CN110919017B - Method and device for preparing spherical metal powder by hot wire assisted plasma arc - Google Patents

Method and device for preparing spherical metal powder by hot wire assisted plasma arc Download PDF

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CN110919017B
CN110919017B CN201911327904.4A CN201911327904A CN110919017B CN 110919017 B CN110919017 B CN 110919017B CN 201911327904 A CN201911327904 A CN 201911327904A CN 110919017 B CN110919017 B CN 110919017B
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wire
power supply
auxiliary power
pipeline
powder
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CN110919017A (en
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李辉
魏艺斌
曲浩然
林健
符寒光
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Beijing Yili Additive Technology Co ltd
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Beijing University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • B22F9/082Making 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 atomising using a fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • B22F9/082Making 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 atomising using a fluid
    • B22F2009/0824Making 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 atomising using a fluid with a specific atomising fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • B22F9/082Making 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 atomising using a fluid
    • B22F2009/0848Melting process before atomisation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

Abstract

The invention discloses a method and a device for preparing spherical metal powder. The method utilizes direct current plasma arc to heat, melt and atomize the metal wire, and applies an auxiliary power supply to the metal wire directly, the main power supply and the auxiliary power supply are insulated, the auxiliary power supply performs resistance heating on the wire, and the heating power required by melting and atomizing of the wire can be greatly reduced. The invention also discloses a device for preparing spherical metal powder by using the method, which comprises the following steps: a powder making pipeline; a power supply comprising a main power supply and an auxiliary power supply; the cathode of the spray gun is connected with the negative pole of the main power supply, and the front end of the anode is provided with a through hole; the insulating mechanism comprises an insulating gasket at the front end of the anode nozzle and an insulating ceramic wire guide nozzle at the front end of the wire feeding pipeline; the wire feeding device is arranged in the sealed bin and is provided with a wire feeding pipeline connected with the spray gun; a powder flight duct; and the powder collecting cylinder is arranged at the tail part of the powder flying pipeline.

Description

Method and device for preparing spherical metal powder by hot wire assisted plasma arc
Technical Field
The invention mainly relates to the fields of powder metallurgy technology, surface engineering and the like, in particular to the technical field of preparing spherical metal powder by a plasma hot wire spraying method.
Background
The spherical metal powder has wide application prospect in the fields of metallurgy, energy, electronics, medical treatment, aerospace and the like, and the fields have higher requirements on the physical properties of the powder, such as high sphericity, narrow particle size distribution, low impurity content, high purity and the like. The plasma arc has the advantages of simple operation, high temperature, easy parameter adjustment and the like, and the prepared powder has high sphericity and low impurity content, so the plasma arc has wide application prospect in atomizing metal spherical powder. At present, multi-electrode plasma arc, non-transferred arc and transferred arc are used in plasma arc atomization, which are the most important spherical metal powder preparation methods.
The patent US 5,259,433 adopts multi-electrode plasma arc to prepare spherical metal powder, a heating source of the multi-electrode plasma arc is composed of three plasma spray guns, raw material wires are atomized after being heated and melted intensively by the plasma arc, and the atomized particles are solidified into the spherical metal powder. Patent CN104475744A discloses a method for preparing spherical powder by adopting a non-transferred arc, wherein wire raw materials can be continuously supplied and continuously atomized under an inert gas environment, and the method has the defects that the distance from a nozzle to an atomization point of atomization airflow is too long, the energy and heat loss of plasma jet is large, the particle melting is not good, and the fine powder yield is low. The patent CN108637267A discloses a technology for preparing spherical powder by adopting a transferred arc method, the method is low in energy consumption and high in wire conversion efficiency, but due to the fact that the transferred arc is adopted, arc breaking is easy to occur when the flow of atomized gas is large, air flow after the wires are melted is difficult to effectively break a liquid film, and finally integral particles are coarse.
In summary, when the plasma arc is used for atomizing the wire material to obtain the spherical metal powder, the requirements of sufficient melting and sufficient atomization of the wire material are both met, which inevitably results in very large energy consumption, especially in order to obtain particles with smaller particle size, a high air flow velocity is needed to crush the melted wire material, and the stability of the plasma arc itself is difficult to guarantee, so the development of a method and a device with low energy consumption, low cost and high efficiency is urgently needed in the field to solve the above problems.
Disclosure of Invention
The invention discloses a method and a device for preparing spherical metal powder, which solve the problems of poor melting of atomized particles and poor sphericity caused by insufficient heating of wires and frequent occurrence of the traditional non-transferred plasma arc, and also improve the problem that the arc is easy to extinguish because of high air flow velocity in the original transferred arc method. The invention uses the additional auxiliary power supply to act on the cathode of the spray gun and the end part of the wire material, and uses the resistance heat of the auxiliary power supply as a second heat source to heat the wire material in advance, thereby greatly reducing the power required for melting the wire material during atomization and being beneficial to the formation of fine powder.
A method of preparing spherical metal powder, characterized by: the plasma torch comprises a cathode, an anode and an insulating connecting piece which are coaxial, wherein the cathode is connected with the negative pole of a power supply, the anode is connected with the positive pole of the power supply, and plasma gas is introduced from the insulating connecting piece; two poles of the auxiliary power supply are respectively applied to the wire and the cathode of the spray gun, the wire is connected with the anode of the auxiliary power supply, the cathode of the spray gun is connected with the cathode of the auxiliary power supply, the resistance heat of the auxiliary power supply is utilized to heat the wire in advance, and the temperature of the front end of the wire entering the plasma jet is ensured to be between 200 ℃ and 900 ℃.
The front end of the wire material utilizes a ceramic wire guide nozzle to ensure that an arc starting point generated by an auxiliary power supply is only at the foremost end of the atomized wire material, so that the melting and atomizing point of the wire material is kept stable.
In order to achieve the purpose, the invention provides a continuous powder making device, which mainly comprises the following main parts: the plasma spray gun comprises a cathode, an anode and an insulating connecting piece which are coaxial, wherein the center of the anode is provided with an electric arc compression duct and a through hole; the power supply comprises a main power supply for generating plasma jet and an auxiliary power supply for heating wire materials; the powder flying pipeline comprises a spray gun mounting base, a vacuum pipeline, a pipeline water cooling channel, a vacuum pump, a pressure release valve, a filter and a flowmeter, wherein the plasma spray gun is mounted on the base, and the vacuum pipeline is connected with the vacuum pump, the pressure release valve and the filter to ensure that atomized particles fly and are cooled in a vacuum environment or an inert atmosphere bin; the insulating part comprises an insulating gasket at the front end of the anode nozzle and an insulating ceramic wire guide nozzle at the front end, and ensures that the two power supplies do not interfere with each other during working; wire drive feed unit, including sending a machine, controller, sending a sealed storehouse, flexible silk pipe, ceramic silk guide mouth etc. send a machine to be arranged in the sealed storehouse, rotate through the motor and adjust a speed, send by sealed flexible silk pipe between wire drive feed unit and the spray gun base and link to each other, send one end of silk pipe and send a sealed storehouse to be connected, one end is connected with aforementioned ceramic silk guide mouth.
The invention also provides an operation step for preparing the spherical metal powder by adopting the preparation device, which comprises the following steps:
s1, wire feeding preparation: selecting raw material wires, placing the wires on a wire feeder in a wire feeding sealed bin, and enabling the wires to pass through a flexible wire feeding pipe and a ceramic wire guide nozzle to reach a position right below an anode nozzle.
S2, preparing an inert atmosphere: the whole pipeline is pumped by a vacuum pump, and the whole pipeline comprises a powder flying pipeline, a wire feeding sealed bin and a powder collecting cylinder. When the pipeline pressure reaches-0.1 Mpa, the vacuum pump is closed; introducing high-purity argon (99.99%) to make the pressure in the pipeline reach 0.1Mpa, and starting the vacuum pump again to vacuumize; repeating the above operations for three times;
s3: atomizing: simultaneously starting a power supply and an auxiliary power supply of the plasma spray gun, firstly adjusting parameters of the auxiliary power supply to ensure that the front end of the wire is heated to a red hot state by the auxiliary power supply, and then adjusting parameters of the plasma spray gun to perform spinning atomization;
s4: powder collection preparation: and after the atomization is finished, starting the vacuum pump again to exhaust the whole equipment, closing the vacuum pump when the pressure reaches-0.1 MPa, injecting high-purity argon to 0.1MPa, vacuumizing again, then opening the exhaust port, and collecting metal powder at the tail part after the air is filled in the equipment.
Further, in the step S2, the cathode of the plasma torch is connected to the negative electrode of the main power supply, and the anode is connected to the positive electrode of the main power supply. The anode of the auxiliary power supply is connected with the wire feeding pipe, and the cathode of the auxiliary power supply is connected with the cathode of the plasma spray gun.
Further, the diameter of the wire ranges from 0.8 to 3.2mm, preferably from 1.2 to 2.0mm;
further, the feeding speed of the wire is 1-300mm/s, and the preferable feeding speed is 10-100mm/s;
further, the distance between the front end of the wire and the plasma anode nozzle is 1-8mm, preferably 2mm;
further, the atomizing gas is Ar or N 2 He, and a mixed gas thereof, preferably 20% by weight 2 Ar + H of (A) 2 The mixed gas of (1).
Further, the process can be optimized according to the following formula to obtain spherical metal powder with different particle sizes:
Figure BDA0002328852930000031
in the above formula, d c Is the diameter (mm) of the outlet of the plasma anode nozzle, d w Is the diameter (mm) of the wire, Q is the plasma gas flow (m) 3 S) rho is gas density (kg/m) 3 ) P is the plasma power (kw), σ is the surface tension (N/m) of the wire as it melts, K 1 And K 2 Experimental constants associated with the anode nozzle and with the plasma gas, respectively, were determined experimentally.
Compared with the prior art, the embodiment of the invention has the following outstanding characteristics:
1. due to the heating of the auxiliary power supply, the wire is heated to a higher temperature before reaching the atomization point, and the wire is more easily heated and melted when the plasma jet with the same power is used, so that the energy consumption is reduced;
2. the traditional plasma jet atomization needs higher input power to ensure the temperature when using the atmospheric flow, so the fine powder yield is very low, the invention can obtain higher atomization airflow speed by using large airflow under the condition of ensuring the melting of wire materials, thus particles with smaller particle size are easy to produce, and the powder production efficiency is also improved.
3. The device has simple structure and large operation process window, can obtain the metal spherical powder with different particle size distributions by coordinating a plurality of parameters such as wire diameter, wire feeding speed, atomizing gas flow, main power supply power, auxiliary power supply power and the like, and is particularly suitable for preparing the spherical metal powder in small batch.
Drawings
One or more examples are illustrated by way of example in the accompanying drawings, which are not to be construed as limiting the embodiments.
FIG. 1 is an enlarged partial schematic view of the apparatus of the present invention;
FIG. 2 is a metal spherical powder prepared according to example 1 in the present invention;
FIG. 3 is a metal spherical powder prepared according to example 2 in the present invention;
FIG. 4 is a metal spherical powder prepared according to example 3 in the present invention;
FIG. 5 is a metal spherical powder prepared according to example 4 in the present invention;
Detailed Description
The following examples illustrate specific aspects of the present invention, but the present invention is by no means limited to the following examples.
Example 1
A disc of iron-based wire (17 Cr-13 Ni) with a diameter of 1.2mm was selected as a stock wire, and an anode nozzle with a diameter of 6.5mm was used. The wire is placed on a wire feeder in a wire feeding sealed bin, the wire sequentially passes through a flexible wire feeding pipeline and a ceramic wire guide nozzle to reach the center of the front end of the nozzle, the vertical distance from the wire to the nozzle is 2mm, and the feeding speed is set to be 50mm/s. Opening a vacuum pump to vacuumize the whole equipment, and closing the vacuum pump when the pressure reaches-0.1 Mpa; introducing argon into the device to enable the internal pressure to reach 0.1Mpa, then starting the vacuum pump again to extract vacuum, and repeating the operation for three times until the whole pipeline is in an argon atmosphere; plasma arc is used as a heat source, the parameters are adjusted to be current 400A, hydrogen gas 5L/min and argon gas 100L/min, after the electric arc is stabilized, the wire feeding speed is adjusted to be 70mm/s, then an auxiliary power supply is turned on to adjust the current to be 30A, and the wire is subjected to spinning atomization after being heated to a red hot state by the auxiliary power supply. The wire material is melted into metal droplets at the front end of the nozzle, and then is broken into a plurality of spherical droplets by the gas sprayed from the nozzle, the droplets enter a flight pipeline and are naturally cooled, and finally prepared metal powder is shown in figure 2, the shape of the powder is regular, the size is uniform, and the particle size is about 60-100 μm.
Example 2
Selecting an iron-based wire material (17 Cr-10 Ni) with the diameter of 1.4mm as a raw wire material, selecting a plasma anode nozzle with the outlet diameter of 7mm, placing the wire material on a wire feeder in a wire feeding sealed bin, enabling the wire material to sequentially pass through a wire feeding pipeline and a wire guiding pipe to reach the central position of the nozzle, enabling the vertical distance from a metal wire material to the nozzle to be 4mm, setting the feeding speed to be 70mm/s, starting a vacuum pump to vacuumize the whole equipment, and closing the vacuum pump when the pressure reaches-0.1 MPa; introducing argon into the device to enable the internal pressure to reach 0.1Mpa, then starting the vacuum pump again to extract vacuum, and repeating the operation for three times until the whole pipeline is in an argon atmosphere; and (3) utilizing a plasma arc as a heat source, adjusting parameters to be current 450A, hydrogen gas 6L/min and argon gas 80L/min, adjusting the wire feeding speed to be 80mm/s after the arc is stabilized, then turning on an auxiliary power supply to adjust the current to 28A, observing that the wire is heated to a red hot state by the auxiliary power supply, and then carrying out spinning atomization. As shown in FIG. 3, the particle size distribution of the finally prepared metal powder is about 100 μm.
Example 3
Selecting an iron-based wire (15 Cr-9 Ni) with the diameter of 1.6mm as a raw material wire, selecting a plasma anode nozzle with the diameter of an outlet of 7.5mm, placing the wire on a wire feeder in a wire feeding sealed bin, enabling the wire to sequentially pass through a wire feeding pipeline and a wire guiding pipe to reach the central position of the nozzle, enabling the vertical distance from the metal wire to the nozzle to be 5mm, setting the feeding speed to be 75mm/s, starting a vacuum pump to vacuumize the whole equipment, and closing the vacuum pump when the pressure reaches-0.1 Mpa; introducing argon into the device to enable the internal pressure to reach 0.1Mpa, then starting the vacuum pump again to extract vacuum, and repeating the operation for three times until the whole pipeline is in an argon atmosphere; and (3) utilizing a plasma arc as a heat source, adjusting parameters to 500A of current, 6.5L/min of hydrogen and 80L/min of argon, adjusting the wire feeding speed to 95mm/s after the arc is stabilized, then turning on an auxiliary power supply to adjust the current to 25A, observing that the wire is heated to a red hot state by the auxiliary power supply, and carrying out spinning atomization. As shown in FIG. 4, the particle size distribution of the finally prepared metal powder is about 100 μm.
Example 4
Selecting a disc of iron-based wire (10 Cr-10 Ni) with the diameter of 2.0mm as a raw material wire, selecting a plasma anode nozzle with the outlet diameter of 6mm, placing the wire on a wire feeder in a wire feeding sealed bin, enabling the wire to sequentially pass through a wire feeding pipeline and a wire guiding pipe to reach the central position of the nozzle, enabling the vertical distance from the metal wire to the nozzle to be 6mm, setting the feeding speed to be 70mm/s, starting a vacuum pump to vacuumize the whole equipment, and closing the vacuum pump when the pressure reaches-0.1 MPa; introducing argon into the device to enable the internal pressure to reach 0.1Mpa, then starting the vacuum pump again to extract vacuum, and repeating the operation for three times until the whole pipeline is in an argon atmosphere; and (3) utilizing a plasma arc as a heat source, adjusting parameters to be current 550A, hydrogen 7L/min and argon 90L/min, adjusting the wire feeding speed to be 100mm/s after the arc is stabilized, then turning on an auxiliary power supply to adjust the current to 20A, observing that the wire material is heated to a red hot state by the auxiliary power supply, and then carrying out spinning atomization. As shown in FIG. 5, the particle size distribution of the finally prepared metal powder is about 100 μm.

Claims (1)

1. A method of preparing spherical metal powder characterized by: the plasma torch comprises a cathode, an anode and an insulating connecting piece which are coaxial, wherein the cathode is connected with the negative pole of a power supply, the anode is connected with the positive pole of the power supply, and plasma gas is introduced from the insulating connecting piece; two poles of the auxiliary power supply are respectively applied to the wire and the cathode of the spray gun, the wire is connected with the anode of the auxiliary power supply, the cathode of the spray gun is connected with the cathode of the auxiliary power supply, the wire is heated in advance by using the resistance heat of the auxiliary power supply, and the temperature of the front end of the wire entering the plasma jet is ensured to be between 200 and 900 ℃; the specific operation steps are as follows: s1, wire feeding preparation: selecting raw material wires, placing the wires on a wire feeder in a wire feeding sealed bin, and enabling the wires to pass through a flexible wire feeding pipe and a ceramic wire guide nozzle to reach a position right below an anode nozzle; s2, preparing an inert atmosphere: pumping the whole pipeline by using a vacuum pump, wherein the whole pipeline comprises a powder flying pipeline, a wire feeding sealed bin and a powder collecting barrel; when the pipeline pressure reaches-0.1 Mpa, the vacuum pump is closed; introducing 99.99% high-purity argon to make the pressure in the pipeline reach 0.1Mpa, and then starting the vacuum pump again to vacuumize; repeating the above operations for three times; s3: atomizing: simultaneously starting a power supply and an auxiliary power supply of the plasma spray gun, firstly adjusting parameters of the auxiliary power supply to ensure that the front end of the wire is heated to a red hot state by the auxiliary power supply, and then adjusting parameters of the plasma spray gun to perform spinning atomization; s4: powder collection preparation: after atomization is completed, the vacuum pump is started again to extract air from the whole equipment, when the pressure reaches-0.1 MPa, the vacuum pump is closed, high-purity argon is injected to 0.1MPa, vacuumizing is performed again, then an exhaust port is opened, and metal powder is collected at the tail part after the inside of the equipment is filled with air;
the front end of the wire material ensures that the arcing point generated by the auxiliary power supply is only at the foremost end of the atomized wire material by using the ceramic wire guide nozzle, so that the melting and atomizing point of the wire material is kept stable; the feeding speed of the wire is 1-300mm/s; the distance between the front end of the wire and the plasma anode nozzle is 1-8mm;
the device used in the method comprises a main body: the plasma spray gun comprises a cathode, an anode and an insulating connecting piece which are coaxial, wherein the center of the anode is provided with an electric arc compression duct and a straight-through hole; the power supply comprises a main power supply for generating plasma jet and an auxiliary power supply for heating the wire; the powder flying pipeline comprises a spray gun mounting base, a vacuum pipeline, a pipeline water cooling channel, a vacuum pump, a pressure release valve, a filter and a flowmeter, wherein the plasma spray gun is mounted on the base, and the vacuum pipeline is connected with the vacuum pump, the pressure release valve and the filter to ensure that atomized particles fly and are cooled in a vacuum environment or an inert atmosphere bin; the insulating part comprises an insulating gasket at the front end of the anode nozzle and an insulating ceramic wire guide nozzle at the front end, and ensures that the two power supplies do not interfere with each other during working; wire feeding unit, including sending a machine, controller, sending a sealed storehouse, flexible silk pipe, pottery seal wire mouth, send a machine to be arranged in sealed storehouse, rotate through the motor and adjust a speed, send to link to each other by sealed flexible silk pipe between wire feeding unit and the spray gun base, send the one end of silk pipe and send a sealed storehouse to be connected, one end is connected with pottery seal wire mouth.
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