CN111804926A - Method for preparing refractory metal powder - Google Patents
Method for preparing refractory metal powder Download PDFInfo
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- CN111804926A CN111804926A CN202010638152.XA CN202010638152A CN111804926A CN 111804926 A CN111804926 A CN 111804926A CN 202010638152 A CN202010638152 A CN 202010638152A CN 111804926 A CN111804926 A CN 111804926A
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- 239000000843 powder Substances 0.000 title claims abstract description 78
- 239000003870 refractory metal Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910052751 metal Inorganic materials 0.000 claims abstract description 33
- 239000002184 metal Substances 0.000 claims abstract description 33
- 230000001681 protective effect Effects 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000000725 suspension Substances 0.000 claims abstract description 18
- 238000002844 melting Methods 0.000 claims abstract description 16
- 230000008018 melting Effects 0.000 claims abstract description 16
- 239000002923 metal particle Substances 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 11
- 230000006698 induction Effects 0.000 claims abstract description 11
- 238000007670 refining Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 229910001338 liquidmetal Inorganic materials 0.000 claims abstract description 9
- 238000009833 condensation Methods 0.000 claims abstract description 8
- 230000005494 condensation Effects 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000003723 Smelting Methods 0.000 claims abstract description 7
- 239000007769 metal material Substances 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 9
- 239000007789 gas Substances 0.000 description 34
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 238000000889 atomisation Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 7
- 230000008569 process Effects 0.000 description 5
- 239000000498 cooling water Substances 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 239000010955 niobium Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- CSDQQAQKBAQLLE-UHFFFAOYSA-N 4-(4-chlorophenyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine Chemical compound C1=CC(Cl)=CC=C1C1C(C=CS2)=C2CCN1 CSDQQAQKBAQLLE-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000001883 metal evaporation Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
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
- B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material
Abstract
The invention relates to a method for preparing refractory metal powder, belonging to the technical field of metal powder preparation. Processing refractory metal raw materials into particles; placing the obtained granular raw materials in an induction coil of electromagnetic suspension refining equipment, introducing protective gas pure Ar, and suspending and melting the metal particles into liquid suspended in the air after switching on a power supply; continuing suspension smelting of suspended metal particles, evaporating liquid metal when the temperature of liquid metal droplets is far higher than the melting temperature of the liquid metal droplets to generate metal powder suspended in protective gas, and collecting condensed powder in the protective gas at a gas outlet after condensation; and drying the condensed powder to prepare the refractory metal powder. The method can solve the problem of preparing the powder of the refractory metal material, and can realize the fast, simple and environment-friendly preparation of the refractory metal powder.
Description
Technical Field
The invention relates to a method for preparing refractory metal powder, belonging to the technical field of metal powder preparation.
Background
Refractory metals play an important role in the development of new materials and the improvement of the performance of existing materials. For new materials with higher precision, the added alloy elements need to meet the requirements of granularity and quality at the same time. At present, the main preparation methods of metal powder are a plasma rotating electrode method, a gasification atomization method and a physical chemical method.
The plasma rotating electrode method is easy to prepare spherical powder with better sphericity but not easy to prepare powder, and the material utilization rate is not high; the gasification atomization method is divided into a traditional atomization technology and a novel atomization technology, the traditional atomization technology is suitable for preparing low-melting-point metal powder such as aluminum, the hot gas atomization method in the novel atomization technology can provide higher atomization rate and is widely applied to the production of alloy powder such as stainless steel, iron alloy, nickel alloy, magnetic material and the like, but due to the special design of a heating nozzle, few mechanisms are researched; the physical chemical method is a mature process technology for manufacturing metal powder, but the method is only limited to metal materials which are easy to react with hydrogen and have increased brittleness after absorbing hydrogen so as to be easy to break. In light of the above process characteristics, progress has been made in the preparation of refractory metal powders.
Niobium powder is an important component element in high-end technology products such as aviation, low-temperature superconduction and the like, and can improve the heat resistance, strength and thermal conductivity of the products. The current molten salt electrolysis method can be used for preparing niobium powder, because the graphite anode and the graphite cathode are simultaneously dissolved in the molten salt, the control of the potential in the molten salt, the precipitation of impurities at the cathode and side reactions caused by the impurities are all the problems encountered at present, and meanwhile, the preparation of the method also needs to consume a large amount of time over 12 hours. CN200610149612 describes a method for preparing niobium powder for powder metallurgy, which comprises: pressing the powder into a billet, performing vacuum sintering, preparing powder by hydrogenation, performing deoxidation and dehydrogenation heat treatment, and then performing acid washing, water washing and drying to obtain the niobium powder.
The titanium powder is widely applied to the fields of aerospace, medical appliances, metallurgy and the like, and has the advantages of reducing the weight of materials, improving the strength, resisting acid and alkali corrosion and the like. CN201711022391 describes a method for preparing titanium powder, which comprises: mixing, pressing and sintering a titanium material and calcium oxide, mixing and pressing a sintered product and calcium hydride to obtain a pre-reduced blank, performing vacuum thermal reduction to obtain a crude product, and performing acid washing, water washing and drying on the crude product to finally obtain titanium powder, wherein the whole process takes 6 hours or more.
At present, the methods can realize the preparation of refractory metal powder, but the methods have the problems of complicated equipment, long process route, long consumption time and environmental pollution caused by generated by-products or used solvents.
Disclosure of Invention
In view of the problems and deficiencies of the prior art, the present invention provides a method for producing refractory metal powder. The method can solve the problem of preparing the powder of the refractory metal material, and can realize the fast, simple and environment-friendly preparation of the refractory metal powder.
In order to solve the technical problem, the invention adopts the following technical scheme:
a method of producing refractory metal powder comprising the steps of:
step 1: wire cutting or grinding refractory metal raw materials into particles, wherein the particle size of the particles is about less than 16 mm;
step 2: placing the granular raw materials obtained in the step 1 in an induction coil of electromagnetic suspension refining equipment, introducing protective gas pure Ar, and controlling a power supply system: inputting current of 200-400A, input power of 3000-4500W and input frequency of 180-450 kHz, and suspending and melting metal particles into liquid state suspended in the air after the power supply is switched on;
and step 3: continuing suspension smelting of the metal particles suspended in the step 2, evaporating the liquid metal when the temperature of the liquid metal molten drops is far higher than the melting temperature of the liquid metal molten drops to generate metal powder suspended in the protective gas, and collecting condensed powder in the protective gas at a gas outlet after condensation;
and 4, step 4: and (4) drying the condensed powder obtained in the step (3) to prepare refractory metal powder.
In the step 1, the refractory metal raw material is a metal material with a melting point below 3000K, such as: niobium having a melting point of 2750K, titanium having a melting point of 1933K, nickel having a melting point of 1728K, and the like.
And in the step 2, the flow speed of the protective gas pure Ar gas is 0.5-1.5L/min.
And the time for collecting the condensed powder in the steps 2 to 3 is 50-120 min.
The electromagnetic suspension refining equipment in the step 2 and the step 3 is shown in fig. 1, and comprises a temperature measuring system, a power supply system, main body equipment and a filtering system, wherein a prism is arranged at the top of the main body equipment, a protective gas pure Ar inlet is arranged at the upper part of the side surface of the main body equipment, a magnetic induction coil is arranged in the middle of the main body equipment and is connected with the power supply system, a gas outlet is arranged at the lower part of the side surface of the main body equipment, the filtering system (such as a bag filter) is arranged outside the powder outlet, and the temperature measuring system is used for measuring the temperature of the.
The principle of the method is as follows:
(1) the electromagnetic suspension principle is as follows: when the induction coil is introduced with high-frequency alternating current, Lorentz force opposite to the gravity direction is generated inside the induction coil, and when the Lorentz force is larger than or equal to the gravity of the molten drop, the metal material is suspended; meanwhile, the high-frequency alternating current generates a changing magnetic field to cause the change of magnetic flux inside the coil, so that the metal raw material generates induction current to generate joule heat, and when the temperature is higher than the melting point of the metal material, the metal material is melted from a solid state to a liquid state molten drop.
(2) The principle of evaporation powder preparation: when the metal material is melted and heated to a higher temperature, the metal material is evaporated and generates steam, and metal steam condensation nucleation and grain growth occur in the process of continuous friction collision between atoms in the steam and inert protective gas atoms, and metal powder is formed.
The evaporation amount can be represented by the following formula:
wherein N is the metal evaporation capacity, R is the molar gas constant, T is the evaporation time, T is the metal temperature, s is the evaporation surface area, M is the relative atomic mass of the metal, pmThe vapor pressure of the metal at a temperature T (K).
The invention has the beneficial effects that:
1. the method can realize the preparation of refractory metal powder with high melting point and high activity, and provides a new method for the preparation of refractory metal powder.
2. Compared with the existing metal powder preparation technology, the method has the advantages of simple and convenient operation, short flow and less time consumption, and can realize the rapid preparation of the infusible metal powder.
3. Compared with the prior art for preparing metal powder, the method does not use chemical solvents such as leaching solution and the like, avoids the generation of waste residues or harmful byproducts, and avoids the pollution to the environment.
4. The method is completed by electromagnetic suspension refining equipment, the metal material is not contacted with a crucible in the powder preparation process, the metal material is prevented from being polluted, the high-activity and high-quality metal powder can be obtained, strong electromagnetic stirring is carried out in the material, the internal components are uniform, the surface updating speed is high, and the preparation of the metal powder which is uniform in components and difficult to melt is facilitated.
Drawings
FIG. 1 is a diagram of an electromagnetic suspension refining apparatus of the present invention.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
Example 1
As shown in FIG. 1, the method for preparing refractory metal powder comprises the following steps:
step 1: performing wire cutting and grinding on a refractory metal raw material niobium, and processing into particles, wherein the particle size of the particles is 10 mm;
step 2: placing 3.5g of the granular raw material obtained in the step 1 in an induction coil of electromagnetic suspension refining equipment, introducing protective gas pure Ar (the gas flow rate is 1.0L/min), opening coil cooling water and electrifying after introducing gas for 3min, and controlling a power supply system: the input current is 400A, the input power is 4500W, the input frequency is 400kHz, and after the power supply is switched on, metal particles are suspended and melted into liquid state and suspended in the air;
and step 3: continuing suspension smelting of the metal particles suspended in the step 2, evaporating molten drops when the temperature reaches 2950K to generate metal powder suspended in the protective gas, and collecting condensed powder in the protective gas at a gas outlet after condensation;
and 4, step 4: and (4) putting the condensed powder obtained in the step (3) into a drying box, and keeping the temperature for 373K for 30min to prepare the niobium metal powder.
The time for completion of collecting the condensed powder in the steps 2 to 3 is 75 min.
In this example, 2.9g of metal powder was produced, and the fine powder yield reached 82.8%.
Example 2
As shown in FIG. 1, the method for preparing refractory metal powder comprises the following steps:
step 1: carrying out wire cutting and grinding on metal titanium which is a refractory metal raw material, and processing the metal titanium into particles, wherein the particle size of the particles is 11 mm;
step 2: placing 2.5g of the granular raw material obtained in the step 1 in an induction coil of electromagnetic suspension refining equipment, introducing protective gas pure Ar (the gas flow rate is 1.0L/min), opening coil cooling water and electrifying after introducing gas for 3min, and controlling a power supply system: inputting current 300A, input power 4000W and input frequency 330kHz, and suspending and melting metal particles into liquid to suspend in the air after the power supply is switched on;
and step 3: continuing suspension smelting of the metal particles suspended in the step 2, evaporating molten drops when the temperature reaches 2133K to generate metal powder suspended in protective gas, and collecting condensed powder in the protective gas at a gas outlet after condensation;
and 4, step 4: and (4) putting the condensed powder obtained in the step (3) into a drying box, and keeping the temperature for 373K for 30min to prepare the metal titanium powder.
The time for completion of collecting the condensed powder in the steps 2 to 3 was 115 min.
This example produced 2.2g of powder, with a fines yield of 88%.
Example 3
As shown in FIG. 1, the method for preparing refractory metal powder comprises the following steps:
step 1: carrying out wire cutting and grinding on metal nickel which is a refractory metal raw material, and processing the metal nickel into particles, wherein the particle size of the particles is 10 mm;
step 2: placing 3.2g of the granular raw material obtained in the step 1 in an induction coil of electromagnetic suspension refining equipment, introducing protective gas pure Ar (the gas flow rate is 1.5L/min), opening coil cooling water and electrifying after introducing gas for 3min, and controlling a power supply system: inputting current 280A, input power 3500W and input frequency 220kHz, and suspending and melting metal particles into liquid suspended in the air after the power supply is switched on;
and step 3: continuing suspension smelting of the metal particles suspended in the step 2, evaporating molten drops when the temperature reaches 1928K to generate metal powder suspended in the protective gas, and collecting condensed powder in the protective gas at a gas outlet after condensation;
and 4, step 4: and (4) putting the condensed powder obtained in the step (3) into a drying box, and keeping the temperature for 373K for 30min to prepare the metallic nickel powder.
The time for completion of collecting the condensed powder in the steps 2 to 3 is 80 min.
This example produced 2.8g of powder, with a fines yield of 87.5%.
Example 4
As shown in FIG. 1, the method for preparing refractory metal powder comprises the following steps:
step 1: carrying out wire cutting or grinding on a metal copper raw material, and processing the metal copper raw material into granules, wherein the granularity of the granules is 9 mm;
step 2: placing 3.4g of the granular raw material obtained in the step 1 in an induction coil of electromagnetic suspension refining equipment, introducing protective gas pure Ar (the gas flow rate is 1.0L/min), opening coil cooling water and electrifying after introducing gas for 3min, and controlling a power supply system: inputting current 200A, input power 3800W and input frequency 180kHz, and suspending and melting metal particles into liquid suspended in the air after the power supply is switched on;
and step 3: continuing suspension smelting of the metal particles suspended in the step 2, evaporating molten drops when the temperature reaches 1557K to generate metal powder suspended in the protective gas, and collecting condensed powder in the protective gas at a gas outlet after condensation;
and 4, step 4: and (4) putting the condensed powder obtained in the step (3) into a drying box, and keeping the temperature for 373K for 30min to prepare the metal copper powder.
The time for completion of collecting the condensed powder in the steps 2 to 3 was 95 min.
This example produced 3g of powder with a fines yield of 88.2%.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (4)
1. A method for preparing refractory metal powder is characterized by comprising the following steps:
step 1: performing linear cutting or grinding on a refractory metal raw material, and processing the refractory metal raw material into particles;
step 2: placing the granular raw materials obtained in the step 1 in an induction coil of electromagnetic suspension refining equipment, introducing protective gas pure Ar, and controlling a power supply system: inputting current of 200-400A, input power of 3000-4500W and input frequency of 180-450 kHz, and suspending and melting metal particles into liquid state suspended in the air after the power supply is switched on;
and step 3: continuing suspension smelting of the metal particles suspended in the step 2, evaporating the liquid metal when the temperature of the liquid metal molten drops is far higher than the melting temperature of the liquid metal molten drops to generate metal powder suspended in the protective gas, and collecting condensed powder in the protective gas at a gas outlet after condensation;
and 4, step 4: and (4) drying the condensed powder obtained in the step (3) to prepare refractory metal powder.
2. The method for producing a refractory metal powder as defined in claim 1, wherein: in the step 1, the refractory metal raw material is a metal material with a melting point below 3000K.
3. The method for producing a refractory metal powder as defined in claim 1, wherein: and in the step 2, the flow speed of the protective gas pure Ar gas is 0.5-1.5L/min.
4. The method for producing a refractory metal powder as defined in claim 1, wherein: and the time for collecting the condensed powder in the steps 2 to 3 is 50-120 min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112946012A (en) * | 2021-03-08 | 2021-06-11 | 昆明理工大学 | Device and method for measuring melting point of metal alloy |
| CN113252863A (en) * | 2021-04-19 | 2021-08-13 | 昆明理工大学 | Electromagnetic suspension device and method for detecting evolution of metal alloy solidification structure |
| CN115533109A (en) * | 2022-03-01 | 2022-12-30 | 哈尔滨工业大学（深圳） | Device and method for manufacturing tin ball based on magnetic suspension technology |
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| CN113252863A (en) * | 2021-04-19 | 2021-08-13 | 昆明理工大学 | Electromagnetic suspension device and method for detecting evolution of metal alloy solidification structure |
| CN115533109A (en) * | 2022-03-01 | 2022-12-30 | 哈尔滨工业大学（深圳） | Device and method for manufacturing tin ball based on magnetic suspension technology |
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