CN111644631A - Preparation method of spherical vanadium powder - Google Patents
Preparation method of spherical vanadium powder Download PDFInfo
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- CN111644631A CN111644631A CN202010521104.2A CN202010521104A CN111644631A CN 111644631 A CN111644631 A CN 111644631A CN 202010521104 A CN202010521104 A CN 202010521104A CN 111644631 A CN111644631 A CN 111644631A
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- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 52
- 238000005242 forging Methods 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000010894 electron beam technology Methods 0.000 claims abstract description 14
- 238000003825 pressing Methods 0.000 claims abstract description 14
- 238000000889 atomisation Methods 0.000 claims abstract description 12
- 238000003723 Smelting Methods 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims description 17
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 16
- 239000002245 particle Substances 0.000 abstract description 11
- 239000011148 porous material Substances 0.000 abstract description 6
- 238000000465 moulding Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 15
- 239000002184 metal Substances 0.000 description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000011068 loading method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/10—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying using centrifugal force
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention relates to a preparation method of spherical vanadium powder, which comprises the steps of pressing and molding high-purity vanadium powder, sintering the high-purity vanadium powder into blank bars in vacuum, smelting the blank bars into vanadium rods by using electron beams, forging the vanadium rods, and preparing the spherical vanadium powder with the particle size of 10-150 micrometers by using a plasma rotary electrode atomization method. The spherical vanadium powder prepared by the method has the advantages of high sphericity, good fluidity, high tap density, good powder compactness, few pores and low content of hollow spheres, and the single-stage powder collecting system is adopted to reduce the loss of fine powder and improve the yield of the spherical vanadium powder.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a preparation method of spherical vanadium powder.
Background
Vanadium, a so-called metal vitamin, is a rare metal with important strategic importance in the world due to its excellent physicochemical properties. The prepared vanadium metal material has the advantages of low neutron irradiation activity, high heat transfer rate, low thermal expansion coefficient, excellent high-temperature strength, good ductility, corrosion resistance and the like, so that the spherical vanadium powder has wide application in the fields of 3D printing, nuclear power, aerospace and plasma spraying.
At present, few companies for producing spherical vanadium powder are available in China, and the preparation method of the spherical vanadium powder adopts an induction smelting method, then a vanadium rod is crushed, and then the vanadium powder is subjected to a plasma torch spheroidizing method. In the method, the vanadium powder particles pass through the high-temperature plasma torch region for only tens of milliseconds, a small amount of molten metal on the surface layer of the particles is coated on the particles under the action of surface tension to form spherical particles, and the spherical vanadium powder is obtained after cooling. The spherical vanadium powder produced by the method has more defects of hollow and pore in the spherical vanadium powder particles due to pores and air holes, the powder compactness is seriously influenced, meanwhile, plasma torch spheroidizing equipment is expensive, a powder collecting system is usually provided with multiple stages, and the spherical powder is low in yield due to the fact that the small particle powder is strong in adsorbability and cannot be effectively recovered due to the fact that the powder is attached to the inner wall of a pipeline.
Disclosure of Invention
The spherical vanadium powder prepared by the method has the advantages of high sphericity, good fluidity, high tap density, good powder compactness, few pores and low hollow sphere content, and the single-stage powder collecting system is adopted to reduce the loss of fine powder and improve the yield of the spherical vanadium powder.
The method comprises the steps of performing compression molding on high-purity vanadium powder, sintering the high-purity vanadium powder into a billet in vacuum, smelting the billet into a vanadium rod by using an electron beam, forging the billet, preparing spherical vanadium powder with the particle size of 10-150 microns by using a plasma rotary electrode atomization method, continuously melting the end face of a vanadium metal rod rotating at a high speed by using a plasma arc as a heat source, and rapidly solidifying the molten vanadium metal liquid drops under the action of centrifugal force to form the spherical vanadium powder.
The preparation method of the spherical vanadium powder comprises the following steps: vanadium powder press forming → vacuum sintering → electron beam melting → forging → vacuum annealing → plasma rotary electrode atomization, the specific technical scheme is as follows:
1) press forming
Pressing into a mold by using a cold isostatic press, filling vanadium powder into a strip-shaped rubber mold sleeve, sealing, putting into the cold isostatic press, and taking out after demolding to obtain a pressed vanadium strip;
2) vacuum sintering
Sintering the vanadium strip in the step 1) in a vacuum furnace, and cooling along with the furnace.
3) Electron beam melting
Adopting a 250kw electron beam melting furnace, putting the sintered vanadium rod into the furnace through an inlet valve, and vacuumizing to 10 DEG-4~10- 5pa, slowly feeding the vanadium strips into a bombardment area of an electron gun, and dripping molten vanadium metal into the water-cooled copper crucible. And dropping the vanadium liquid into a crucible to slowly and spirally pull down the bottom pad to form a vanadium ingot with phi of 60-70 mm, and peeling the vanadium ingot after smelting.
4) Forging
Heating the vanadium ingot in the step 3) to 900-1100 ℃, preserving heat for 10-25 min, forging, wherein the initial forging temperature is 1000-1100 ℃, and the final forging temperature is 850-950 ℃ to obtain a vanadium rod;
5) vacuum annealing
Step 4) the vanadium rod is in a vacuum degree of 10-4~10-5Annealing under pa, wherein the annealing temperature is 900-1000 ℃, the heat preservation time is 30-45 min, and furnace cooling is carried out;
6) plasma rotary electrode atomization
The vanadium rod annealed in the step 5) is vacuumized 10-4~10-5Under pa, under the protective atmosphere of 99.99% helium, a vanadium rod is placed in a rotary feeding device, a rotary button and a plasma gun power supply are started, and spherical vanadium powder with the particle size of 10-150 microns is formed through atomization of a plasma rotary electrode.
The pressing pressure in the step 1) is 200-280 MPa, and the pressure maintaining time is 60-120 s.
Step 2) vacuum degree of vacuum sintering 10-5pa。
The sintering system in the step 2) is 400-600 ℃, and the temperature is kept for 30-60 min; preserving heat for 60-90 min at 1000-1200 ℃; and (3) preserving the heat at 1300-1500 ℃ for 120-150 min, wherein the temperature rise speed is 10 ℃/min.
And 6) the protective gas is helium.
Step 7) the plasma rotating electrode atomization method comprises the following steps: the rotating speed of the electrode bar is 16000-19000 r/min, the current intensity is 1500-1800A, and the feeding rate is 0.6-1.0 mm/s.
Advantageous effects of the invention
(1) The method for preparing the vanadium rod by using electron beam melting can improve the purity, reduce the content of trace element impurities in the vanadium and improve the processability of the vanadium rod.
(2) The invention adopts the rotary swaging process, so that the vanadium rod has more uniform and compact structure, and the residual processing stress in the vanadium rod is eliminated by vacuum annealing.
(3) The spherical vanadium powder prepared by adopting the plasma rotary electrode for atomization has the advantages of high sphericity, good fluidity, high tap density, good powder compactness, few pores and low content of hollow spheres, and the single-stage powder collecting system is adopted to reduce the loss of fine powder and improve the yield of the spherical vanadium powder.
The purity of the raw material vanadium powder in the preparation method is more than or equal to 99.99 percent.
The Fisher-type particle size of the spherical vanadium powder obtained by the method is 10-50 microns, the particle size is normally distributed, and the powder particles are irregular.
Drawings
Fig. 1 and 2 show the morphology of spherical vanadium powder.
Detailed Description
Example 1:
(1) and (3) pressing and forming vanadium powder: pressing into a mold by using a cold isostatic press, filling vanadium powder into a long strip-shaped rubber mold sleeve, sealing, putting into the cold isostatic press, pressing at 220MPa for 80s, and taking out after demolding.
(2) Vacuum sintering, namely putting the pressed and formed vanadium strip into a vacuum intermediate frequency sintering furnace for sintering, wherein the vacuum degree is 1.0 × 10-5pa, the sintering system is that the temperature is kept at 450 ℃ for 60min, the temperature is kept at 1000 ℃ for 90min, the temperature is kept at 1500 ℃ for 120min, the temperature rising speed is 10 ℃/min, and the sintering is cooled along with the furnace.
(3) Electron beam melting, namely adopting a 250kw electron beam melting furnace, putting the sintered vanadium strip into the furnace through an inlet valve, and vacuumizing to 1.0 × 10-5pa, slowly feeding the vanadium strips into a bombardment area of an electron gun, and dripping molten vanadium metal into the water-cooled copper crucible. And dropping the vanadium liquid into a crucible to slowly and spirally pull down the bottom pad to form a vanadium ingot with the diameter of 60mm, and peeling the vanadium ingot after smelting.
(4) Forging: the forging equipment is a 200 kg air hammer, the heating temperature is 1100 ℃, the heat preservation time is 15min, the initial forging temperature is 1100 ℃, the final forging temperature is 950 ℃, the vanadium ingot is processed to a vanadium metal rod with the diameter of 50mm, and peeling is carried out after forging.
(5) Vacuum annealing, namely annealing the vanadium metal rod with the vacuum degree of 1.0 × 10-5pa, annealing temperature 950 ℃, heat preservation time 45min, and furnace cooling.
(6) Plasma rotary electrode atomization, namely loading a vanadium rod into a rotary feeding device, and vacuumizing to 1.0 × 10-5After pa, helium with the purity of 99.99 percent is filled, a rotating button and a plasma gun power supply are started, the rotating speed of an electrode bar is 19000r/min, the current intensity is 1500A, the feeding rate is 0.8mm/s, and the formed granularity is 20-120 micronsSpherical vanadium powder of rice.
Example 2:
(1) and (3) pressing and forming vanadium powder: pressing into a mold by using a cold isostatic press, filling vanadium powder into a long strip-shaped rubber mold sleeve, sealing, putting into the cold isostatic press, pressing at 240Mpa for 90s, and taking out after demolding.
(2) Vacuum sintering, namely putting the pressed and formed vanadium strip into a vacuum intermediate frequency sintering furnace for sintering, wherein the vacuum degree is 1.3 × 10-5pa, the sintering system is that the temperature is kept at 500 ℃ for 40min, the temperature is kept at 1100 ℃ for 60min, the temperature is kept at 1400 ℃ for 150min, the temperature rising speed is 10 ℃/min, and the sintering is cooled along with the furnace.
(3) Electron beam melting, namely adopting a 250kw electron beam melting furnace, putting the sintered vanadium strip into the furnace through an inlet valve, and vacuumizing to 1.3 × 10-5pa, slowly feeding the vanadium strips into a bombardment area of an electron gun, and dripping molten vanadium metal into the water-cooled copper crucible. And dropping the vanadium liquid into a crucible to slowly and spirally pull down the bottom pad to form a vanadium ingot with the diameter of 70mm, and peeling the vanadium ingot after the smelting is finished.
(4) Forging: the forging equipment is a 200 kg air hammer, the heating temperature is 1000 ℃, the heat preservation time is 20min, the initial forging temperature is 1050 ℃, the final forging temperature is 920 ℃, the vanadium ingot is processed to a vanadium metal rod with the diameter of 45mm, and peeling is carried out after forging.
(5) Vacuum annealing, namely annealing the vanadium metal rod with the vacuum degree of 1.3 × 10-5pa, annealing temperature of 980 ℃, heat preservation time of 30min, and furnace cooling.
(6) Plasma rotary electrode atomization, namely loading a vanadium rod into a rotary feeding device, and vacuumizing to 1.3 × 10-5And pa, filling helium with the purity of 99.99%, starting a rotary button and a plasma gun power supply, wherein the rotating speed of an electrode rod is 18000r/min, the current intensity is 1700A, and the feeding rate is 1.0mm/s, so that spherical vanadium powder with the granularity of 40-150 micrometers is formed.
Example 3:
(1) and (3) pressing and forming vanadium powder: pressing into a mold by using a cold isostatic press, filling vanadium powder into a long strip-shaped rubber mold sleeve, sealing, putting into the cold isostatic press, pressing at 260MPa for 60s, and taking out after demolding.
(2) Vacuum sintering, namely putting the pressed and formed vanadium strip into a vacuum intermediate frequency sintering furnace for sintering, wherein the vacuum degree is 1.5 × 10-5pa, the sintering system is that the temperature is preserved for 40min at 550 ℃, 60min at 1200 ℃, 150min at 1400 ℃, the heating rate is 10 ℃/min, and the sintering system is cooled along with the furnace.
(3) Electron beam melting, namely adopting a 250kw electron beam melting furnace, putting the sintered vanadium strip into the furnace through an inlet valve, and vacuumizing to 1.5 × 10-5pa, slowly feeding the vanadium strips into a bombardment area of an electron gun, and dripping molten vanadium metal into the water-cooled copper crucible. And dropping the vanadium liquid into a crucible to slowly and spirally pull down the bottom pad to form a vanadium ingot with the diameter of 60mm, and peeling the vanadium ingot after smelting.
(4) Forging: the forging equipment is a 200 kg air hammer, the heating temperature is 1050 ℃, the heat preservation time is 20min, the initial forging temperature is 1050 ℃, the final forging temperature is 950 ℃, the vanadium ingot is processed to a vanadium metal rod with the diameter of 30mm, and peeling is carried out after forging.
(5) Vacuum annealing, namely annealing the vanadium metal rod with the vacuum degree of 1.5 × 10-5pa, annealing temperature of 960 ℃, holding time of 35min, and furnace cooling.
(6) Plasma rotary electrode atomization, namely loading a vanadium rod into a rotary feeding device, and vacuumizing to 1.5 × 10-5And pa, filling helium with the purity of 99.99%, starting a rotary button and a plasma gun power supply, wherein the rotating speed of an electrode bar is 16000r/min, the current intensity is 1800A, and the feeding rate is 0.6mm/s, so that spherical vanadium powder with the granularity of 50-150 micrometers is formed.
The observation of the spherical vanadium powder obtained in the embodiments 1 to 3 by an electron microscope shows that the spherical vanadium powder has high sphericity, good fluidity, high tap density, good powder compactness, less pores and low content of hollow spheres.
Claims (6)
1. The preparation method of the spherical vanadium powder is characterized by comprising the following steps:
1) press forming
Filling vanadium powder into a die sleeve, and pressing into vanadium strips;
2) vacuum sintering
Sintering the vanadium strip in the step 1) in a vacuum furnace, and cooling along with the furnace;
3) electron beam melting
Putting the sintered vanadium strip into an electron beam smelting furnace, and vacuumizing to 10 DEG-4~10-5pa, melting the vanadium strips in the bombardment area, and carrying out ingot dummy on the vanadium liquid to obtain vanadium ingots;
4) forging
Heating the vanadium ingot in the step 3) to 900-1100 ℃, preserving heat for 10-25 min, forging, wherein the initial forging temperature is 1000-1100 ℃, and the final forging temperature is 850-950 ℃ to obtain a vanadium rod;
5) vacuum annealing
Step 4) the vanadium rod is in a vacuum degree of 10-4~10-5Annealing under pa, wherein the annealing temperature is 900-1000 ℃, the heat preservation time is 30-45 min, and furnace cooling is carried out;
6) plasma rotary electrode atomization
The vanadium rod annealed in the step 5) is vacuumized 10-4~10-5And pa, atomizing the vanadium rod into spherical vanadium powder with the granularity of 10-150 microns through a plasma rotating electrode in a protective atmosphere.
2. The method of claim 1, wherein: the pressing pressure in the step 1) is 200-280 MPa, and the pressure maintaining time is 60-120 s.
3. The method of claim 1, wherein: step 2) vacuum degree of vacuum sintering 10-5pa。
4. The method of claim 1, wherein: the sintering system in the step 2) is 400-600 ℃, and the temperature is kept for 30-60 min; preserving heat for 60-90 min at 1000-1200 ℃; and (3) preserving the heat at 1300-1500 ℃ for 120-150 min, wherein the temperature rise speed is 10 ℃/min.
5. The method of claim 1, wherein: and 6) the protective gas is helium.
6. The method of claim 1, wherein: step 7) the plasma rotating electrode atomization method comprises the following steps: the rotating speed of the electrode bar is 16000-19000 r/min, the current intensity is 1500-1800A, and the feeding rate is 0.6-1.0 mm/s.
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CN113770349A (en) * | 2021-09-14 | 2021-12-10 | 有研工程技术研究院有限公司 | High-purity spherical metal vanadium powder and preparation method and application thereof |
CN114367669A (en) * | 2021-12-15 | 2022-04-19 | 重庆材料研究院有限公司 | Preparation method of TaW10 alloy spherical powder for 3D printing |
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