CN115502405A - Method for preparing spherical nickel powder by using controllable plasma method - Google Patents
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- CN115502405A CN115502405A CN202211091732.7A CN202211091732A CN115502405A CN 115502405 A CN115502405 A CN 115502405A CN 202211091732 A CN202211091732 A CN 202211091732A CN 115502405 A CN115502405 A CN 115502405A
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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
- B22F9/026—Spray drying of solutions or suspensions
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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
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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
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE 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
- B33Y70/00—Materials specially adapted for additive manufacturing
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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
- 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 method for preparing spherical nickel powder by using a controllable plasma method, which comprises the steps of firstly mixing polyvinyl alcohol (PVA) with raw material nickel powder to prepare 0.5-2.5 g/L feed liquid, and preparing spherical precursor nickel powder from the feed liquid by a spray granulation method; the precursor nickel powder is treated by controllable plasma spheroidizing equipment to obtain the compact spherical nickel powder. The spheroidized powder of the invention has high quality and low equipment operation cost, and can solve the problem of generating by-products in the powder preparation process in the prior art while ensuring simple process and easy operation as much as possible.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a method for preparing spherical nickel powder by using a controllable plasma method.
Background
The metal nickel is widely applied in modern industry, pure nickel has excellent welding performance, processing performance and mechanical performance, meanwhile, pure nickel also has excellent corrosion resistance, higher electric vacuum performance and electromagnetic control performance, and is widely applied to the aspects of mechanical electronics, chemical engineering and the like, and pure nickel has high melting point, excellent corrosion resistance and good hot pressure processing performance, so the pure nickel is widely applied to the aspects of precision instrument components, medical instruments and the like. With the rapid development of 3D printing technology, the requirements for powder materials are also higher and higher, so that the preparation of spherical powder with excellent quality has a crucial influence on the performance of shaped parts.
At present, the preparation methods of metal powder for 3D printing mainly include electrode induction atomization (EIGA), plasma rotating electrode atomization (PREP), induction plasma spheroidization (PA), vacuum induction melting gas atomization (VIGA), and water atomization. Segregation of an electrode during electrode induction atomization (EIGA) smelting can cause uneven components of alloy powder to a certain extent, the whole particle size distribution of the powder is wide, and more satellite powder, special-shaped powder and hollow powder exist in particles, so that the flowability of the powder is reduced, and the loose packing density and the tap density are low. The yield of fine powder by the rotary electrode process (PREP) is less than 10%, and the cost is relatively high. The induction plasma spheroidization (PA) method is a method for preparing spherical metal powder by utilizing plasma heat source atomization. The preparation process of the gas atomization method (VIGA) is easy to be polluted, and the preparation requirement of high-activity and high-purity alloy powder cannot be met. In the water atomization method (WA), the shape of metal molten drops is often irregular due to too fast condensation, the sphericity of powder is often difficult to ensure, the particle size distribution of the powder is relatively dispersed, and meanwhile, part of metals and alloys with high activity, such as aluminum, can contact with water and react, so that the oxygen content in the powder is increased, and the high oxygen content is easy to deteriorate the mechanical property of products.
The powder making process with controllable plasma process has the basic principle that controllable induction electromagnetic field acts on water cooled copper ring to ionize work gas and produce plasma, so as to shrink and spheroidize material powder to prepare compact spherical powder. The method can effectively control the gas ionization degree, further control the temperature and realize the spheroidization and alloying of the raw material powder. Meanwhile, the production flow is shortened, the equipment operation cost is reduced, the volatilization of low-melting-point components is avoided, alloy powder which is in accordance with the design is obtained, and the 3D printing powder is prepared.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing spherical nickel powder by using a controllable plasma method, wherein the quality of the spheroidized powder is high, and the equipment operation cost is low.
In order to solve the problems, the method for preparing the spherical nickel powder by using the controllable plasma method is characterized by comprising the following steps: firstly, mixing polyvinyl alcohol (PVA) and a raw material nickel powder to prepare a feed liquid of 0.5-2.5 g/L, and preparing the feed liquid into a precursor nickel powder of a sphere-like shape by a spray granulation method; the precursor nickel powder is treated by controllable plasma spheroidizing equipment to obtain the compact spherical nickel powder.
The precursor nickel powder is prepared by the following method: after passing through a sieve of 60 to 120 meshes, the feed liquid is pumped to a nozzle in the middle of a drying chamber of a spray dryer by a high-pressure pump, and the feed liquid is rapidly atomized and dried to form granular nickel powder; the particle nickel powder is prepared by sintering and degumming.
The spray drying condition is that the temperature is 240 to 400 ℃.
The sintering condition is that the particle nickel powder is put into a pusher furnace to be sintered, the atmosphere is hydrogen, the temperature is 800 ℃, and the sintering time is 1~2 hours.
The degumming condition is that the sintered particle nickel powder is put into a pusher furnace to be degummed, the atmosphere is hydrogen, the dew point of the hydrogen is 45, and the degumming time is 1~2 hours.
The controllable plasma spheroidizing equipment comprises a plasma torch furnace body, a vacuum system and a collecting system; the powder inlet at the top of the plasma torch body and the bottom of the plasma torch body are connected with the collecting system through a quencher; the powder inlet is connected with a powder feeding pipe, and the powder feeding pipe passes through the built-in preheating cavity and is connected with a feeding system; the plasma torch furnace body is internally provided with a primary plasma heating area and a secondary plasma heating area from top to bottom, and is connected with the vacuum system through a pipeline.
The plasma in the plasma torch body is tungsten.
The compact spherical nickel powder is prepared by the following method:
the controllable plasma spheroidizing equipment is characterized in that pre-vacuumizing is repeated for several times before operation, so that original gas is completely discharged;
before starting arc, filling argon with the purity of 95% into a vacuum system, so that the reaction chamber is in a protective atmosphere environment; the three-phase 380V alternating current is converted into direct current through a voltage regulator, a high-rectification transformer and a high-voltage silicon rectifier, then is converted into high-frequency current through a high-frequency oscillator, high-frequency energy is added to an induction coupling coil, argon is used as ionized gas, a stable high-heat-energy vortex region is formed through a high-frequency electromagnetic field, and the gas is continuously ionized under the action of a tungsten plasma torch, so that a high-temperature plasma torch is formed; after the plasma torch runs stably, a mechanical pump is adopted to pre-pump the plasma torch to the vacuum degree of 0.1-0.3 atmospheric pressure, and the effect of guiding powder and plasma airflow is achieved;
thirdly, introducing working gas formed by mixed gas of argon and hydrogen into a vacuum chamber in the vacuum system, switching on high voltage, adjusting the voltage to be 400-800V, simultaneously inputting the working gas, side gas and carrier gas into the plasma torch, switching on a heating and ignition button, and instantly forming a self-sustaining plasma torch; the working air flow for gas flow arcing is 3 to 10L/min, the side air flow is 5 to 30L/min, and the carrier air flow is 1 to 20L/min;
fourthly, starting a feeding system, and conveying the precursor nickel powder carried by carrier gas into a primary plasma heating area and a secondary plasma heating area through the feeding system for spheroidization, wherein the powder conveying speed is 20 to 50g/min; the powder particles pass through a plasma high-temperature area to absorb heat, melt and spheroidize instantly, and are condensed into spherical liquid drops under the action of surface tension;
fifthly, enabling the spherical liquid drops to enter a cooling chamber, quickly condensing the liquid drops into spherical powder through a quencher, and collecting the powder in a collecting system to obtain compact spherical nickel powder; and (4) opening the electromagnetic valve at regular time, and enabling the powder to enter the powder collecting tank through a discharge hole of the collecting system.
The hydrogen in the mixed gas of the argon and the hydrogen accounts for 5 to 20 percent of the total volume, and the pressure is one atmosphere.
The average particle size of the compact spherical nickel powder is 1.0-200 mu m.
Compared with the prior art, the invention has the following advantages:
1. the precursor nickel powder is prepared by a spray granulation method, and can meet the size requirement of the spherical nickel powder for 3D printing; and spheroidizing by using a plasma spheroidizing method, wherein the obtained powder can meet the requirements of the spherical nickel powder for 3D printing on the performances such as flowability, apparent density and the like. Therefore, the invention can solve the problem that by-products are generated in the powder preparation process in the prior art while ensuring simple and easy operation of the process as much as possible.
2. The invention utilizes the controllable plasma spheroidizing equipment to generate plasma, so that the raw material powder is shrunk and spheroidized, thereby preparing the compact spherical powder, the average granularity of the prepared spherical powder is 1.0-200 mu m, and the spheroidization rate is more than or equal to 97 percent.
3. The method can effectively reduce the ionization degree of the gas and further control the temperature, thereby realizing the aim of spheroidizing the raw material powder, shortening the production flow and reducing the operation cost of equipment.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a schematic flow chart of the present invention.
Fig. 2 is a schematic structural diagram of a controllable plasma spheroidizing device in the present invention.
FIG. 3 is an SEM image of a precursor nickel powder prepared by a spray granulation method according to the present invention.
FIG. 4 is an SEM image of spherical nickel powder prepared by a plasma method according to the present invention.
FIG. 5 is a graph of the movement trace of the precursor nickel powder of the present invention in a plasma.
FIG. 6 is an SEM image of spherical nickel powders prepared at different feed rates in accordance with the present invention; wherein, (a) 20g/min; (b) 50g/min.
In the figure: 1-plasma torch body; 2-a collection system; 3-quenching the cooler; 4-powder feeding pipe; 5-preheating chamber; 6-primary plasma heating zone; 7-secondary plasma heating zone.
Detailed Description
As shown in figure 1, a method for preparing spherical nickel powder by using a controllable plasma method is characterized in that firstly, polyvinyl alcohol (PVA) is mixed with raw material nickel powder to prepare 0.5-2.5 g/L feed liquid, and the feed liquid is prepared into spheroidal precursor nickel powder with fluidity by a spray granulation method; the precursor nickel powder is treated by controllable plasma spheroidizing equipment to obtain compact spherical nickel powder with the average particle size of 1.0-200 mu m.
Wherein: the precursor nickel powder is prepared by the following method: after passing through a sieve of 60-120 meshes, the feed liquid is pumped to a nozzle in the middle of a drying chamber of a spray dryer by a high-pressure pump, and the feed liquid is rapidly atomized under the condition of 240-400 ℃, so that the surface area of liquid drops is greatly increased, the liquid drops meet and contact with hot air, the water is rapidly evaporated, and the material is dried into particle nickel powder in a very short time; the particle nickel powder is firstly put into a pusher furnace for sintering, the atmosphere is hydrogen, the temperature is 800 ℃, the sintering time is 1~2 hours, then the sintered particle nickel powder is put into the pusher furnace for degumming, the atmosphere is hydrogen, the dew point of the hydrogen is 45, and the degumming time is 1~2 hours, so that the precursor nickel powder is obtained.
The controllable plasma spheroidizing apparatus includes a plasma torch body 1, a vacuum system, and a collection system 2 (shown in FIG. 2). The top powder inlet and the bottom of the plasma torch body 1 are connected with a collecting system 2 through a quencher 3; the powder inlet is connected with a powder feeding pipe 4, and the powder feeding pipe 4 passes through a built-in preheating cavity 5 to be connected with a feeding system; a primary plasma heating zone 6 and a secondary plasma heating zone 7 are arranged in the plasma torch body 1 from top to bottom and are connected with a vacuum system through pipelines.
The plasma in the plasma torch body 1 is tungsten.
The compact spherical nickel powder is prepared by the following method:
the controllable plasma spheroidizing equipment is characterized in that pre-vacuumizing is repeated for several times before operation, so that original gas is completely exhausted.
Before starting arc, filling argon with the purity of 95% into a vacuum system, so that the reaction chamber is in a protective atmosphere environment; the three-phase 380V alternating current is converted into direct current through a voltage regulator, a high-rectification transformer and a high-voltage silicon rectifier, then is converted into high-frequency current through a high-frequency oscillator, high-frequency energy is added to an induction coupling coil, argon is used as ionized gas, a stable high-heat-energy vortex region is formed through a high-frequency electromagnetic field, and the gas is continuously ionized under the action of a tungsten plasma torch, so that a high-temperature plasma torch is formed; after the plasma torch runs stably, the plasma torch is pre-pumped to the vacuum degree of 0.1-0.3 atmospheric pressure by a low-power mechanical pump, and the effect of guiding powder and plasma airflow is achieved.
And thirdly, introducing a working gas consisting of a mixed gas of argon and hydrogen into a vacuum chamber in the vacuum system, wherein the argon forms a protective atmosphere, and the hydrogen forms a reducing atmosphere. Connecting a high voltage, adjusting the voltage to be 400-800V, simultaneously inputting working gas, side gas and carrier gas into a plasma torch, connecting a heating button and an ignition button, and instantly forming a self-sustaining plasma torch; the working air flow for gas flow arcing is 3 to 10L/min, the side air flow is 5 to 30L/min, and the carrier air flow is 1 to 20L/min; the carrier gas and the edge gas are both argon. The hydrogen in the mixed gas of argon and hydrogen accounts for 5 to 20 percent of the total volume, and the pressure is one atmosphere.
Fourthly, starting the feeding system, and conveying the precursor nickel powder carried by carrier gas into the primary plasma heating zone 6 and the secondary plasma heating zone 7 through the feeding system for spheroidization, wherein the powder conveying speed is 20 to 50g/min; the powder particles pass through a plasma high-temperature zone to absorb heat, melt and spheroidize instantly, and are condensed into spherical liquid drops under the action of surface tension.
Fifthly, enabling the spherical liquid drops to enter a cooling chamber, quickly condensing the liquid drops into spherical powder through a quencher 3, and collecting the powder in a collecting system 2 to obtain compact spherical nickel powder; and (4) opening the electromagnetic valve at regular time, and enabling the powder to enter the powder collecting tank through a discharge hole of the collecting system 2.
The raw material nickel powder is irregular particles (as shown in fig. 3), the precursor nickel powder is loose spherical shell (as shown in fig. 4), contains certain organic matters, and is not suitable for 3D printing and forming.
After plasma spheroidizing, the loose powder can be densified to obtain the dense spherical powder. Organic matters are gasified due to the high temperature effect in the plasma spheroidizing process, and a small amount of hydrogen in the plasma is helpful for reducing the powder, as shown in 5~6.
The starting materials in the present invention are all commercially available.
Claims (10)
1. A method for preparing spherical nickel powder by using a controllable plasma method is characterized by comprising the following steps: firstly, mixing polyvinyl alcohol and a raw material nickel powder to prepare a feed liquid of 0.5-2.5 g/L, and preparing the spherical precursor nickel powder from the feed liquid by a spray granulation method; the precursor nickel powder is processed by controllable plasma spheroidizing equipment to obtain the compact spherical nickel powder.
2. The method for preparing spherical nickel powder according to claim 1, wherein the method comprises the steps of: the precursor nickel powder is prepared by the following method: the feed liquid passes through a sieve of 60 to 120 meshes and is conveyed to a nozzle in the middle of a drying chamber of a spray dryer by a high-pressure pump, and the feed liquid is rapidly atomized and dried to form nickel powder particles; the particle nickel powder is prepared by sintering and degumming.
3. The method for preparing spherical nickel powder using a controlled plasma method according to claim 2, wherein: the spray drying condition is that the temperature is 240 to 400 ℃.
4. The method for preparing spherical nickel powder using a controlled plasma method according to claim 2, wherein: the sintering condition is that the particle nickel powder is put into a pusher furnace to be sintered, the atmosphere is hydrogen, the temperature is 800 ℃, and the sintering time is 1~2 hours.
5. The method for preparing spherical nickel powder using a controlled plasma method according to claim 2, wherein: the degumming condition is that the sintered particle nickel powder is put into a pusher furnace to be degummed, the atmosphere is hydrogen, the dew point of the hydrogen is 45, and the degumming time is 1~2 hours.
6. The method for preparing spherical nickel powder according to claim 1, wherein the method comprises the steps of: the controllable plasma spheroidizing equipment comprises a plasma torch furnace body (1), a vacuum system and a collecting system (2); the top powder inlet and the bottom of the plasma torch body (1) are connected with the collecting system (2) through a quencher (3); the powder inlet is connected with a powder feeding pipe (4), and the powder feeding pipe (4) passes through a built-in preheating cavity (5) to be connected with a feeding system; a primary plasma heating zone (6) and a secondary plasma heating zone (7) are arranged in the plasma torch body (1) from top to bottom and are connected with the vacuum system through pipelines.
7. The method for preparing spherical nickel powder according to claim 6, wherein the method comprises the steps of: the plasma in the plasma torch body (1) is tungsten.
8. The method for preparing spherical nickel powder according to claim 1, wherein the method comprises the steps of: the compact spherical nickel powder is prepared by the following method:
the controllable plasma spheroidizing equipment is characterized in that pre-vacuumizing is repeated for several times before operation, so that original gas is completely discharged;
before starting arc, filling argon with the purity of 95% into a vacuum system, so that the reaction chamber is in a protective atmosphere environment; the three-phase 380V alternating current is converted into direct current through a voltage regulator, a high-rectification transformer and a high-voltage silicon rectifier, then is converted into high-frequency current through a high-frequency oscillator, high-frequency energy is added to an induction coupling coil, argon is used as ionized gas, a stable high-heat-energy vortex region is formed through a high-frequency electromagnetic field, and the gas is continuously ionized under the action of a tungsten plasma torch, so that a high-temperature plasma torch is formed; after the plasma torch runs stably, the vacuum degree is pre-pumped to 0.1 to 0.3 atmospheric pressure by a mechanical pump, and the function of guiding powder and plasma airflow is achieved;
thirdly, introducing working gas formed by mixed gas of argon and hydrogen into a vacuum chamber in the vacuum system, switching on high voltage, adjusting the voltage to be 400-800V, simultaneously inputting the working gas, side gas and carrier gas into the plasma torch, switching on a heating and ignition button, and instantly forming a self-sustaining plasma torch; the working air flow for gas flow arcing is 3 to 10L/min, the side air flow is 5 to 30L/min, and the carrier air flow is 1 to 20L/min;
fourthly, starting a feeding system, and conveying the precursor nickel powder carried by carrier gas into a primary plasma heating zone (6) and a secondary plasma heating zone (7) through the feeding system for spheroidizing, wherein the powder conveying speed is 20-50g/min; the powder particles pass through a plasma high-temperature area to absorb heat, melt and spheroidize instantly, and are condensed into spherical liquid drops under the action of surface tension;
the spherical liquid drops enter the cooling chamber, are rapidly condensed into spherical powder through the quencher (3), and are collected in the collection system (2), so that the dense spherical nickel powder is obtained; and (3) opening the electromagnetic valve at regular time, and enabling the powder to enter the powder collecting tank through a discharge hole of the collecting system (2).
9. The method for preparing spherical nickel powder according to claim 8, wherein the method comprises the steps of: the hydrogen in the mixed gas of the argon and the hydrogen accounts for 5 to 20 percent of the total volume, and the pressure is one atmosphere.
10. The method for preparing spherical nickel powder according to claim 1 or 8, wherein: the average particle size of the compact spherical nickel powder is 1.0-200 mu m.
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