CN111644631B - Preparation method of spherical vanadium powder - Google Patents
Preparation method of spherical vanadium powder Download PDFInfo
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- CN111644631B CN111644631B CN202010521104.2A CN202010521104A CN111644631B CN 111644631 B CN111644631 B CN 111644631B CN 202010521104 A CN202010521104 A CN 202010521104A CN 111644631 B CN111644631 B CN 111644631B
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- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 47
- 238000005242 forging Methods 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000010894 electron beam technology Methods 0.000 claims abstract description 14
- 238000003825 pressing Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000000889 atomisation Methods 0.000 claims abstract description 11
- 238000003723 Smelting Methods 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims description 15
- 238000002844 melting Methods 0.000 claims description 14
- 230000008018 melting Effects 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 8
- 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
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 4
- 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
- 238000004321 preservation Methods 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000010146 3D printing Methods 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
- 239000007789 gas Substances 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
- 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
-
- 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]
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention relates to a preparation method of 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 microns 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 having important significance 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 in China exist, and in the preparation method of the spherical vanadium powder, after induction melting is adopted, 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 droplets 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 -5 pa, 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 V ingot with phi 60-70 mm, and peeling the V ingot after the smelting is finished.
4) Forging
Heating the vanadium ingot obtained in the step 3) to 900-1100 ℃, keeping the temperature 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 -5 Annealing at 900-1000 ℃ for 30-45 min under pa, and cooling along with the furnace;
6) Plasma rotary electrode atomization
The vanadium rod annealed in the step 5) is vacuumized 10 -4 ～10 -5 Under pa, under the protective atmosphere of 99.99% helium, a vanadium rod is put into 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 atomized through 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 -5 pa。
The sintering system in the step 2) is 400-600 ℃, and the temperature is kept for 30-60 min; keeping the temperature at 1000-1200 ℃ for 60-90 min; the temperature is kept at 1300-1500 ℃ for 120-150 min, and the temperature rising 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 rotary swaging process is adopted, so that the vanadium rod is more uniform and compact in 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) And (3) vacuum sintering: the pressed and formed vanadium strip is put into a vacuum intermediate frequency sintering furnace for sintering, the vacuum degree is 1.0 multiplied by 10 -5 pa, the sintering system is that the temperature is kept for 60min at 450 ℃, 90min at 1000 ℃,120 min at 1500 ℃, the temperature rising speed is 10 ℃/min, and the sintering system is cooled 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, vacuumizing to 1.0 × 10 -5 pa, slowly feeding the vanadium strip 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: annealing the vanadium metal rod with the vacuum degree of 1.0 multiplied by 10 -5 pa, annealing temperature 950 ℃, holding time 45min, and furnace cooling.
(6) Plasma rotating electrode atomization: putting the vanadium rod into a rotary feeding device, and vacuumizing to 1.0 multiplied by 10 -5 And pa, filling helium with the purity of 99.99 percent, starting a rotary button and a plasma gun power supply, wherein the rotating speed of an electrode bar is 19000r/min, the current intensity is 1500A, and the feeding rate is 0.8mm/s, so that spherical vanadium powder with the granularity of 20-120 microns is formed.
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) And (3) vacuum sintering: putting the pressed and formed vanadium strip into a vacuum intermediate frequency sintering furnace for sintering, wherein the vacuum degree is 1.3 multiplied by 10 -5 pa, 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 rise speed is 10 ℃/min, and the sintering is cooled 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 1.3 multiplied by 10 -5 pa, 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) And (3) vacuum annealing: annealing the vanadium metal rod with the vacuum degree of 1.3 multiplied by 10 -5 pa, annealing temperature 980 ℃, holding time 30min, and furnace cooling.
(6) Plasma rotating electrode atomization: putting a vanadium rod into a rotary feeding device, and vacuumizing to 1.3 multiplied by 10 -5 And pa, filling helium with the purity of 99.99 percent, 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) And (3) vacuum sintering: putting the pressed and formed vanadium strip into a vacuum intermediate frequency sintering furnace for sintering, wherein the vacuum degree is 1.5 multiplied by 10 -5 pa, the sintering system is that the temperature is preserved at 550 ℃ for 40min, the temperature is preserved at 1200 ℃ for 60min, the temperature is preserved at 1400 ℃ for 150min, the temperature rising speed is 10 ℃/min, and the sintering is cooled 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 1.5 multiplied by 10 -5 pa, slowly feeding the vanadium strip 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: annealing the vanadium metal rod with the vacuum degree of 1.5 multiplied by 10 -5 pa, annealing temperature of 960 ℃, holding time of 35min, and furnace cooling.
(6) Plasma rotating electrode atomization: putting the vanadium rod into a rotary feeding device, and vacuumizing to 1.5 multiplied by 10 -5 And pa, filling helium with the purity of 99.99 percent, 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 microns 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 (4)
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;
the sintering system is 400-600 ℃, and the temperature is kept for 30-60 min; keeping the temperature at 1000-1200 ℃ for 60-90 min; the temperature is kept between 1300 ℃ and 1500 ℃ for 120min to 150min, and the temperature rise speed is 10 ℃/min;
3) Electron beam melting
Putting the sintered vanadium strip into an electron beam smelting furnace, and vacuumizing to 10 DEG -4 ～10 -5 pa, 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 obtained in the step 3) to 900-1100 ℃, keeping the temperature 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 -5 Annealing at 900-1000 ℃ for 30-45 min under pa, and cooling along with the furnace;
6) Plasma rotary electrode atomization
The vanadium rod annealed in the step 5) is vacuumized 10 -4 ～10 -5 Under pa, atomizing a vanadium rod into spherical vanadium powder with the granularity of 10-150 microns through a plasma rotating electrode in a protective atmosphere;
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.
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 -5 pa。
4. The method of claim 1, wherein: and 6) helium is used as the protective atmosphere.
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