and the sphericity reaches 90 percent. The main chemical element content of the vanadium alloy powder product is shown in table 4; the oxygen content of the powder particles was 583ppm, the oxygen gain during the preparation was 62ppm, the nitrogen content was 132ppm and the nitrogen gain was 21 ppm. The particle size distribution of the spherical vanadium alloy powder is shown in figure 3, the particle size distribution of the obtained vanadium alloy powder particles is mainly in the range of 53-150 micrometers, and the powder flowability is 23s/50 g.
TABLE 3 main chemical composition (mass fraction, wt%) of V-5Cr-5Ti based vanadium alloy rods
Element(s) Cr Ti O N Impurity element V
Content (wt.) 4.79 4.91 0.0521 0.0105 ≤0.25 Balance of
TABLE 4 EXAMPLE 2 main chemical composition (mass fraction, wt%) of the obtained vanadium alloy powder
Element(s) Cr Ti O N Impurity element V
Content (wt.) 4.79 4.91 0.0583 0.0126 ≤0.25 Balance of
The invention also provides spherical vanadium alloy powder. The spherical vanadium alloy powder can comprise the vanadium alloy powder prepared by the preparation method.
The vanadium alloy powder has high sphericity, narrow size interval distribution, accurate and uniform chemical composition and low oxygen content. In addition, the physical properties of the vanadium alloy powder also include: fine powder grain size, narrow grain diameter distribution interval, high powder grain sphericity, good fluidity, large apparent density, high tap density, less impurities, etc. The particle size of the vanadium alloy powder can be 15-2000 μm.
In another aspect, the invention provides an application of the spherical vanadium alloy powder. Applications may include applications in the field of laser or electron beam 3D printing, for example in the field of high speed laser cladding deposition, in the field of selective electron beam melting, etc.
In summary, the advantages of the spherical vanadium alloy powder, the preparation method and the application thereof of the invention can include:
(1) the preparation method has high production efficiency and low cost.
(2) The invention combines an electric arc melting system and a rotary centrifugal atomization system, and the produced vanadium alloy powder has the following characteristics: fine powder grain diameter, narrow grain diameter distribution interval, high powder grain sphericity, good fluidity, large apparent density, high tap density and less impurities.
(3) Under the condition that vanadium is toxic, the device has a good sealing effect, and the risk of leakage of vanadium pollutants is reduced by adopting a vacuum and inert gas protection mode.
(4) The spherical vanadium alloy powder prepared by the invention can be used for developing a large number of complex vanadium alloy powder parts through an additive manufacturing technology so as to meet the requirements of aerospace and national defense war industry.
Although the present invention has been described above by referring to the exemplary embodiments and the accompanying drawings, it will be apparent to those skilled in the art that various modifications and changes can be made to the exemplary embodiments of the present invention without departing from the spirit and scope defined by the claims.

Claims (10)

1. The preparation method of the spherical vanadium alloy powder is characterized by comprising the following steps of:
placing the vanadium alloy rod in a vacuum environment; introducing inert gas into the vacuum environment to replace air, wherein the oxygen content in the vacuum environment after replacement is less than 5 ppm;
melting the end face of the vanadium alloy rod to obtain a liquid film by using an electric arc;
rotating the vanadium alloy rod, and breaking a liquid film into fine liquid drops under the action of centrifugal force;
and cooling to obtain spherical vanadium alloy powder.
2. The method for preparing the spherical vanadium alloy powder according to claim 1, wherein the mass fraction of vanadium in the vanadium alloy rod is 89-92%.
3. The method for preparing spherical vanadium alloy powder according to claim 1, wherein the vacuum degree of the vacuum environment is controlled to be 7 × 10 in the initial stage of the process of melting the end face of the vanadium alloy rod out of the liquid film by using the electric arc-3Pa or less.
4. The method for preparing the spherical vanadium alloy powder according to claim 1, wherein the vanadium alloy rod rotates at a speed of 2000-26000 rpm.
5. The method for preparing the spherical vanadium alloy powder according to claim 1, wherein the electric arc is output by an arc melting system, and the working current output of the arc melting system is 1500-4000A.
6. The method for preparing the spherical vanadium alloy powder according to claim 1, wherein the inert gas comprises a mixed gas composed of argon and helium, and the volume ratio of helium in the mixed gas is 10-90%;
alternatively, the inert gas comprises argon.
7. The method for preparing spherical vanadium alloy powder according to claim 1, wherein the step of placing the vanadium alloy rod in a vacuum environment comprises:
putting the vanadium alloy rod into an electric arc melting rotary atomization deviceDrawing vacuum and controlling the vacuum degree in the device to be 7 × 10-3Pa or less.
8. The method for preparing spherical vanadium alloy powder according to claim 1, further comprising the steps of:
and screening the cooled vanadium alloy powder by using an ultrasonic vibration screen or a standard screen under a protective atmosphere, and grading according to the granularity to obtain vanadium alloy powder of different grades.
9. Spherical vanadium alloy powder, characterized in that it comprises spherical vanadium alloy powder prepared by the method of any one of claims 1 to 8.
10. The use of the spherical vanadium alloy powder of claim 9, comprising: the method is applied to the field of laser or electron beam additive manufacturing and the field of laser or electron beam cladding.
CN202010500957.8A 2020-06-04 2020-06-04 Spherical vanadium alloy powder and preparation method and application thereof Pending CN111618310A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113492213A (en) * 2021-09-07 2021-10-12 西安欧中材料科技有限公司 Preparation method and equipment of high-sphericity low-oxygen-content TiAl alloy powder
CN113770349A (en) * 2021-09-14 2021-12-10 有研工程技术研究院有限公司 High-purity spherical metal vanadium powder and preparation method and application thereof

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020051728A1 (en) * 2000-03-14 2002-05-02 Koji Sato Solder ball and method for producing same
CN102336038A (en) * 2010-07-26 2012-02-01 核工业西南物理研究院 Composite structural material and process for manufacturing pipeline component using same
CN204545419U (en) * 2015-03-10 2015-08-12 沈阳好智多新材料制备技术有限公司 A kind of high vacuum induction is without crucible and have crucible inert gas atomizer powder manufacturing apparatus
CN105689730A (en) * 2016-02-24 2016-06-22 西安欧中材料科技有限公司 Method for preparing Inconel 625 alloy spherical powder
CN106670482A (en) * 2016-12-19 2017-05-17 西安欧中材料科技有限公司 Preparing method for superfine high-grade spherical GH4133 alloy powder
CN106853535A (en) * 2016-12-19 2017-06-16 西安欧中材料科技有限公司 A kind of preparation method of high-quality γ TiAl spherical powders
CN108380895A (en) * 2018-04-23 2018-08-10 安徽哈特三维科技有限公司 A kind of preparation method and application of Ti-Al-V-Fe-O alloy powders
CN108588582A (en) * 2018-06-29 2018-09-28 钢铁研究总院 3D printing high strength stainless steel powder and preparation process under low temperature Service Environment
CN110405220A (en) * 2019-07-10 2019-11-05 陕西斯瑞新材料股份有限公司 A method of GRCop-84 spherical powder is prepared based on plasma rotating atomization

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020051728A1 (en) * 2000-03-14 2002-05-02 Koji Sato Solder ball and method for producing same
CN102336038A (en) * 2010-07-26 2012-02-01 核工业西南物理研究院 Composite structural material and process for manufacturing pipeline component using same
CN204545419U (en) * 2015-03-10 2015-08-12 沈阳好智多新材料制备技术有限公司 A kind of high vacuum induction is without crucible and have crucible inert gas atomizer powder manufacturing apparatus
CN105689730A (en) * 2016-02-24 2016-06-22 西安欧中材料科技有限公司 Method for preparing Inconel 625 alloy spherical powder
CN106670482A (en) * 2016-12-19 2017-05-17 西安欧中材料科技有限公司 Preparing method for superfine high-grade spherical GH4133 alloy powder
CN106853535A (en) * 2016-12-19 2017-06-16 西安欧中材料科技有限公司 A kind of preparation method of high-quality γ TiAl spherical powders
CN108380895A (en) * 2018-04-23 2018-08-10 安徽哈特三维科技有限公司 A kind of preparation method and application of Ti-Al-V-Fe-O alloy powders
CN108588582A (en) * 2018-06-29 2018-09-28 钢铁研究总院 3D printing high strength stainless steel powder and preparation process under low temperature Service Environment
CN110405220A (en) * 2019-07-10 2019-11-05 陕西斯瑞新材料股份有限公司 A method of GRCop-84 spherical powder is prepared based on plasma rotating atomization

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
沃尔夫冈.霍费尔纳: "《核电厂材料》", 30 January 2017, 上海科学技术出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113492213A (en) * 2021-09-07 2021-10-12 西安欧中材料科技有限公司 Preparation method and equipment of high-sphericity low-oxygen-content TiAl alloy powder
CN113492213B (en) * 2021-09-07 2021-12-07 西安欧中材料科技有限公司 Preparation method and equipment of high-sphericity low-oxygen-content TiAl alloy powder
CN113770349A (en) * 2021-09-14 2021-12-10 有研工程技术研究院有限公司 High-purity spherical metal vanadium powder and preparation method and application thereof

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