CN114653322B - Device and process for preparing micro-nano powder - Google Patents
Device and process for preparing micro-nano powder Download PDFInfo
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- CN114653322B CN114653322B CN202210178302.2A CN202210178302A CN114653322B CN 114653322 B CN114653322 B CN 114653322B CN 202210178302 A CN202210178302 A CN 202210178302A CN 114653322 B CN114653322 B CN 114653322B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
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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 belongs to the field of micro-nano powder preparation, and in particular relates to a device and a process for preparing micro-nano powder based on a vacuum cold cathode arc target technology (metal target steam arc in a vacuum environment), an electromagnetic field constraint forming plasma beam technology and a high-speed uniform flow gas field technology. The device is a water-cooled vacuum device, and consists of a magnetic field arranged outside a vacuum chamber, an arc source cathode target material corresponding to the vacuum chamber, a high-speed uniform flow gas field arranged inside the vacuum chamber, an annular porous cooler and a powder collector, wherein a focused plasma beam moves to the opposite annular porous cooler, and meanwhile, the high-speed uniform flow gas field further cools and sweeps the ion beam in the annular porous cooler to the collector. The invention can realize the rapid preparation of uniform micro-nano powder, and is a new application of arc ion plating in the aspect of micro-nano powder preparation.
Description
Technical Field
The invention belongs to the field of micro-nano powder preparation, and in particular relates to a device and a process for preparing micro-nano powder based on a vacuum cold cathode arc target technology (metal target steam arc in a vacuum environment), an electromagnetic field constraint forming plasma beam technology and a high-speed uniform flow gas field technology.
Background
The nanometer material refers to a material with a microstructure such as crystal grains and grain boundaries reaching the level of nanometer scale. Along with nanocrystallization of the material, the electronic structure and the crystal structure of the material change, and surface effects and singular characteristics which are not possessed by macroscopic objects are generated, so that the material has a series of excellent electrical, magnetic, optical, mechanical, chemical and other characteristics, and is attractive. The nano powder material is a novel material with wide application prospect, and the preparation technology is key because the research and control of the preparation technology and the process have important influence on the microstructure and macroscopic performance of the nano powder. There are two general approaches to preparing nanopowders: firstly, crushing, namely gradually crushing coarse particulate matters through mechanical action, such as a mechanical ball milling method; the other is a granulation method, i.e. synthesis by two stages of nucleation and growth using atoms, ions or molecules. Such as spray drying method, sol-gel method, chemical precipitation method, vacuum evaporation condensation method, laser high temperature combustion method, etc., which have their own characteristics, and at the same time have certain limitations, because of the limitations of process conditions and production cost, most of the methods have the limitations of low yield, low purity of prepared products, difficult removal of contained impurities, high cost of raw materials, etc., and industrial mass production is difficult to realize, so that it is important to develop a preparation method with high yield, low cost and high quality.
The plasma method is a new technology for producing nano powder at present, because the arc plasma and jet flow thereof generated by medium discharge have the temperature of a molten pool as high as thousands of degrees and even tens of thousands of degrees, almost all materials can be melted, and the environment atmosphere of the medium discharge can be controlled conveniently. The plasma method can be used for preparing the simple substance nano material and the alloy type nano material. The equipment required by preparing the nano material by the plasma is simple, the operation is convenient, the yield is high, the application range is wide, and the plasma is successfully used for preparing simple substance metal nano powder, nitride, oxide, carbide powder and the like at present.
The chinese patent (publication No. CN2488622Y, apparatus for producing nano metal powder) provides an apparatus for producing nano material by using plasma, which mainly uses a plasma arc generated by discharging a high-frequency power supply as a heat source to vaporize and evaporate metal or alloy material, and then cooling and condensing the vaporized material by a collector, thereby generating nano powder, but the relative position between a plasma gun and a crucible of the apparatus cannot be adjusted, and the prepared metal powder has larger particles (-100 micrometers), and requires an additional feeder and an intermediate frequency induction coil, and the apparatus can only be used for preparing metal micrometer-sized powder. For this reason, chinese patent (publication No. CN2712505Y, apparatus for preparing nano metal powder by plasma) has improved this, and the disadvantages of the above apparatus are overcome. However, the plasma in these devices serves only as a heat source for evaporating the metal raw material contained in the crucible. In addition, it is necessary to provide additional accessories such as a moving cathode, etc., complicating the apparatus.
Recent chinese patent (publication No. CN102378461a, an annular uniform gas flow powder supply device) adopts a direct current arc plasma method to prepare nano powder. The direct current arc plasma method is a material preparation method in which a gas is ionized by arc discharge under an inert atmosphere or a reactive atmosphere to generate high temperature plasma, so that physical or chemical changes occur in a plasma enhanced atmosphere to generate vapor deposition. And (3) introducing the required reaction gas into the plasma reactor, so that the nano material of metal or various compounds can be formed after the gas is discharged. However, this method requires the provision of additional powder feeding means to melt the metal or alloy feedstock in the plasma zone and then cool it to form nano-powders. In the method, the particle size and uniformity of the powder are difficult to ensure because the ion beam current is not controlled after the melting. Moreover, the above-described plasma methods all require additional equipment such as a crucible, a powder supply device, etc. to supply raw materials of the powder.
The anode arc discharge plasma method is also a common method for preparing nano powder. The principle is that in a short time after the electric arc is ignited, the anode metal is heated, melted and evaporated to form steam, a large amount of granular soot collides with surrounding inert gas atoms and diffuses to the periphery to form metal nano powder. However, the greatest problem with this approach is that the anode loss is particularly high and it is very difficult to control and match the major process parameters such as gas pressure, arc current, arc voltage, gas species, electrode spacing, and cooling background.
Vacuum arc is the generation of a large number of arc spots on the surface of a cathode target in a vacuum chamber, the spot melt pool is locally high in temperature, so that cathode materials serving as targets are instantaneously evaporated and ionized, and a plasma beam with high ionization degree and high ion energy is generated, and the beam comprises electrons, metal ions, neutral atoms and molten liquid drops (namely large particles). If the arc plasma is constrained by an electromagnetic field, the arc column may be compressed to form a bunched arc plasma. Compared with the common electric arc, the temperature of the arc column of the bunched arc plasma is increased after constraint compression, the temperature gradient is increased, the energy density of the electric arc plasma is increased, the ionization rate is higher, the plasma ion beam is caused to be in a jet shape and separate from a high-temperature region of the electric arc to form supersaturated steam, and then the supersaturated steam is diffused under the action of high-speed uniform flow cooling gas and ion beam on the high-speed uniform flow gas field flow, so that nano particles are formed by nucleation and condensation growth and deposited on a collector. The growth mechanism of the nano particles mainly comprises adsorption growth and agglomeration growth. The size of the adsorption growth speed of the crystal nucleus is related to the surface area of the crystal nucleus and the vapor density, and the larger the crystal nucleus size is, the larger the vapor density is, the faster the growth speed of the crystal nucleus is; when the concentration of particles in the vapor reaches a certain degree and the density of the vapor is small, brownian collision occurs between crystal nuclei to perform coacervation growth, and the crystal nuclei can be quickly fused and grown once the collision occurs under the action of high-temperature environment temperature.
In the plasma generated by the conventional vacuum arc source, a large amount of large particles exist, for example, a metal cathode target is taken as an example, and the discharge mode is low voltage and high current, so that a plurality of highly bright cathode spots on the surface of the metal target move rapidly. The products of the cathode spot are electrons, metal ions, neutral atoms and molten droplets (i.e. large particles). The movement of the cathode spot determines the movement of the whole arc and is related to a plurality of key problems such as the stability of arc discharge, the effective utilization of cathode targets, the purification of large particles and the like. Because the motion of the arc spots has a great relation with the distribution of the magnetic field, an axial magnetic field consisting of a permanent magnet is usually applied to the rear part of the cathode target to restrict the motion of the arc spots and improve the arc discharge stability, but the effect is not obvious.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a device and a process for preparing micro-nano powder based on a vacuum cold cathode arc target technology (metal target steam arc under a vacuum environment), an electromagnetic field constraint forming plasma beam technology and a high-speed uniform flow gas field technology, wherein a plasma source is used as a raw material of the powder, the nucleation rate of nano particles is improved, and the micro-nano powder with uniform particles and small particle size is produced.
In order to achieve the above object, the technical scheme of the present invention is as follows:
the device is a vacuum device, and consists of a magnetic field arranged outside a vacuum chamber, an arc source cathode target material corresponding to the vacuum chamber, a high-speed uniform flow gas field arranged inside the vacuum chamber, an annular cooler and a collector, wherein the magnetic field is arranged outside the vacuum chamber: the magnetic fields are respectively positioned at the rear part of the arc source cathode target, the front part of the arc source cathode target, the outlet of the arc source cathode target for emitting plasma and the transmission channel of the plasma; the front part of the cathode target of the arc source corresponds to the annular cooler, the plasma beam after being focused by the magnetic field is opposite to the annular cooler, high-speed uniform flow gas fields are respectively arranged above and below the annular cooler, and the powder collector is arranged at the bottom of the vacuum chamber.
The magnetic field of the micro-nano powder preparation device is generated by the electromagnetic coil.
The electromagnetic coil is arranged outside the vacuum chamber, sleeved on the flange sleeve outside the cathode target of the arc source, protected by insulation between the electromagnetic coil and the flange sleeve, and coaxially arranged with the cathode target of the arc source, and the position of the electromagnetic coil is adjustable.
The high-speed uniform gas field of the micro-nano powder preparation device consists of a gas nozzle and gas sprayed out of the gas nozzle, wherein the gas is nitrogen or argon.
The annular cooler is formed by a double-layer hollow porous panel or a double-layer hollow porous panel with an annular fence frame and a notch, the notch is positioned at the periphery of the porous panel, and the annular fence frame is positioned at the annular hollow part of the porous panel.
The number of the cuts of the micro-nano powder preparation device is 4-12, and the inlet direction and the normal direction form an included angle of 30-60 degrees; the annular fence frame is composed of more than 20 rectangular fences with outwards radial uniform gap distribution around.
The device for preparing micro-nano powder is characterized in that a vacuum chamber wall cooling water pipe is arranged on the periphery of the whole vacuum device, and the powder collector is connected with the vacuum chamber body part through a rubber O-shaped ring for sealing.
A process for preparing micro-nano powder comprises the following steps:
(1) Vacuumizing until the vacuum degree in the vacuum chamber reaches (1-10) x 10 -3 In the case of Pa, the pressure of the gas,argon is introduced and the gas pressure of the vacuum chamber is maintained at 0.5Pa to 5.0Pa;
(2) The current of the restraining magnetic field coil is regulated to be 1.0-3.0A, and the corresponding magnetic induction intensity is 100-300 gauss;
(3) Opening a switch of the beam-forbidden magnetic field rotating device, and adjusting the current of a beam-forbidden magnetic field coil to be 2.0-3.0A, wherein the current corresponds to the magnetic induction intensity of 200-300 gauss; the method comprises the steps of carrying out a first treatment on the surface of the
(4) Adjusting the current of the beam-focusing magnetic field electromagnetic coil I to 3.0-5.0A, wherein the corresponding magnetic induction intensity is 300-500 gauss; adjusting the current of the beam-focusing magnetic field electromagnetic coil II to 5.0-7.0A, wherein the corresponding magnetic induction intensity is 500-700 gauss;
(5) Regulating the flow of argon to maintain the pressure of the vacuum chamber at 0.5-5.0 Pa; opening vacuum wall cooling water, introducing gas into a high-speed uniform gas field, wherein the flow rate of the high-speed uniform gas field I is 150-300 sccm, and the flow rate of the high-speed uniform gas field II is 50-150 sccm; after the flow is stable, starting arc discharge of an arc source cathode target material, wherein the arc flow is 50-100A, and after the normal work, starting preparation of the micron or nano particles;
the plasma ion beam after focusing by the beam focusing magnetic field moves to a right annular cooler, meanwhile, the ion beam is further cooled by the air flow generated by a group of high-speed uniform flow air fields at the other side of the annular cooler, and is blown to the vacuum chamber wall through cooling water by the air flow generated by another group of high-speed uniform flow air fields, and is deposited in a powder collector after being cooled by the cooling water of the vacuum chamber wall, so as to form nano or micron powder.
The air flow of the high-speed uniform air field is controlled by a mass flowmeter to change the cooling speed of cooling powder particles and the size of the powder particles, and the air flow of the high-speed uniform air field I is larger than the air flow of the high-speed uniform air field II; generating micro powder under the conditions that the flow rates of the high-speed uniform flow gas field I and the high-speed uniform flow gas field II are 100sccm and 150sccm respectively, wherein the particle size range of the micro powder is 10-100 micrometers; the flow rates of the high-speed uniform flow gas field I and the high-speed uniform flow gas field II are respectively 150sccm and 200sccm, so that nano powder is produced, and the particle size range of the nano powder is 10-500 nanometers.
The process for preparing the micro-nano powder adopts a pure metal target as an arc source cathode target: titanium target, zinc target, chromium target, magnesium target, niobium target, tin target, aluminum target, zirconium target, copper target, silver target, cobalt target, gold target, yttrium target, cerium target, or molybdenum target; alternatively, the arc source cathode target adopts a metal alloy target: titanium-aluminum alloy targets, chromium-aluminum alloy targets, MCrAlY alloy targets, or tungsten diboride alloy targets; thus, a metal, metal alloy, metal nitride, metal carbide, metal oxide or metal carbonitride micro-or nano-powder is prepared.
The technical principle of the invention is as follows:
the invention takes plasma beam generated by a controlled cold cathode target as raw material of powder, adopts a magnetic field composed of three electromagnetic coils arranged outside a vacuum chamber, and sequentially adopts a constraint magnetic field, a beam-forbidden magnetic field and a beam-converging magnetic field, so as to control the movement of arc spots on the surface of the cathode target, reduce the emission of large particles of the target, improve the discharge form and the working stability of the arc spots, focus the plasma beam and increase the density of the plasma beam. And the quenching speed is improved by using two groups of high-speed uniform gas fields, so that the problem of emission of large particles in an electric arc source is effectively reduced, the nucleation rate of nano particles can be improved, and the nano powder with uniform particles and small particle size is produced.
The invention adopts the annular cooler composed of double-layer hollow porous panels or double-layer hollow porous panels with annular fence frames and notches, the bunched plasma flow passes through the holes, the air flow generated by one group of high-speed uniform flow air fields is sprayed and cooled from the notches through the annular fences to form powder, and the powder is blown into the collector by the air flow generated by the other group of high-speed uniform flow air fields, so that not only the uniform powder discharge in all directions is ensured, but also the cooling speed is improved.
The high-speed uniform flow gas field adds an orientation speed to the nucleation particles in the whole growth area, promotes the particles to leave the high-temperature growth area rapidly, and inhibits the adsorption growth and agglomeration growth of the nucleation particles, so that the particle size is smaller, and the particle size distribution range is narrower.
The high-temperature gradient field generated by convection between the arc center of the bunched arc plasma and the external high-speed uniform cold air field is adopted, so that the metal vapor beam is very fast and easily diffused to a low-temperature area to form high-supersaturated vapor, and the nucleation rate is relatively high; the energy density of the bunching arc plasma is relatively high, so that the nucleation rate of the nano particles is improved, and the generated nano particles are uniform and have small particle size.
In order to reduce large particles, the area and the intensity of the transverse magnetic field component are expanded as much as possible, and the movement of the arc spots is limited. Therefore, the invention designs and uses a constraint magnetic field and a beam-forbidden magnetic field which are composed of electromagnetic coils on the cathode target of the arc source, and the constraint magnetic field acts on the rear part of the cathode target of the arc source so as to restrain the arc spot to move only on the surface of the cathode target; the beam-forbidden magnetic field acts on the front part of the cathode target of the arc source to occlude and control the movement of the arc spot on the surface of the cathode target, so as to reduce the emission of large particles of the target and improve the discharge form and the working stability of the arc spot. The design realizes the etching movement of the arc spot on the whole target surface, effectively improves the discharge form of the arc spot, restricts the ejection of large liquid drop particles, and solves the control problem of the sizes of the micro-nano powder from the source. Meanwhile, a set of two groups of beam-focusing magnetic fields formed by electromagnetic coils are arranged at the outlet of the arc plasma to form beam-focusing arc plasma, the supercooling degree of the plasma beam is improved by the air flow generated by the high-speed uniform air field, and nano particles with uniform particles and small particle size are formed under the combined action of cooling water arranged on the wall of the vacuum chamber.
Therefore, the invention is based on vacuum cold cathode arc target technology (metal target material vapor arc under vacuum environment) and adopts corresponding electromagnetic field constraint to form plasma beam technology, and uses high-speed uniform gas field to improve quenching speed (delta T), thus micro-nano powder with uniform and controllable grain size can be obtained. The invention provides a brand-new device and process for preparing a micro-nano material.
The invention has the advantages and positive effects that:
1. the invention provides a device and a process for preparing micro-nano powder based on a vacuum cold cathode arc target technology (metal target material vapor arc under a vacuum environment), an electromagnetic field constraint forming plasma beam technology and a high-speed uniform flow gas field technology. ) The device integrates three magnetic fields formed by electromagnetic coils, not only can effectively control the movement of arc spots in an arc source, but also can restrict the injection of large liquid drop particles, solves the problem of controlling the sizes of micro-nano powder from the source, greatly reduces the large particles in the arc source, and can prepare micro-nano powder with uniform particles and small particle size.
2. According to the device provided by the invention, three sets of magnetic fields are arranged outside the vacuum chamber, so that the electromagnetic coil is easy to cool, and particularly, the limitation of high temperature is avoided when the strength of the magnetic field is improved.
3. The device provided by the invention has the combined effect of the airflow of the high-speed uniform airflow field and the cooling water added to the vacuum chamber wall, and can realize rapid cooling of particles in plasma.
4. The device provided by the invention can control the air flow of the high-speed uniform air field through the mass flowmeter so as to change the cooling speed of the cooled powder particles and control the size of the powder particles.
5. The arc source cathode target material can adopt a pure metal target material: titanium target, zinc target, chromium target, magnesium target, niobium target, tin target, aluminum target, zirconium target, copper target, silver target, cobalt target, gold target, yttrium target, cerium target, or molybdenum target. Metal alloy targets may also be used: titanium-aluminum alloy targets, chromium-aluminum alloy targets, MCrAlY alloy targets, or tungsten diboride alloy targets. The target material can be used for preparing metal, metal alloy micro-nano powder, and micro-nano powder such as metal nitride, metal carbide, metal oxide or metal carbonitride can be prepared by selecting different reaction gases.
6. According to the device provided by the invention, the collector is connected and sealed with the vacuum cavity through the rubber O-shaped ring, so that the collector can be separated from the vacuum cavity to facilitate powder taking.
Drawings
FIG. 1 is a schematic view of the whole device structure of the present invention.
FIG. 2 is a schematic cross-sectional view of the annular cooler of the present invention. Wherein, (a) is an annular cooler consisting of double-layer hollow porous panels; (b) The figure shows an annular cooler consisting of double-layer hollow porous panels with annular fence frames and notches.
In the figure, 1 an arc source cathode target; 2 an arc source cathode target cooling water pipe; 3, an arc striking coil; 4, striking an arc needle; 5 restraining the magnetic field electromagnetic coil; 6, disabling the beam magnetic field electromagnetic coil; 7, disabling a cooling water pipe of the magnetic field electromagnetic coil; 8, a high-speed uniform flow gas field I;9, bunching a magnetic field electromagnetic coil I;10, a beam-focusing magnetic field electromagnetic coil II;11 bunching plasma; 12 high-speed uniform flow gas field II;13 an annular cooler; 14 vacuum chamber wall cooling water pipes; 15 a powder collector; a 16 vacuum chamber; 17 cuts; a porous panel 18; 19 fence frame.
Detailed Description
In the specific implementation process, the invention is based on a vacuum cold cathode arc target technology (metal target material vapor arc under a vacuum environment), an electromagnetic field constraint forming plasma beam technology and a high-speed uniform flow gas field technology to prepare micro-nano powder. The device is a vacuum device, and is composed of three sets of magnetic fields arranged outside a vacuum chamber, an arc source cathode target material corresponding to the vacuum chamber, two groups of high-speed uniform gas fields arranged inside the vacuum chamber, an annular cooler and a collector, wherein the three sets of magnetic fields are respectively a constraint magnetic field, a beam-forbidden magnetic field and a beam-focusing magnetic field, and the three sets of magnetic fields comprise: the restraining magnetic field acts on the rear part of the cathode target of the arc source to restrain the arc spot to move only on the surface of the cathode target; the beam-forbidden magnetic field acts on the front part of the cathode target of the arc source to restrict and control the movement of arc spots on the surface of the cathode target so as to restrict the ejection of large particles of the target, improve the discharge form and the working stability of the arc spots and generate plasma beams composed of particles with uniform micro-nano size; the beam focusing magnetic fields are divided into two groups and are respectively positioned at the outlet of the plasma emitted by the cathode target of the arc source and on the transmission channel of the plasma so as to focus the ion beam current of the plasma; the focused plasma ion beam moves to the opposite annular cooler, and meanwhile, the ion beam is further cooled by the air flow generated by one group of high-speed uniform flow air fields at the other side of the annular cooler, and is purged into the collector by the air flow generated by the other group of high-speed uniform flow air fields.
In the invention, the whole vacuum device is cooled by cooling water, and two groups of high-speed uniform flow air field cooling powder particles are arranged in the vacuum chamber.
In the invention, all three magnetic fields, such as a confining magnetic field, a beam-forbidden magnetic field, a beam-converging magnetic field and the like, are generated by electromagnetic coils.
In the invention, a beam-forbidden magnetic field electromagnetic coil is arranged outside a vacuum chamber, sleeved on a flange sleeve outside an arc source cathode target material, and protected with the flange sleeve through insulation; the flange sleeve is made of non-magnetic stainless steel, is of a hollow structure and is protected by cooling water; the beam-forbidden magnetic field electromagnetic coil, the flange sleeve and the arc source cathode target are coaxially arranged, and the position of the beam-forbidden magnetic field electromagnetic coil on the flange sleeve is adjustable.
In the invention, the high-speed uniform flow gas field consists of a gas nozzle and gas sprayed by the gas nozzle, wherein the gas is nitrogen or argon.
In the invention, the air flow of the high-speed uniform air field can be controlled by a mass flowmeter to change the cooling speed of the cooled powder particles and the size of the powder particles.
In the invention, the cathode target used in the device can be a pure metal target: titanium target, zinc target, chromium target, magnesium target, niobium target, tin target, aluminum target, zirconium target, copper target, silver target, cobalt target, gold target, yttrium target, cerium target, or molybdenum target. Or a metal alloy target can be adopted: titanium-aluminum alloy targets, chromium-aluminum alloy targets, MCrAlY alloy targets, and tungsten diboride alloy targets. Can be used for preparing metal, metal alloy, metal nitride, metal carbide, metal oxide and metal carbonitride micro-nano powder.
In the invention, the annular cooler is composed of double-layer hollow porous panels or double-layer hollow porous panels with annular fence frames and incisions.
In the invention, the number of the cuts is 4-12, and the inlet direction and the normal direction form an included angle of 30-60 degrees.
In the invention, the annular fence frame consists of more than 20 rectangular fences with outwards radial uniform gap distribution at the periphery.
In the invention, the collector and the vacuum cavity are connected and sealed through the rubber O-shaped ring, so that the collector and the vacuum cavity can be separated from the vacuum cavity to facilitate powder taking.
As shown in fig. 1, the device for preparing micro-nano powder comprises an arc source cathode target material 1, an arc source cathode target cooling water pipe 2, an arc striking coil 3, an arc striking needle 4, a restraint magnetic field electromagnetic coil 5, a beam-forbidden magnetic field electromagnetic coil 6, a beam-forbidden magnetic field electromagnetic coil cooling water pipe 7, a high-speed uniform gas field I8, a beam-focusing magnetic field electromagnetic coil I9, a beam-focusing magnetic field electromagnetic coil II10, a beam-focusing plasma 11, a high-speed uniform gas field II12, an annular cooler 13, a vacuum chamber wall cooling water pipe 14, a powder collector 15, a vacuum chamber 16 and the like, and has the following specific structures:
the invention is provided with a vacuum chamber 16, a vacuum chamber wall cooling water pipe 14 is arranged outside the vacuum chamber 16, a powder collector 15 is arranged at the bottom of the vacuum chamber 16, and the powder collector 15 and the vacuum chamber body are connected and sealed through a rubber O-shaped ring, so that the powder can be separated from the vacuum chamber body to be convenient to take. The middle lower part of the vacuum chamber 16 is a semi-hollow structure, wherein an arc source cathode target 1, a restraint magnetic field electromagnetic coil 5, a beam-forbidden magnetic field electromagnetic coil 6, a beam-forbidden magnetic field electromagnetic coil I9 and a beam-forbidden magnetic field electromagnetic coil II10 are arranged in the semi-hollow structure, the arc source cathode target 1, the restraint magnetic field electromagnetic coil 5, the beam-forbidden magnetic field electromagnetic coil 6, the beam-forbidden magnetic field electromagnetic coil I9 and the beam-forbidden magnetic field electromagnetic coil II10 are all positioned outside the vacuum chamber 16, and the middle upper part of the vacuum chamber 16 is provided with a high-speed uniform gas field II12. The invention is provided with an arc source cathode target 1, a constraint magnetic field electromagnetic coil 5 is arranged at the rear part of the arc source cathode target 1, and an arc source cathode target cooling water pipe 2 used for the arc source cathode target 1 comprises a water inlet pipe and a water outlet pipe and is used for cooling the target. The invention is provided with an arc striking coil 3 and an arc striking needle 4 connected with the arc striking coil 3, wherein the front end of an arc source cathode target 1 is provided with the arc striking needle 4, and the arc striking needle 4 is connected with the arc striking coil 3 and is used for striking an arc on the surface of the arc source cathode target. The beam-forbidden magnetic field electromagnetic coil 6 is sleeved on a flange sleeve outside the cathode target of the arc source and is protected with the flange sleeve through insulation. The beam-forbidden magnetic field electromagnetic coil cooling water pipe 7 used by the beam-forbidden magnetic field electromagnetic coil 6 comprises a water inlet pipe and a water outlet pipe and is used for cooling the beam-forbidden magnetic field electromagnetic coil. A beam-focusing magnetic field electromagnetic coil I9 is arranged at a plasma outlet emitted by the arc source cathode target material 1, and a beam-focusing magnetic field electromagnetic coil II10 is arranged at a plasma transmission channel where the plasma enters the vacuum chamber.
The beam-forbidden magnetic field electromagnetic coil generates a beam-forbidden magnetic field and is used for confining and controlling the movement of arc spots on the surface of the cathode target material so as to reduce the emission of large particles of the target material and improve the discharge form and the working stability of the arc spots. After the beam-forbidden magnetic field acts, the plasma emitted by the cathode target 1 of the arc source is constrained into beam-focused plasma 11 by a beam-focused magnetic field electromagnetic coil I9 arranged at the outlet and a beam-focused magnetic field generated by a beam-focused magnetic field electromagnetic coil II10 arranged on the plasma transmission channel, so that the density of the beam-focused plasma is increased.
The annular cooler 13 is located at the middle upper part in the vacuum chamber 16 and between the bunched plasma 11 and the high-speed uniform gas field II12, the lower part of the annular cooler 13 corresponds to the bunched plasma 11, and the upper part of the annular cooler 13 corresponds to the high-speed uniform gas field II12.
As shown in FIG. 2, the annular cooler 13 is composed of two layers of hollow porous panels 18 (FIG. 2 a) which are arranged in parallel up and down, the average pore diameter of the porous panels 18 is 0.5-1 mm, the thickness of the porous panels 18 is 1-2 mm, and the distribution density of through holes on the porous panels 18 is 1.27X10 6 ～5.09×10 6 Individual/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Alternatively, the annular cooler 13 is composed of a double-layer hollow perforated panel 18 with annular fence frames 19 and cut-outs 17 arranged in parallel up and down (fig. 2 b), the cut-outs 17 are located at the periphery of the perforated panel 18, and the annular fence frames 19 are located at the annular hollow portions of the perforated panel 18.
In the embodiment, the number of the cuts is 8, and the inlet direction forms an included angle of 45 degrees with the normal direction. The annular fence frame 19 is composed of 20 rectangular fences with outwards radial uniform gap distribution around.
As shown in fig. 1 and 2b, the bunched plasma 11 is sprayed to an annular cooler 13 consisting of a double-layer hollow annular fence frame 19 and a porous panel 18 with a notch 17, and after passing through the porous panel 18 in the annular cooler, the bunched plasma is blown by a high-speed uniform gas field II12 to the notch 17 through the fence frame 19 for cooling, and is blown out of the annular cooler along the tangential direction to form micro-or nano-powder, so that the powder material has enough time to be uniformly distributed in all directions. Meanwhile, the powder discharged from the high-speed uniform gas field I8 is blown to the vacuum chamber wall through cooling water, and is deposited in the powder collector 15 after being cooled by the vacuum chamber wall cooling water pipe 14 to form micro-powder or nano-powder, wherein the air flow of the high-speed uniform gas field I8 is larger than that of the high-speed uniform gas field II12, the flow of the high-speed uniform gas field I8 is 150-300 sccm, and the flow of the high-speed uniform gas field II12 is 50-150 sccm.
The invention is further illustrated by the following examples.
Example 1
In this embodiment, the preparation process of the nano powder is as follows:
firstly, vacuumizing until the vacuum degree in the vacuum chamber reaches 6 multiplied by 10 -3 During Pa, argon is introduced and the gas pressure of the vacuum chamber is maintained at 1.0Pa; adjusting the current of the restraining magnetic field coil to be 2.0A, wherein the corresponding magnetic induction intensity is 200 gauss; opening a switch of the beam-forbidden magnetic field rotating device, and adjusting the current of the beam-focusing magnetic field electromagnetic coil I to 4.0A, wherein the current corresponds to the magnetic induction intensity of 400 Gauss; adjusting the current of the beam-focusing magnetic field electromagnetic coil II to 6.0A, wherein the corresponding magnetic induction intensity is 600 Gauss; then, the flow rate of argon gas was adjusted so that the pressure in the vacuum chamber was maintained at 0.5Pa. And (3) opening vacuum wall cooling water, and introducing gas into the high-speed uniform gas field, wherein the flow rates of the high-speed uniform gas field I8 and the high-speed uniform gas field II12 are respectively 150sccm and 200sccm. After the flow is stable, starting arc discharge of an arc source cathode target material, wherein the arc flow is 60A, and starting the preparation of the nano particles after the normal work. The powder discharged from the high-speed uniform flow air field I8 is blown to the vacuum chamber wall through which cooling water is introduced, and is deposited in the powder collector 15 after being cooled by the vacuum chamber wall cooling water pipe 14 to form nano powder.
In the embodiment, the target material is a titanium target, and the granularity of the nano powder is 10-500 nanometers. The air flow through the high-speed uniform air field can be controlled by a mass flowmeter to change the cooling speed of the cooled powder particles and control the size of the powder particles.
Example 2
In this embodiment, the preparation process of the micro powder is as follows:
firstly, vacuumizing until the vacuum degree in the vacuum chamber reaches 1 multiplied by 10 -2 During Pa, argon is introduced and the gas pressure of the vacuum chamber is maintained at 2.0Pa; adjusting the current of the restraining magnetic field coil to be 1.0A, wherein the corresponding magnetic induction intensity is 100 gauss; opening a switch of the beam-forbidden magnetic field rotating device; electromagnetic coil for adjusting beam-focusing magnetic fieldI current is 2.0A, and the corresponding magnetic induction intensity is 200 Gauss; adjusting the current of the beam-focusing magnetic field electromagnetic coil II to 3.0A, wherein the corresponding magnetic induction intensity is 300 Gauss; then, the flow rate of argon gas was adjusted so that the pressure in the vacuum chamber was maintained at 1.0Pa. And (3) opening vacuum wall cooling water, and introducing gas into the high-speed uniform gas field, wherein the flow rates of the high-speed uniform gas field I8 and the high-speed uniform gas field II12 are respectively 100sccm and 150sccm. And after the flow is stable, starting arc discharge of an arc source cathode target material, wherein the arc flow is 50A, and after the normal work, starting preparation of the micron particles. The powder discharged from the high-speed uniform flow air field I8 is blown to the vacuum chamber wall through which cooling water is introduced, and is deposited in the powder collector 15 after being cooled by the vacuum chamber wall cooling water pipe 14 to form micro powder.
In this embodiment, the target is a titanium target, and the particle size of the micro powder is 10-100 microns. The air flow through the high-speed uniform air field can be controlled by a mass flowmeter to change the cooling speed of the cooled powder particles and control the size of the powder particles.
The example results show that the invention can realize the rapid preparation of uniform micro-nano powder, and is a new application of arc ion plating in the aspect of micro-nano powder preparation.
Claims (8)
1. The device is characterized by being a vacuum device, and consists of a magnetic field arranged outside a vacuum chamber, an arc source cathode target material corresponding to the vacuum chamber, a high-speed uniform flow gas field arranged inside the vacuum chamber, an annular cooler and a collector, wherein the magnetic field is arranged outside the vacuum chamber: the magnetic fields are respectively positioned at the rear part of the arc source cathode target, the front part of the arc source cathode target, the outlet of the arc source cathode target for emitting plasma and the transmission channel of the plasma; the front part of the cathode target of the arc source corresponds to the annular cooler, the plasma beam after being focused by the magnetic field is opposite to the annular cooler, high-speed uniform flow gas fields are respectively arranged above and below the annular cooler, and the powder collector is arranged at the bottom of the vacuum chamber;
the annular cooler is formed by a double-layer hollow porous panel with an annular fence frame and a notch, the notch is positioned at the periphery of the porous panel, and the annular fence frame is positioned at the annular hollow part of the porous panel;
the number of the cuts is 4-12, and the inlet direction and the normal direction form an included angle of 30-60 degrees; the annular fence frame is composed of more than 20 rectangular fences with outwards radial uniform gap distribution around.
2. The apparatus for preparing micro-nano powder according to claim 1, wherein the magnetic field is entirely generated by an electromagnetic coil.
3. The micro-nano powder preparation device according to claim 2, wherein the electromagnetic coil is arranged outside the vacuum chamber, sleeved on the flange sleeve outside the arc source cathode target, protected by insulation between the electromagnetic coil and the flange sleeve, and coaxially arranged with the arc source cathode target, and the position of the electromagnetic coil is adjustable.
4. The apparatus for preparing micro-nano powder according to claim 1, wherein the high-speed uniform gas field is composed of a gas nozzle and a gas sprayed from the gas nozzle, and the gas is nitrogen or argon.
5. The device for preparing micro-nano powder according to claim 1, wherein a cooling water pipe of a vacuum chamber wall is arranged on the periphery of the whole vacuum device, and the powder collector is connected and sealed with the vacuum chamber body through a rubber O-shaped ring.
6. A process for preparing micro-nano powder by using the device of claim 1, which is characterized by comprising the following steps:
(1) Vacuumizing until the vacuum degree in the vacuum chamber reaches (1-10) x 10 -3 During Pa, argon is introduced and the gas pressure of the vacuum chamber is maintained at 0.5-5.0 Pa;
(2) The current of the restraining magnetic field coil is regulated to be 1.0-3.0A, and the corresponding magnetic induction intensity is 100-300 gauss;
(3) Opening a switch of the beam-forbidden magnetic field rotating device, and adjusting the current of a beam-forbidden magnetic field coil to be 2.0-3.0A, wherein the current corresponds to the magnetic induction intensity of 200-300 gauss;
(4) Adjusting the current of the beam-focusing magnetic field electromagnetic coil I to 3.0-5.0A, wherein the corresponding magnetic induction intensity is 300-500 gauss; adjusting the current of the beam-focusing magnetic field electromagnetic coil II to 5.0-7.0A, wherein the corresponding magnetic induction intensity is 500-700 gauss;
(5) Regulating the flow of argon to maintain the pressure of the vacuum chamber at 0.5-5.0 Pa; opening vacuum wall cooling water, introducing gas into a high-speed uniform gas field, wherein the flow rate of the high-speed uniform gas field I is 150-300 sccm, and the flow rate of the high-speed uniform gas field II is 50-150 sccm; after the flow is stable, starting arc discharge of an arc source cathode target material, wherein the arc flow is 50-100A, and after the normal work, starting preparation of the micron or nano particles;
the plasma ion beam after focusing by the beam focusing magnetic field moves to a right annular cooler, meanwhile, the ion beam is further cooled by the air flow generated by a group of high-speed uniform flow air fields at the other side of the annular cooler, and is blown to the vacuum chamber wall through cooling water by the air flow generated by another group of high-speed uniform flow air fields, and is deposited in a powder collector after being cooled by the cooling water of the vacuum chamber wall, so as to form nano or micron powder.
7. The process for preparing micro-nano powder according to claim 6, wherein the air flow of the high-speed uniform air field is controlled by a mass flowmeter to change the cooling speed of the cooled powder particles and the size of the powder particles, and the air flow of the high-speed uniform air field is larger than the air flow of the high-speed uniform air field II; generating micro powder under the conditions that the flow rates of the high-speed uniform flow gas field I and the high-speed uniform flow gas field II are 100sccm and 150sccm respectively, wherein the particle size range of the micro powder is 10-100 micrometers; the flow rates of the high-speed uniform flow gas field I and the high-speed uniform flow gas field II are respectively 150sccm and 200sccm, so that nano powder is produced, and the particle size range of the nano powder is 10-500 nanometers.
8. The process for preparing micro-nano powder according to claim 6, wherein the arc source cathode target is a pure metal target: titanium target, zinc target, chromium target, magnesium target, niobium target, tin target, aluminum target, zirconium target, copper target, silver target, cobalt target, gold target, yttrium target, cerium target, or molybdenum target; alternatively, the arc source cathode target adopts a metal alloy target: titanium-aluminum alloy targets, chromium-aluminum alloy targets, MCrAlY alloy targets, or tungsten diboride alloy targets; thus, a metal, metal alloy, metal nitride, metal carbide, metal oxide or metal carbonitride micro-or nano-powder is prepared.
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