CN111545766A - Equipment and method for preparing high-purity spherical metal powder - Google Patents
Equipment and method for preparing high-purity spherical metal powder Download PDFInfo
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- CN111545766A CN111545766A CN202010579822.5A CN202010579822A CN111545766A CN 111545766 A CN111545766 A CN 111545766A CN 202010579822 A CN202010579822 A CN 202010579822A CN 111545766 A CN111545766 A CN 111545766A
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Classifications
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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
Abstract
The invention discloses equipment and a method for preparing high-purity spherical metal powder, wherein the equipment comprises an automatic powder feeding device, a reaction generation chamber connected with the automatic powder feeding device, and a radio frequency plasma generator connected with the reaction generation chamber, wherein the automatic powder feeding device is used for feeding raw material powder particles with irregular shapes into the reaction generation chamber, and the radio frequency plasma generator is used for heating and melting the raw material powder particles fed into the reaction generation chamber to form the high-purity spherical metal powder. The invention adopts the radio frequency plasma generator to heat and melt the raw material powder particles, and can prepare the spherical metal powder with high spheroidization rate, high purity, large density and relatively narrow particle size distribution by utilizing the advantages of high energy density, high heating strength, large volume of plasma moment and the like of the radio frequency plasma generator; the invention does not pollute the product due to electrode evaporation, and is beneficial to ensuring the high purity of the prepared spherical metal powder.
Description
Technical Field
The invention relates to the field of preparation of spherical metal powder, in particular to equipment and a method for preparing high-purity spherical metal powder.
Background
The core of metal 3D printing technology is material and device, and along with the development of metal 3D printing technology, the device is mature gradually, but the material that can be used for metal 3D to print at present is few in kind, the performance is unstable, and metal powder material for traditional metallurgy still can not be suitable for metal 3D printing technology completely. In addition, the metal powder for 3D printing is required to have high sphericity, low oxygen content and narrow particle size distribution, and is relatively poor in the aspects of metal powder material performance research, preparation technology data accumulation and the like in China. At present, most of materials used in the 3D printing rapid prototyping technology in China need to be imported from abroad, or equipment manufacturers invest great energy and cost for research and development, and the price is high, so that the production cost is increased. Therefore, the problems of good material performance and cost are solved, and the development of the rapid forming technology in China can be better promoted.
In the existing spherical metal powder processing process, two heating modes of crucible heating and electrode induction heating are generally adopted to melt metal, the melted metal is blown away and cooled under the action of airflow to produce corresponding powder, and then the powder is used in subsequent printing.
However, the existing spherical metal powder processing method has the problems of high energy consumption, low spheroidization rate, wide particle size distribution and low purity of the spherical metal powder caused by the fact that the spherical metal powder is easily polluted by electrode evaporation.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide equipment and a method for preparing high-purity spherical metal powder, and aims to solve the problems that the conventional spherical metal powder processing mode has high energy consumption, low spheroidization rate and wide particle size distribution, and the spherical metal powder is easy to be polluted by electrode evaporation, so that the purity of the spherical metal powder is low.
The technical scheme of the invention is as follows:
the equipment for preparing the high-purity spherical metal powder comprises an automatic powder feeding device, a reaction generating chamber connected with the automatic powder feeding device, and a radio frequency plasma generator connected with the reaction generating chamber, wherein the automatic powder feeding device is used for feeding raw material powder particles with irregular shapes into the reaction generating chamber, and the radio frequency plasma generator is used for heating and melting the raw material powder particles fed into the reaction generating chamber to form the high-purity spherical metal powder.
The equipment for preparing the high-purity spherical metal powder further comprises a control system electrically connected with the radio frequency plasma generator, and a radio frequency power supply electrically connected with the radio frequency plasma generator is arranged in the control system.
The equipment for preparing the high-purity spherical metal powder further comprises a gas holder which is respectively communicated with the radio frequency plasma generator and the automatic powder feeding device, and the gas holder is used for storing plasma reaction gas, protective gas and carrier gas.
The equipment for preparing the high-purity spherical metal powder also comprises a vacuum glove box powder collecting system communicated with the reaction generating chamber.
The equipment for preparing the high-purity spherical metal powder further comprises a cyclone dust removal device communicated with the vacuum glove box powder collecting system.
The equipment for preparing the high-purity spherical metal powder also comprises a dust removal and powder collection tank arranged at the bottom of the cyclone dust removal device.
The equipment for preparing the high-purity spherical metal powder also comprises a water ring type vacuum pump set communicated with the reaction generating chamber and the radio frequency plasma generator.
A method for preparing high-purity spherical metal powder based on the equipment comprises the following steps:
the automatic powder feeding device feeds the raw material powder particles into the reaction generating chamber;
starting a radio frequency plasma generator to heat and melt raw material powder particles sent into the reaction generating chamber to obtain spherical metal droplets, and solidifying the spherical metal droplets to form the high-purity spherical metal powder.
Has the advantages that: the invention provides equipment for preparing high-purity spherical metal powder, which comprises an automatic powder feeding device, a reaction generating chamber connected with the automatic powder feeding device, and a radio frequency plasma generator connected with the reaction generating chamber, wherein the automatic powder feeding device is used for feeding irregular-shaped raw material powder particles into the reaction generating chamber, and the radio frequency plasma generator is used for heating and melting the raw material powder particles fed into the reaction generating chamber to form the high-purity spherical metal powder. The invention adopts the radio frequency plasma generator to heat and melt the raw material powder particles, and can prepare the spherical metal powder with high nodulizing rate, high purity, large density and relatively narrow particle size distribution by utilizing the advantages of high energy density, high heating strength, large volume of plasma moment, simple process of processing materials and the like of the radio frequency plasma generator; the invention does not use electrodes, does not pollute products due to electrode evaporation, and is favorable for ensuring the high purity of the prepared spherical metal powder.
Drawings
FIG. 1 is a schematic structural diagram of a preferred embodiment of an apparatus for preparing high purity spherical metal powder according to the present invention.
FIG. 2 is a flow chart of a preferred embodiment of the method for preparing high purity spherical metal powder according to the present invention.
Detailed Description
The present invention provides an apparatus and a method for preparing high purity spherical metal powder, and the present invention is further described in detail below in order to make the objects, technical solutions, and effects of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, fig. 1 is a schematic view of an apparatus for preparing high-purity spherical metal powder according to the present invention, which includes an automatic powder feeding device 10, a reaction generating chamber 20 connected to the automatic powder feeding device 10, and a radio frequency plasma generator 30 connected to the reaction generating chamber 20, wherein the automatic powder feeding device 10 is configured to feed irregular-shaped raw material powder particles into the reaction generating chamber 20, and the radio frequency plasma generator 30 is configured to heat and melt the raw material powder particles fed into the reaction generating chamber 20 to form high-purity spherical metal powder.
In this embodiment, the raw material powder particles are heated and melted by the rf plasma generator to obtain molten particles, and the molten particles can form metal droplets with high spherical shape under the action of surface tension and rapidly solidify in a very short time, so as to form high-purity spherical metal powder.
In the embodiment, the radio frequency plasma generator is adopted to heat and melt raw material powder particles, and the spherical metal powder with high spheroidization rate, high purity, high density and relatively narrow particle size distribution can be prepared by utilizing the advantages of high energy density, high heating strength, large volume of plasma moment, simple material processing process and the like of the radio frequency plasma generator; the invention does not use electrodes, does not pollute products due to electrode evaporation, and is favorable for ensuring the high purity of the prepared spherical metal powder.
In some embodiments, the raw powder particles may be copper powder particles, titanium powder particles, molybdenum powder particles, or gold powder particles, but are not limited thereto. Taking molybdenum powder particles as an example, the equipment provided by the invention is used for preparing the molybdenum powder particles into high-purity spherical metal powder, the productivity of the high-purity spherical metal powder is more than or equal to 3kg/h, the spheroidization rate is more than or equal to 95%, and the granularity D50 is 20-35 mu m.
In some embodiments, the automatic powder feeding device 10 has an automatic feeding function, and can feed irregular-shaped raw material powder particles into the reaction generating chamber 20 under the protection of inert gas. In this embodiment, the particle size range of the raw material powder particles is 10 to 200 micrometers, the powder feeding rate of the automatic powder feeding device 10 is 1 to 40kg/h, and the automatic powder feeding device can continuously monitor and immediately regulate and control in the feeding process. Specifically, a feeding bin, a continuous feeding bin and a pneumatic feeding structure are arranged in the automatic feeding device 10, and for example, the volume of the feeding bin is 6L, and the volume of the feeding bin is 5L.
In some embodiments, the plasma is classified into two categories, i.e., a complete ionization plasma (e.g., a nuclear concentration degree) with ultrahigh temperature and ultrahigh energy density and a weak ionization plasma (e.g., an arc discharge plasma) with an ionization degree less than 1%, according to the difference of the ionization degree, and the weak ionization plasma is further classified into a balance plasma, i.e., a high temperature plasma and a non-balance plasma (e.g., a low temperature plasma), according to whether neutral particles, ions and electrons of the weak ionization plasma are in a thermal equilibrium state. The temperature of the high-temperature plasma is very high, about 4500 ℃ to tens of thousands of ℃, the heat capacity is very large, and the high-temperature plasma can be used for heating and melting materials; the low-temperature plasma is formed by ionizing working gas by a high-voltage electric field or filament electron emission and other methods under a vacuum condition, has a low temperature which is generally not more than 1000 ℃, has very small heat capacity, and is mainly used for surface treatment of materials.
In some embodiments, the rf plasma generator may be a plasma heating gun. The plasma heating gun comprises an electric arc plasma gun and a high-frequency plasma gun, and the principle of the plasma heating gun is as follows: an arc formed by arc discharge of a working gas is generated between a cathode (usually thoriated tungsten or cerium tungsten electrode) and a copper nozzle as an anode, and the arc plasma forms a small-diameter jet stream at a temperature of about 3000 ℃ and a gas flow rate of generally 10m/s or more and as high as 5000m/s due to the pressure of the working gas and the compression of a nozzle opening. The arc is not transferred to the heated material, so the arc is called a non-transfer arc type; if the arc generated between the electrode and the nozzle is transferred to the material connected with the anode of the power supply after being generated, the arc transfer type is called. The arc between the cathode and the material is strongly compressed due to the combined action of the mechanical compression effect (caused by the nozzle opening), the thermal contraction effect (because the center of the arc column is higher than the temperature of the periphery thereof, the ionization degree is high, the conductivity is large, the current naturally tends to the center of the arc column) and the magnetic compression effect (caused by the magnetic field of the arc column), and the arc column becomes slender (thin like a needle, and can also be as long as more than 1 m). Under the condition of keeping balance with the expansion pressure in the arc column, the gas at the center of the arc column is highly ionized, the temperature can reach 10000-52000 ℃, and the air flow speed can reach 10000 m/s. Transferred arc plasma guns are most widely used in plasma heating. In practice, sometimes the arc-sustaining arc between the cathode and the copper nozzle remains in addition to the arc-main arc between the cathode and the material.
The working gas is excited and ionized by the high-frequency induction coil and the capacitance electrode respectively, and the generated plasma can be sprayed out through the nozzle to form plasma flame and can also be left in the working area for heating materials. The high-frequency plasma has the advantages of no pollution caused by electrode materials, high production cost, low generator power and less consumption. The power supply of the arc plasma gun is generally a direct current power supply with the characteristic of steep drop, is positively connected, is also provided with a three-phase alternating current power supply, has no-load voltage which is generally within the range of 75-400V for machining and can be more than 3000V for smelting, and is generally a high-frequency electron tube oscillator with the frequency within the range of 0.4-75 MHz. The heating device varies with the application of the equipment, such as a plasma smelting furnace with a refractory lining or a furnace body of a water-cooled crystallizer; a workbench or a working trolley of the plasma cutting and spraying device.
In some embodiments, the maximum temperature generated by the rf plasma generator in this embodiment can reach 10000 degrees celsius, and the rf plasma generator is provided with a ceramic plasma confinement tube, which can provide high-purity processing capability; the ceramic plasma confinement tube is of a water cooling structure, and an induction coil which is embedded into the torch body and connected to a radio frequency power supply is arranged on the other side of the cooling channel; a gas distribution head upstream of the discharge chamber allows different gas flows to enter.
In some embodiments, as shown in fig. 1, the reaction generation chamber 20 is of a water-cooled double-wall stainless steel (ss304) structure, a vacuum glove box powder collecting system 40 is arranged at the bottom of the reaction generation chamber and communicated with the reaction generation chamber, the vacuum glove box powder collecting system 40 comprises a vacuum glove box and a plurality of powder collecting tanks arranged in the vacuum glove box, the powder collecting tanks are provided with airtight valves and water-cooled structures and are all located in the vacuum glove box, and the inert atmosphere protection can be performed to ensure that the heated and melted metal powder is not contacted with air all the way and ensure the purity of the metal powder.
In some embodiments, as shown in fig. 1, the apparatus for preparing high-purity spherical metal powder further comprises a cyclone dust collection device 50 communicated with the vacuum glove box powder collecting system 40, wherein the cyclone dust collection device 50 adopts a plurality of flexible composite material filter elements to collect powder and is provided with a gas purging device. The bottom of the cyclone dust removal device 50 is provided with a dust removal and powder collection tank 60, the dust removal and powder collection tank 60 is provided with an airtight valve and a water cooling structure, and the metal powder can be protected by inert atmosphere to ensure that the metal powder is not contacted with air in the whole process.
In some embodiments, as shown in fig. 1, the apparatus for preparing high-purity spherical metal powder further comprises a control system 70 electrically connected to the rf plasma generator 30, and an rf power source electrically connected to the rf plasma generator 30 is disposed in the control system 70. The control system 70 can control the output power of the radio frequency power supply, the output power of the radio frequency power supply is 15-80kw, 380V three-phase alternating current is input, 50Hz power can be continuously and stably output; the frequency of the radio frequency plasma generator is 2-3 MHz.
In some specific embodiments, as shown in meat 1, a touch display screen 71 electrically connected with the control system 70 is further arranged on the control system 70, the control system 70 comprises an industrial personal computer and a PLC, the industrial personal computer and the PLC can control equipment for preparing high-purity spherical metal powder, the control system 70 has two functions of automatic control and manual control, the operation process is completely realized on the touch display screen 71, and human-machine operation interfaces such as formula setting, a vacuum system, a process system, an inflation system, a cooling system and the like are provided; the setting of program technological process and equipment parameters can be realized on an industrial personal computer in a formula parameter setting mode. The industrial personal computer is provided with a plurality of serial port cards and is connected with various controllers in an RS232 or RS485 mode; the power control cabinet adopts international standards, the industrial personal computer and most of controllers are installed in an upper rack type, and the power control cabinet is connected with the host machine by a control cable, so that the reliability is high, and the maintenance is convenient; the high-voltage parts in the power control cabinet and the main machine are respectively provided with a protective cover, so that the safety of equipment is improved; the main electric appliance purchased parts in the electric control cabinet require the products of manufacturers passing CE certification or ISO9001 certification, so that safety and reliability are ensured.
In some embodiments, as shown in fig. 1, the apparatus for preparing high-purity spherical metal powder further comprises a gas holder 80 in communication with the rf plasma generator 30 and the automatic powder feeding device 10, respectively, wherein the gas holder 80 is used for storing a plasma reaction gas, a shielding gas and a carrier gas. The inside gas circuit system that is provided with of gas holder 80, gas holder 80 top is provided with air exit and hydrogen detector, the hydrogen detector can report to the police and warn the operator under the high condition of hydrogen concentration, be provided with parts such as mass flowmeter, manometer, pressure sensor, air-vent valve, stop valve, pipeline and joint in the gas circuit system. The plasma reaction gas may be argon, hydrogen, helium, nitrogen, oxygen or air, but is not limited thereto; the protective gas and the carrier gas can be argon, nitrogen or helium.
In some embodiments, as shown in fig. 1, the apparatus for preparing high purity spherical metal powder further comprises a water ring vacuum pump set 90 in communication with the reaction generating chamber 20 and the rf plasma generator 30. The water-ring vacuum pump set has a gas-liquid separator, a plate heat exchanger and a pressure control valve, and the working water temperature is 15 ℃, and the pre-vacuum degree is less than or equal to 20 kPa.
In some embodiments, the apparatus for preparing high-purity spherical metal powder further comprises a pressure control system, wherein the pressure control system forms closed-loop control through a vacuum pump, a controllable butterfly valve, a film gauge and a gas mass flow controller; the pressure control system is interlocked with the radio frequency plasma generator system, the operation atmosphere and pressure can freely select inert, reducing or oxidizing operation atmosphere, the pressure is controllable within the range of 150-.
In some embodiments, the equipment for preparing high-purity spherical metal powder further comprises a cooling system, wherein the cooling system is provided with a complete water cooling system pipeline and is provided with a flow safety locking device; the system is provided with a water temperature and flow monitoring and alarming system; the system is provided with a circulating water safety treatment system under the conditions of water cut-off and power failure, so that the equipment safety is ensured. The cooling system can provide necessary cooling for the plasma power supply, provide necessary cooling for the plasma torch and the powder feeding pipe, ensure the continuous use of the powder feeding pipe at high temperature, and provide necessary cooling for the reaction chamber, the cyclone dust removal powder collection tank and the like; the water-saving cooling water can also be used as emergency water to supplement circulating cooling water and used for supplementing deionized water through softening under the conditions of water cut and power cut, so that the safety of equipment is ensured.
In some embodiments, as shown in fig. 2, there is also provided a method for preparing high purity spherical metal powder based on the apparatus, comprising the steps of:
s10, feeding raw material powder particles into a reaction generating chamber by an automatic powder feeding device;
and S20, starting a radio frequency plasma generator to heat and melt the raw material powder particles fed into the reaction generating chamber to obtain spherical metal droplets, and solidifying the spherical metal droplets to form the high-purity spherical metal powder.
In this embodiment, the raw material powder particles are heated and melted by the rf plasma generator to obtain molten particles, and the molten particles can form metal droplets with high spherical shape under the action of surface tension and rapidly solidify in a very short time, so as to form high-purity spherical metal powder. In the embodiment, the radio frequency plasma generator is adopted to heat and melt raw material powder particles, and the spherical metal powder with high spheroidization rate, high purity, high density and relatively narrow particle size distribution can be prepared by utilizing the advantages of high energy density, high heating strength, large volume of plasma moment, simple material processing process and the like of the radio frequency plasma generator; the invention does not use electrodes, does not pollute products due to electrode evaporation, and is favorable for ensuring the high purity of the prepared spherical metal powder.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (8)
1. The equipment for preparing the high-purity spherical metal powder is characterized by comprising an automatic powder feeding device, a reaction generating chamber connected with the automatic powder feeding device, and a radio frequency plasma generator connected with the reaction generating chamber, wherein the automatic powder feeding device is used for feeding raw material powder particles with irregular shapes into the reaction generating chamber, and the radio frequency plasma generator is used for heating and melting the raw material powder particles fed into the reaction generating chamber to form the high-purity spherical metal powder.
2. The apparatus for preparing high purity spherical metal powder according to claim 1, further comprising a control system electrically connected to the radio frequency plasma generator, wherein a radio frequency power source electrically connected to the radio frequency plasma generator is disposed in the control system.
3. The apparatus for preparing high purity spherical metal powder according to claim 1, further comprising a gas holder in communication with the rf plasma generator and the automatic powder feeder, respectively, the gas holder being configured to store a plasma reaction gas, a shielding gas, and a carrier gas.
4. The apparatus for preparing high purity spherical metal powder according to claim 1, further comprising a vacuum glove box powder collection system in communication with the reaction generation chamber.
5. The apparatus for preparing high purity spherical metal powder according to claim 4, further comprising a cyclone dust removal device in communication with the vacuum glove box powder collection system.
6. The apparatus for preparing high purity spherical metal powder according to claim 5, further comprising a dust collection tank disposed at the bottom of the cyclone dust collector.
7. The apparatus for preparing high purity spherical metal powder according to claim 1, further comprising a water ring vacuum pump set in communication with the reaction generating chamber and the radio frequency plasma generator.
8. A method for producing a high-purity spherical metal powder based on the apparatus of any one of claims 1 to 7, comprising the steps of:
the automatic powder feeding device feeds the raw material powder particles into the reaction generating chamber;
starting a radio frequency plasma generator to heat and melt raw material powder particles sent into the reaction generating chamber to obtain spherical metal droplets, and solidifying the spherical metal droplets to form the high-purity spherical metal powder.
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| CN112947051A (en) * | 2020-12-23 | 2021-06-11 | 苏州汉霄等离子体科技有限公司 | Control method and device for radio frequency plasma powder making equipment, storage medium and electronic equipment |
| CN113231633A (en) * | 2021-04-06 | 2021-08-10 | 北京碳垣新材料科技有限公司 | Graphene copper-based composite powder and preparation method thereof |
| CN113244863A (en) * | 2021-04-06 | 2021-08-13 | 北京碳垣新材料科技有限公司 | Preparation equipment of composite material and use method thereof |
| CN113400533A (en) * | 2021-06-07 | 2021-09-17 | 河南能微新材料科技有限公司 | High-temperature dehydroxylation method |
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