KR20200032500A - Method for manufacturing nanopowder using thermal plasma - Google Patents

Abstract

The present invention relates to a method for continuously preparing nanopowders using transfer-type thermal plasma, which comprises: a raw material supply step of supplying raw materials into a crucible; a vaporization step of vaporizing the raw materials received in the crucible by using a plasma electrode; a nanopowder forming step of forming nanopowder by collecting and transferring the raw materials, vaporized in the vaporization step, through a transfer film, which is provided on an upper portion of the crucible and moves along an endless circulation loop; and a packaging step of packaging the nanopowder formed in the nanopowder forming step in a packaging container. The raw material supply step, the vaporization step, the nanopowder forming step and the packaging step are performed in a vacuum state. In addition, the height of the crucible is adjusted or the crucible is rotated to control the amount of evaporation and production, and the distance between the crucible and the transfer film is adjusted to adjust a particle size. The method for continuously manufacturing the nanopowders proceeding as the steps above can easily produce high-quality nanopowder with a uniform particle size in mass and continuously, and can easily produce nanopowder with various properties and compositions.

Description

Method for continuous production of nano powders using a transfer-type thermal plasma {METHOD FOR MANUFACTURING NANOPOWDER USING THERMAL PLASMA}

The present invention relates to a method for continuously manufacturing nano powders using a transfer thermal plasma, and more specifically, it is possible to mass-produce nano powders using a transfer thermal plasma in a vacuum environment, and continuously supplying raw materials, manufacturing nano powders, and the like. The present invention relates to a method for continuously manufacturing nanopowder using a transferable thermal plasma that can be collected.

In general, nano-powder refers to a material having a dimension of less than 100 nm. Nano-powder technology is driving revolutionary changes in all industries including materials, electricity, electronics, bio, chemical, environment, and energy by enabling control and manipulation at the atomic and molecular level of materials.

As a method of manufacturing such a nano powder, there are a wet method or a mechanical grinding method, but in the case of the wet method, there is a problem in that the process is complicated, productivity is low, and harmful substances are discharged to the environment, and the mechanical grinding method produces nano powders of a certain size or less. Have a hard time.

Recently, a method of manufacturing a nano powder using plasma has been disclosed. In the production of nano powders using thermal plasma, when raw material particles are introduced into an ultra-high temperature thermal plasma having a heat source of about 10000 ℃, the vaporized atoms are nucleated into nanoparticles by being completely vaporized and cooled again. Use principles.

The manufacturing method of the nano powder using thermal plasma can be divided into a transported type and a non-transferred type depending on the structure of the torch. In the case of the non-transfer type, all electrodes are mounted inside the torch to generate arcs at the electrodes inside the torch, and the arcs are blown out by the carrier gas from the rear. In the case of the transfer type, the anode and the anode are spaced apart at regular intervals, and the distance between them is adjusted to adjust the arc length.

Republic of Korea Patent Registration No. 10-0788412 discloses an apparatus for manufacturing a nano-powder using thermal plasma. The registered patent includes a power supply unit 110, a plasma torch unit 120, a reaction chamber 130, a vacuum pump 140, a cooling tube 150, a collection unit 160, a scrubber 170, and reaction A structure in which a sample evaporated by plasma in a chamber passes through a cooling tube, crystallizes into nano-powder and is collected in a collection part is disclosed.

However, when the above structure is used, it is difficult to continuously supply raw materials, and after the cooling tube, the nano-powder is collected through a separate collecting device, so the collection process of the nano-powder is complicated and difficult to continuously collect.

In addition, there is a problem that there is a limitation in controlling the amount of evaporation in the above structure or synthesizing different kinds of raw materials in the gas phase.

(Document 0001) Republic of Korea Patent Registration No. 10-0788412 (Registration date: 2007.12.17.) (Document 0002) Republic of Korea Patent Registration No. 10-1055991 (Registration date: 2011.08.04.)

An object of the present invention invented in view of the above points is to provide a method for continuously producing nanopowders for efficiently producing and packaging nanopowders having a uniform particle size, which is easy to mass-produce and continuously produce nanopowders.

In addition, it is to provide a method for continuously manufacturing nano powders in which the evaporation amount of the raw material is easily controlled, different raw materials can be synthesized in the gas phase, and the particle size and production amount are easily controlled.

A method for continuously manufacturing nanopowder using a transfer-type thermal plasma according to an embodiment of the present invention includes a raw material supply step of supplying raw materials into a crucible, and a vaporization step of vaporizing raw materials contained in the crucible using plasma electrodes. , Nano-powder forming step of forming the nano-powder by continuously collecting and transporting the raw material vaporized in the vaporization step on the upper part of the crucible through the transfer film moving along the endless circulation loop, and the nano-powder formed in the nano-powder forming step It includes a packaging step for packaging the packaging container, the raw material supply step, vaporization step, nano-powder forming step and the packaging step is carried out in a vacuum.

In addition, it may include a particle size control process for adjusting the distance between the crucible and the transfer film and a production amount control process for adjusting the distance between the crucible and the plasma electrode.

In addition, the vaporization step may further include an evaporation amount control process of rotating the crucible so that the amount of evaporation of the raw material supplied to the crucible is adjusted.

In addition, the raw material supplying step may supply raw materials of different materials to the crucible.

In addition, the vaporization step may further include an atmospheric gas supply process for supplying atmospheric gas to the vaporized raw material.

In addition, the atmosphere gas supply process can be supplied using a flow controller between the crucible and the transfer film.

In addition, the vaporization step may further include a coating layer forming process of forming a coating layer on the surface of the raw material vaporized in the vaporization step by supplying a coating gas between the crucible and the transfer film.

In addition, the nano-powder forming step may include a cooling water circulation process for circulating cooling water on both sides of the transport film and a surface temperature control process for cooling the surface of the transport film using a cooling plate.

In addition, in the packaging step, the nano-powder can be vacuum packed in a predetermined amount in a packaging container using a load cell.

In addition, the raw material supply step, the vaporization step and the nano-powder forming step may be continuously performed for a predetermined time.

According to one embodiment of the present invention, it is easy to mass-produce and continuously produce nanopowder using various raw materials, and collect the vaporized raw material from the transport film and crystallize it into nanopowder, thereby producing and packaging the nanopowder. Can be shortened.

In addition, it is easy to control the particle size of the nano-powder through the particle size control process, and the production amount of the nano-powder can be easily controlled through the volume control process. The composition ratio of the powder can be adjusted, and the surface coating layer of the nanopowder can be formed through the coating layer forming process.

In addition, the structure in which the nano powder is generated, captured, and packaged in a vacuum state can be prevented from surface oxidation due to atmospheric exposure, thereby minimizing the oxygen content of the nano powder.

1 is a flowchart illustrating a method for continuously manufacturing nanopowders using a transfer-type thermal plasma according to an embodiment of the present invention.
2 and 3 are flow charts showing different vaporization steps according to an embodiment of the present invention.
Figure 4 is a flow chart showing the nano-powder forming step according to an embodiment of the present invention
5 is a block diagram showing a continuous production apparatus for nanopowders that can be used in a method for continuously producing nanopowders according to an embodiment of the present invention.
6 and 7 are perspective views illustrating an apparatus for continuously manufacturing nanopowder according to an embodiment of the present invention.
8 is a side cross-sectional view showing an apparatus for continuously manufacturing nanopowder according to an embodiment of the present invention.
9 is a side view showing an automatic feeding device of the nano powder continuous production apparatus according to an embodiment of the present invention.
10 is a detailed view showing the structure of a crucible according to an embodiment of the present invention.
11 is an exemplary view showing modularization using four nanopowder continuous manufacturing apparatuses according to an embodiment of the present invention.

In the description of the present invention, when it is determined that detailed descriptions of related known functions or configurations may unnecessarily obscure the subject matter of the present invention, detailed descriptions thereof will be omitted.

The embodiments according to the concept of the present invention may be modified in various ways and have various forms, and thus, specific embodiments will be illustrated in the drawings and described in detail in the present specification or application. However, this is not intended to limit the embodiment according to the concept of the present invention to a specific disclosure form, and it should be understood that it includes all modifications, equivalents, or substitutes included in the spirit and scope of the present invention.

The terms used in this specification are only used to describe specific embodiments, and are not intended to limit the present invention. Singular expressions include plural expressions unless the context clearly indicates otherwise. In this specification, the "inclusive" or "gajida" and the terms are staking the features, numbers, steps, operations, elements, parts or geotyiji to be a combination thereof specify the presence, of one or more other features, integers It should be understood that it does not preclude the existence or addition possibilities of, steps, actions, components, parts or combinations thereof.

Hereinafter, the present invention will be described in detail.

1 is a flowchart illustrating a method for continuously manufacturing nanopowders using a transfer-type thermal plasma according to an embodiment of the present invention.

Referring to FIG. 1, a method for continuously manufacturing nanopowders using a transfer-type thermal plasma according to an embodiment of the present invention includes a raw material supply step (S100) for supplying raw material into the crucible 110, the crucible 110 A vaporization step (S200) of vaporizing the raw material contained in the inside of the plasma using the plasma electrode 160, the raw material vaporized in the vaporization step (S200) is provided on the upper portion of the crucible 110 and along an infinite circulation loop Nano-powder forming step (S300) to form nano powder by collecting and transporting through the moving transport film 180, the packaging step of packaging the nano-powder formed in the nano-powder forming step (S300) in a packaging container 340 ( S400), the raw material supply step (S100), vaporization step (S200), nano-powder forming step (S300) and packaging step (S400) proceeds in a vacuum.

In the present invention, the supply of raw materials, the generation of nano-powder, the collection of nano-powder, the packaging of the nano-powder can be carried out continuously as a single mechanism. That is, the raw material supply step (S100), vaporization step (S200) and nano-powder forming step (S300) can be continuously performed for a set time to produce a large amount of nano-powders in large quantities, continuously, and can be automated.

Specifically, in the present invention, after the raw material is melted and evaporated by a transfer thermal plasma method using a crucible 110 and a plasma electrode 160, nano-powder is formed through nucleation and condensation. The crucible 110 The plasma electrode 160 may be provided inside the reaction chamber 100, which is an enclosed space, and the raw material supply step (S100), vaporization step (S200), nano powder formation step (S300), and packaging step ( S400) may be continuously and sequentially performed in one device. In addition, the transfer film 180 used in the present invention is provided inside the reaction chamber 100 and moves along an endless circulation loop, wherein the transfer film 180 is the crucible 110 at the top of the crucible 110. ), The raw material evaporated from the crucible 110 is condensed in the gas phase and has a particle size of a certain size, moves upward, and is collected and transported on the surface of the transfer film 180 as it is spaced apart from the crucible 110. It has a structure that is continuously generated.

The raw material supply step (S100) of the present invention is a step of supplying the raw material that is the base material of the nano-powder to the interior of the crucible 110, the raw material may utilize various materials such as silicon waste.

In the raw material supply step (S100), raw materials of different materials may be supplied to the crucible 110. In this case, the crucible 110 has a plurality of divided internal spaces, and different materials may be accommodated in the plurality of internal spaces.

2 and 3 is a flow chart showing a vaporization step (S200) according to an embodiment of the present invention.

2 and 3, the vaporization step (S200) of the present invention means a step of vaporizing the raw material supplied to the interior of the crucible 110 in the raw material supply step (S100). In the evaporation step (S200), the raw material is melted and evaporated using plasma using the plasma electrode 160, and the evaporated raw material moves to the upper portion while generating nucleation and condensation.

In one embodiment of the present invention, the evaporation step (S200), the particle size control process (S210) for controlling the distance between the crucible 110 and the transfer film 180, the crucible 110 and the plasma electrode ( 160) may include a production control process (S220) for adjusting the distance between.

The particle size of the nano-powder may vary depending on the use, the particle size control process (S210) of the present invention to adjust the particle size of the nano-powder by adjusting the distance between the crucible 110 and the transfer film 180. Specifically, the particle size control process (S210) can adjust the distance between the crucible 110 and the transfer film 180 by varying the height of the crucible 110. When the height of the crucible 110 is increased to closely locate the distance between the crucible 110 and the transfer film 180, the particle size of the nano-powder becomes small and the height of the crucible 110 is lowered to transport the crucible 110 and When the distance between the films 180 is positioned farther, the particle size of the nanopowder is increased.

In addition, in the present invention, the production control process (S220) by adjusting the distance between the crucible 110 and the plasma electrode 160 to control the evaporation amount of the raw material contained in the crucible 110, the production of nano-powder Can be adjusted. For example, when the height of the plasma electrode 160 is adjusted or the height of the crucible 110 is adjusted, when the distance between the plasma electrode and the crucible 110 approaches, the amount of evaporation of the raw material increases, thereby increasing the production of nanopowder. When the amount increases, the amount of evaporation of the raw material decreases when the distance increases, the production amount of the nanopowder can be reduced. In addition, the plasma electric output can be stabilized through the production amount control process (S220), and the phenomenon that plasma is extinguished is prevented to produce stable nanopowders.

In one embodiment of the present invention, the vaporization step (S200) may further include an evaporation amount control process (S230) for rotating the crucible 110 so that the amount of evaporation of the raw material supplied to the crucible 110 is adjusted. . The plasma electrode 160 is generally provided at a predetermined position with a tip. In the evaporation amount control process (S230) of the present invention, the position of the crucible 110 is rotated, so that the raw material contained in the crucible 110 is rotated. Even evaporation can be achieved, and the amount of evaporation can be varied according to the internal position of the crucible 110.

When a plurality of the raw materials are formed of different materials, different materials accommodated inside the crucible 110 as the relative positions of the tip 161 and the crucible 110 are controlled using the evaporation amount control process (S230). Each of the raw materials of the evaporation amount can be adjusted. Specifically, the plasma electrode 160 may have a plurality of tips 161, and the plurality of tips 161 are positioned while being spaced apart from each other by a predetermined distance from the top of the crucible 110. In this case, as the crucible 110 is rotated, the amount of evaporation by position of the crucible can be adjusted, and when raw materials of different materials are accommodated, the amount of evaporation can be set differently for each raw material. The nanomaterials produced by the method for continuously manufacturing nanopowders according to the present invention using such a method may have different compositions of materials, and it is easily performed to adjust the composition ratio of the compositions through the evaporation amount control process (S230). You can. In particular, there is an advantage that it is easy to manufacture the alloy nano powder by controlling the evaporation amount of each of a plurality of powder materials.

In one embodiment of the present invention, the vaporization step (S200), may further include an atmosphere gas supply process (S240) for supplying an atmosphere gas to the vaporized raw material, the atmosphere in the atmosphere gas supply process (S240) The supply of gas may be supplied using a flow controller between the crucible 110 and the transfer film 180. Here, if the mass flow control (MFC) is capable of supplying a gas having a set capacity, its structure or type is not limited.

In the present invention, the atmospheric gas supply process (S240) is to produce nano powders having specific properties such as oxide, carbide, and nitride, and simply inject an inert gas to exclude the influence of external air or generate plasma. The purpose is different. That is, the atmosphere gas of the present invention means to modify the material, properties, composition ratio, etc. of the nano powder. For example, the atmosphere gas is a metal (M) and oxygen (O) -based gas (M + O ₂ , MCl + O ₂ , M (NO ₃ ) _X + O _2, etc.) or metal (M) and nitrogen (N) based gas (M + (NH ₃ / N ₂ ), MCl + (NH ₃ / N ₂ + H ₂ ), M0 _X + (N ₂ + C / N ₂ + H ₂ ), MH _X + NH _3, etc. ), Metal (M) and carbon (C) based gases (M + (CH ₄ / CH ₄ + H ₂ ), MCl + (CH ₄ + H ₂ ), M0 _X + (CH ₄ + H ₂ ), MH _X + CH _4, etc.) or metal (M) and boron (B) based gases (M + B ₂ O ₃ + (CH ₄ ), MCl + BCl ₃ + H ₂ + CxHy, etc.) may be used. . Here, the metal (M) means the raw material, and the metal (M) may be excluded from the atmosphere gas.

In addition, in one embodiment of the present invention, the vaporization step (S200), by supplying a coating gas between the crucible 110 and the transfer film 180 to the surface of the raw material vaporized in the vaporization step (S200) A coating layer forming process (S250) of forming a coating layer may be further included. The coating gas may be controlled through a mass flow control (MFC).

In the coating layer forming process (S250), a functional nanopowder is prepared by supplying a coating gas to a set position inside the reaction chamber 100 to make a nanopowder formed with a coating layer through a coating material contained in the coating gas. It is to do. In the coating layer forming process (S250), it is preferable that the coating gas is supplied between the crucible 110 and the transfer film 180 to induce a coating layer to be formed only on the surface of the nanopowder.

The coating gas is a metal (M) and oxygen (O) based gas (M + O ₂ , MCl + O ₂ , M (NO ₃ ) _X + O _2, etc.) or metal (M) and nitrogen (N) based Gas (M + (NH ₃ / N ₂ ), MCl + (NH ₃ / N ₂ + H ₂ ), M0 _X + (N ₂ + C / N ₂ + H ₂ ), MH _X + NH _3, etc.), metal Gases based on (M) and carbon (C) (M + (CH ₄ / CH ₄ + H ₂ ), MCl + (CH ₄ + H ₂ ), M0 _X + (CH ₄ + H ₂ ), MH _X + CH ₄ Etc.) or metal (M) and boron (B) based gases (M + B ₂ O ₃ + (CH ₄ ), MCl + BCl ₃ + H ₂ + CxHy, etc.) can be used. Here, the metal (M) means the raw material, and the metal (M) may be excluded from the atmosphere gas.

The coating gas supplied from the coating layer forming process (S250) is preferably supplied into the reaction chamber 100 at a higher position than the atmosphere gas supplied from the atmospheric gas supply process (S240).

There is an advantage in that it is possible to easily form nano powders having various materials or properties according to the purpose of use by using the atmospheric gas supply process (S240) or the coating layer forming process (S250).

Figure 4 is a flow chart showing the nano-powder forming step (S300) according to an embodiment of the present invention

Referring to FIG. 4, the nano-powder forming step (S300) of the present invention captures raw materials and / or nano-powders (hereinafter referred to as nano-powders) having a certain size while being vaporized and condensed in the vaporization step (S200). In the step of transferring, the nano-powder is transported at the same time as capture through the transfer film 180.

The transfer film 180 extends in the longitudinal direction and moves repeatedly and continuously in one direction along the infinite trajectory of the endless circulation loop forming a closed curve. The moving direction of the transfer film 180 may be moved in the direction of the collecting unit 300 in which the nano powder is collected in the reaction chamber 100.

In one embodiment of the present invention, the nano-powder forming step (S300), the cooling water circulation process (S310) for circulating the cooling water on both sides of the transfer film 180 and the surface of the transfer film 180 is a cooling plate ( 182) may be used to cool the surface temperature control process (S320). Specifically, the cooling water circulation process (S310) means a step of flowing cooling water inside the transport shaft 181 provided on both sides of the transport film 180, and the surface temperature control process (S320) is the transport film Refers to a process of adjusting the surface of the transfer film 180 to a set temperature by attaching a cooling plate 182 to the surface of 180.

It is preferable that the cooling plate 182 is provided inside the endless circulation loop of the transfer film 180 in the surface temperature control process (S320) so that the collection and transfer of the nano powder are smooth on the bottom surface of the transfer film 180. Do. The transport film 180 is protected through the cooling water circulation process (S310) as described above, and the surface of the transport film 180 is cooled to the temperature set through the surface temperature control process (S320), so that the collection of nano powders can be more smoothly performed. have.

The packaging step (S400) of the present invention refers to a step of packaging the nano-powder transferred to the collection unit 300 in a predetermined amount in a packaging container 340. Specifically, the nano-powder transferred to the collection unit 300 in the nano-powder forming step (S300) falls downward by gravity, and then packs the dropped nano-powder in a vacuum while measuring the weight by a load cell. Method is applied. In the packaging step (S400), the dropped nano powder is vacuum-loaded by a load lock valve, a gate valve, or a screw conveyor that moves the nano powder to a predetermined position while maintaining a vacuum according to the rotation of a screw wound in a spiral. It can be moved in the direction of the packaging container 340.

As described above, in the present invention, since the supply of the raw material in the vacuum state, the generation, collection, transport, and packaging of the nano-powder are continuously performed, it is possible to generate a large amount of nano-powder and ensure the production of a homogeneous nano-powder. have. In addition, raw materials of different materials can be synthesized in the gas phase, and it is easy to control the particle size and production amount of the nano powder.

Hereinafter, a continuous production apparatus for a nanopowder using a transfer-type thermal plasma used in the continuous production method for a nanopowder of the present invention will be described.

5 is a block diagram showing a continuous nano-powder manufacturing apparatus usable in the method for continuously producing nano-powders according to an embodiment of the present invention, and FIGS. 6 and 7 are the nano-powder continuous production apparatus according to an embodiment of the present invention 8 is a side cross-sectional view showing the apparatus for continuously manufacturing the nanopowder according to an embodiment of the present invention.

5 to 8, the nano-powder continuous manufacturing apparatus using a transfer-type thermal plasma according to an embodiment of the present invention uses a plasma electrode 160 and a crucible 110 to react a reaction chamber to vaporize raw materials (100), connected to one side of the reaction chamber 100, the raw material supply unit 200 for supplying the raw material to the reaction chamber 100, the vaporized raw material in the upper inside of the reaction chamber 100 or A collecting film for collecting and transporting the crystallized nano-powder and connected to the other side of the transfer film 180 moving along the closed loop, the other side of the reaction chamber 100, and a collecting unit for recovering the nano-powder transferred through the transfer film 180 ( 300).

Briefly explaining the structure of the nanopowder continuous manufacturing apparatus of the present invention, the plasma electrode 160, the crucible 110, the transfer film 180 is provided inside the reaction chamber 100, on one side of the reaction chamber 100 A raw material supply unit 200 through which raw materials are supplied is provided, and a collection unit 300 through which nanomaterials are collected is provided on the other side. A support frame positioned at a predetermined height while supporting the reaction chamber 100 may be provided below the reaction chamber 100, and the support frame may include the reaction chamber 100 as well as the collection part 300 or Each of the raw material supply units 200 may be supported at a set height. The raw material supplied from the raw material supply unit 200 is vaporized and condensed inside the reaction chamber 100 to change into a nano powder, and the changed nano powder is collected by the collection unit 300.

The reaction chamber 100 has a closed structure, and one side is provided with a material supply port 101 connected to the raw material supply unit 200, and a vacuum port 102 connected to a vacuum pump P, etc. It is connected to communicate with the rejection (300). The reaction chamber 100, the collecting unit 300 and the raw material supply unit 200 is preferably maintained in a vacuum state.

9 is a side view showing an automatic feeding device of the nano powder continuous production apparatus according to an embodiment of the present invention.

Referring to FIG. 9, the raw material supply unit 200 of the present invention may include an automatic feeding device 210 that supplies raw material into the reaction chamber 100. Through the automatic feeding device 210, the raw material supply step (S100) may be performed in the above-described method for continuously manufacturing the nanopowder.

The automatic feeding device 210 includes a feeding housing 211, a feeding screw 212 provided in a spiral shape inside the feeding housing 211, and a feeding motor 215 and the feeding housing for driving the feeding screw 212 It is connected to (211) and includes a feeding nozzle 214 for supplying the raw material into the reaction chamber 100, and the inside of the feeding housing 211 is rotated in the vacuum in the feeding screw 212 By this, the raw material can be moved by an extrusion method.

The feeding housing 211 has a closed structure in a cylindrical shape in the present invention and maintains a vacuum state therein. The feeding nozzle 214 may be connected to one side of the feeding housing 211 and the feeding motor 215 may be connected to the other side. In addition, the feeding housing 211 may be connected to one side of the reaction chamber 100 so that the feeding nozzle 214 smoothly supplies raw materials to the crucible 110 provided inside the reaction chamber 100. .

The feeding housing 211 is provided with an opening / closing opening 213 through which raw materials are supplied, and the opening / closing opening 213 preferably uses a load-lock type valve to minimize the influence on the internal vacuum environment of the feeding housing 211. Do. The raw material introduced through the opening and closing opening 213 is moved in the direction of the feeding nozzle 214 by rotation of the feeding screw 212. The feeding nozzle 214 may continuously supply the raw material to the crucible 110 provided inside the reaction chamber 100.

In addition, a feeding heater 216 may be connected to the outside of the feeding housing 211 so that a raw material accommodated inside the feeding housing 211 has a set temperature, and the feeding heater 216 may be provided in plural. have.

One side of the feeding housing 211 is coupled to the material supply port 101, in which case the feeding nozzle 214 connected to the feeding housing 211 is located inside the reaction chamber 100. The feeding nozzle 214 may have various shapes and structures, and the feeding nozzle 214 may be a plurality.

A crucible 110 and a plasma electrode 160 are provided inside the reaction chamber 100 of the present invention. The crucible 110 and the plasma electrode 160 are arranged to be separated from each other by a predetermined distance, and the plasma generated from the plasma electrode 160 generates an arc in the direction of the crucible 110. Through the crucible 110 and the plasma electrode 160, the vaporization step (S200) of the above-described nanopowder continuous manufacturing method may be performed.

10 is a detailed view showing the structure of the crucible 110 according to an embodiment of the present invention. 10 (a) and 10 (b) show the detailed structure of the crucible 110, and FIG. 10 (c) shows the plasma electrode 160 and the automatic feeding device 210 arranged in the crucible.

Referring to FIG. 10, the crucible 110 is connected to the crucible electrode 120 and can withstand a high temperature atmosphere and may be made of graphite so that current can pass through it. The crucible electrode 120 is connected to the lower center of the crucible 110 and cooling water may be separately introduced and discharged from the crucible electrode 120.

10, in one embodiment of the present invention, the crucible 110 may have a double structure.

The crucible 110 has a first track 111 of a shape settled in the downward direction, a second track 112 having a shape of an inner circumference larger than the outer circumference of the first track 111 and settled in the downward direction. And a blocking jaw 113 provided between the first track 111 and the second track 112 and blocking the first track 111 and the second track 112. Raw materials supplied from the automatic feeding device 210 may be accommodated in the first track 111 and the second track 112, respectively, in accordance with the first track 111 and the second track 112. The plasma electrode 160 may be a plurality. For example, the plasma electrode 160 may include two plasma electrodes 160 on the first track 111 and four plasma electrodes 160 on the second track 112. The number and position of the plasma electrode 160 may be determined in consideration of the circumference of the first track 111 or the second track 112.

The first track 111 and the second track 112 may be supplied with raw materials of the same material or raw materials of different materials. In this case, the automatic feeding device 210 is plural and supplies the raw material to the first track 111 and the second track 112, respectively. That is, the feeding nozzle 214 supplies raw materials of the same material or different materials to the first track 111 and the second track 112, respectively.

The crucible 110 of the present invention having a double structure as described above is the amount or rate of evaporation due to the difference in the position and temperature of the first track 111 and the second track 112 when the raw material of the same material is supplied It can be adjusted effectively. In addition, when raw materials of different materials are supplied, the different raw materials can be synthesized in the gas phase, thereby making it easier to manufacture the composite nano powder.

In one embodiment of the present invention, a crucible height adjusting means 140 for adjusting the height of the crucible 110 or a crucible rotating means 150 for rotating the crucible 110 may be provided.

As shown in FIG. 8, the crucible 110 is provided with a crucible center shaft 130 formed to extend vertically while being connected to the crucible 110 while passing through the reaction chamber 100. ) Further includes a first gear 151 provided along the circumference of the crucible center axis 130 and a second gear 152 engaged with the first gear 151 to rotate the crucible center axis 130. can do. In this case, the second gear 152 is connected to the motor and can be rotated according to the operation of the motor. Specifically, the crucible center shaft 130 is located inside the support frame, the first gear 151 is fixedly coupled to the lower portion of the crucible center shaft 130, and the second gear 152 is The first gear 151 may be connected to the motor in an engaged state. According to the operation of the motor, the second gear 152 rotates clockwise or counterclockwise around a vertical line, and the first gear 151 is rotated by the rotation of the second gear 152. Rotate 110) clockwise or counterclockwise. The motor may be a hydraulic motor driven by hydraulic pressure, and the first gear 151 and the second gear 152 may have a structure such as a spur gear, a worm gear, or a bevel gear.

In the present invention having the above structure, it is possible to control the temperature of the raw material accommodated in the crucible 110 by rotating the crucible 110 connected to the crucible center shaft 130, and accordingly the evaporation rate of the raw material or The amount of evaporation can be adjusted. For example, the raw material accommodated in the crucible 110 may have a different temperature or evaporation amount depending on the location. In the present invention, even rotation of the crucible 110 enables the evaporation of evenly selected raw material and the crucible 110. The evaporation rate or the amount of evaporation is controlled by adjusting the relative positions of the raw material and plasma electrode 160 accommodated in the interior to a distance or close.

In addition, in the present invention, the crucible height adjustment means 140 is coupled to the support frame and connected to the crucible 110 while passing through the reaction chamber 100, and the crucible according to the driving of a ball screw ( 110). For example, although the crucible height adjusting means 140 is not shown in the drawing of the present invention, the first screw shaft 143 (not shown), which extends in the vertical direction and is spirally wound, and the first screw shaft 143 A first screw motor 144 (not shown) for rotating the first screw nut 145 fastened to the first screw shaft 143 and reciprocating up and down according to the rotation of the first screw shaft 143 ( (Not shown), the first ball nut 145 is fixed to the crucible center shaft 130 and the crucible center shaft 130 and the crucible by vertical reciprocating motion of the first ball nut 145 110) may have a structure that reciprocates up and down. In this case, both sides of the first ball nut 145 may be separately connected to the support frame to prevent horizontal departure due to reciprocating motion. The shape of the first ball nut 145 may be varied, and the first screw shaft 143 may be plural.

The present invention provided with the crucible height adjustment means 140 is easy to adjust the height of the crucible 110, it is easy to adjust the amount of evaporation of the raw material according to the arc length or plasma temperature.

The plasma electrode 160 of the present invention is provided at a predetermined distance from the crucible 110 and forms a hot cathode. A tip 161 made of tungsten may be fastened to an end of the plasma electrode 160, and coolant may be separately introduced and discharged at the bottom. In addition, the plasma electrode 160 may be provided with a connection terminal 163 (not shown) connected to a power source on one side of the electrode center shaft 162 formed in the vertical direction and the electrode center shaft 162. In this case, the cooling water may be introduced into the electrode center shaft 162.

In the present invention, an electrode height adjusting means 170 for adjusting the height of the plasma electrode 160 may be further included. Specifically, the electrode height adjusting means 170 is coupled to the support frame, connected to the plasma electrode 160, and can adjust the height of the plasma electrode 160 according to the driving of a ball screw. When the electrode center shaft 162 penetrates the interior of the reaction chamber 100 and is connected to the plasma electrode 160, the electrode height adjusting means 170 adjusts the height of the electrode center shaft 162. The height of the plasma electrode 160 can be adjusted.

For example, the electrode height adjusting means 170 is coupled to the support frame and is formed to extend in the vertical direction and rotates according to the operation of the second screw motor 172, the second screw shaft 171, the second screw It is fastened to the shaft 171 and includes a second ball nut 173 reciprocating up and down according to the rotation of the second screw shaft 171, the second ball nut 173 and the electrode center shaft 162 The plasma electrodes 160 connected to the electrode center shaft 162 may be moved up and down according to the reciprocating motion of the second ball nut 173 connected to each other. The structures of the second screw shaft 171, the second screw motor 172, and the second ball nut 173 are the aforementioned first screw shaft 143, the first screw motor 172, and the second ball nut ( 145).

In the present invention having the above configuration, the height of the plasma electrode 160 is controlled to control the length of the arc generated in the plasma electrode 160 or the evaporation rate or evaporation rate of the raw material.

The rotation of the crucible 110, the height adjustment of the crucible 110 or the height adjustment of the plasma electrode 160 may be changed to have various configurations or structures within the scope of the present invention.

The plasma electrodes 160 may be plural, and the plural plasma electrodes 160 may be arranged at regular intervals according to the shape of the crucible. For example, when the crucible has the above-described dual structure, two plasma electrodes 160 are disposed on the first track 111 and four on the second track 112, and a plurality of plasma electrodes 160 are provided. By simultaneously applying, it is possible to maximize the production of nano powder.

In addition, the structure in which the nano powder is generated, captured, and packaged in a vacuum state can be prevented from surface oxidation due to atmospheric exposure, thereby minimizing the oxygen content of the nano powder.

The transport film 180 of the present invention collects and transports the vaporized raw material through the plasma electrode 160 and the crucible 110, the transport film 180 is provided to be spaced apart from the crucible 110 by a certain distance And some or all of the transfer film 180 is provided on the upper portion of the reaction chamber (100). Through the transfer film 180, the nano-powder forming step (S300) of the above-described method for continuously manufacturing the nano-powder may be performed.

The transfer film 180 is formed of a metal and may collect the vaporized raw material on the surface of the transfer film 180 by electrical or magnetic properties.

The transfer film 180 moves along the closed loop, and both sides of the transfer film 180 are formed to extend in the horizontal direction, respectively, and are provided with a transfer shaft 181 supporting the transfer film 180, and the pair of Cooling water may be introduced into the transfer shaft 181, respectively. The transfer film 180 extends in the direction of the collection section 300 in the reaction chamber 100 and transfers the raw material collected in the reaction chamber 100 to the collection section 300. That is, while the transfer film 180 moves on the caterpillar along the closed loop, it moves inside the collection part 300 within the reaction chamber 100. In addition, the transfer shaft 181 may be provided to penetrate the reaction chamber 100 or the collection part 300 in the horizontal direction to facilitate the introduction or discharge of cooling water.

A motor that rotates the transfer film 180 or the transfer shaft 181 may be provided outside the reaction chamber 100 or the collection part 300.

In one embodiment of the present invention may be further connected to the transfer film 180 and further includes a cooling plate 182 that cools the transfer film 180 to a set temperature.

The cooling plate 182 cools the transfer film 180 to a predetermined temperature, and may contact the inner surface of the transfer film 180. In this case, the vaporized raw material is collected on the outer surface of the transfer film 180 and cooled to a temperature set through the cooling plate 182 in the direction of the collection part 300 in the reaction chamber 100. As it moves, it can be condensed and crystallized into nano powder. Cooling of the transfer film 180 through the cooling plate 182 may be using cooling water or using an inert gas at a set temperature.

One side of the transfer film 180 may be provided with a scraper 183 that is in contact with the transfer film 180 to scrape the nano powder transferred by the transfer film 180. The scraper 183 is formed to extend in the width direction of the transfer film 180 and is located in the collection part 300. In one embodiment of the present invention, the scraper 183 is in contact with the lower surface of the transfer film 180 and the nano-powder is separated from the transfer film 180 by the scraper 183 to collect 300 Is collected through.

The collection unit 300 of the present invention is connected to the first collection unit 310 and the first collection unit 310 for collecting the nano-powder separated from the transfer film 180, the first collection unit 310 It may be composed of a second collection unit 320 for collecting and transporting the collected nano-powder through, and a powder recovery unit 330 through which the nano-powder moved through the second collection unit 320 is recovered. The packaging step (S400) of the above-described nanopowder continuous manufacturing method may be performed through the collection unit 300.

Specifically, the first collection part 310 is provided with a vacuum port 102 connected to a vacuum pump (P), and the like, and moves the nano powder in a downward direction in an environment in which the inside is vacuum. A load lock valve or a gate valve may be provided in the first collecting part 310, and various configurations for collecting and moving the nano powder while maintaining a vacuum state may be additionally provided. The second collecting part 320 is provided with a vacuum port 102 connected to a vacuum pump P or the like, and may have the same configuration as the first collecting part 310. The nano-powder that has passed through the first collecting portion 310 and the second collecting portion 320 is finally recovered from the powder recovery portion 330. It is preferable that the first collection part 310 and the second collection part 320 are independently formed in a vacuum environment, and internal pressures may be different.

In addition, the upper portion of the collection portion 300 is provided with a viewport 301 formed of a transparent material and through the viewport 301 it is possible to visually check the internal situation of the collection portion 300.

The powder recovery unit 330 may be connected to the packaging container 340, a load lock valve is provided to move the nano-powder into the packaging container 340 by a predetermined amount in a vacuum state. In addition, the powder recovery unit 330 may be provided with a screw conveyor, the screw conveyor serves to move the nano-powder to a predetermined position while maintaining a vacuum state according to the rotation of the screw wound in the form of a screw.

The present invention having the above configuration is easy to mass-produce nano-powder with the configuration of the automatic feeding device 210 and the transfer film 180 in the production of nano-powder by using a transfer thermal plasma, evaporation and evaporation of raw materials The speed can be adjusted flexibly and a more homogeneous nanopowder can be recovered in a vacuum.

In the present invention, the raw material supply unit 200, the reaction chamber 100, and the collection unit 300 are all equipped with a vacuum port 102 and connected to a vacuum pump P, thereby supplying raw material in a vacuum environment, of nano powder. Creation and collection can proceed. The present invention, which maintains the above vacuum environment, has a structure of generating, collecting, and packaging nanopowders in a vacuum state, thereby preventing surface oxidation caused by atmospheric exposure to minimize the oxygen content of the nanopowders. In addition, supply of raw materials, generation of nano-powders from the components of the automatic feeding device 210, the transfer film 180, the first collecting portion 310 and the second collecting portion 320, the collection, packaging is continuous Consisting of, mass production is easier.

11 is an exemplary view showing modularization using four nanopowder continuous manufacturing apparatuses according to an embodiment of the present invention.

As shown in FIG. 11, the nano powder continuous manufacturing apparatus can be operated in one module by connecting four in parallel. In this case, by efficiently operating the vacuum pump (P), the automatic feeding device 210, cooling water, etc., it is possible to promote efficient production of nano powder.

According to the present invention having the above configuration, it is possible to continuously supply the raw material to the reaction chamber, to continuously recover the nano powder generated in the reaction chamber, and to easily supply the raw material, automate the production and collection of the nano powder. Do. In addition, as it progresses in a vacuum environment, it is possible to produce, collect and collect high-quality nano powders.

S100: Raw material supply step S200: Vaporization step
S210: particle size control process S220: production volume control process
S230: Evaporation amount control process S240: Atmosphere gas supply process
S250: Coating layer forming process S300: Nano powder forming step
S310: Cooling water circulation process S320: Surface temperature control process
S400: packing step
100: reaction chamber
101: material supply port 102: vacuum port
110: crucible 111: first track
112: second track 113: blocking jaw
120: crucible electrode 130: center of the crucible
140: crucible height adjustment means
143: 1st screw shaft 144: 1st screw motor
145: 1st ball nut
150: crucible rotating means 151: first gear
152: second gear
160: plasma electrode 161: tip
162: electrode center axis 163: connection terminal
170: electrode height adjustment means 171: second screw shaft
172: Second screw motor 173: Second ball nut
180: transfer film 181: transfer axis
182: cooling plate 183: scraper
200: raw material supply unit 210: automatic feeding device
211: Feeding housing 212: Feeding screw
213: opening and closing 214: feeding nozzle
215: Feeding motor 216: Feeding heater
300: collection part
301: viewport
310: first collection unit 320: second collection unit
330: powder recovery unit 340: packaging container
400: support frame
P: Vacuum pump

Claims (10)

A raw material supply step of supplying the raw material into the crucible;
A vaporization step of vaporizing the raw material contained in the crucible using a plasma electrode;
A nano-powder forming step of collecting and transporting the raw material vaporized in the vaporization step through a transfer film provided on an upper portion of the crucible and moving along an endless circulation loop to form a nano-powder;
Including the packaging step of packaging the nano-powder formed in the nano-powder forming step in a packaging container;
The raw material supply step, vaporization step, nano-powder forming step and packaging step is a continuous production method of nano-powder using a transfer type thermal plasma, characterized in that proceeds in a vacuum.
According to claim 1,
The vaporization step,
A particle size control process for adjusting a distance between the crucible and the transfer film; And
Continuous production method of the nano-powder using a transfer-type thermal plasma, characterized in that it comprises; a production control process for adjusting the distance between the crucible and the plasma electrode.
According to claim 2,
The vaporization step,
A method for continuously manufacturing nanopowder using a transferable thermal plasma, further comprising an evaporation amount control process of rotating the crucible so that the amount of evaporation of the raw material supplied to the crucible is adjusted.
According to claim 3,
The raw material supply step,
Continuous method of manufacturing nanopowder using a transferable thermal plasma, characterized in that raw materials of different materials are supplied to the crucible.
According to claim 2,
The vaporization step,
A method for continuously manufacturing nanopowders using a transportable thermal plasma, further comprising an atmospheric gas supply process for supplying atmospheric gas to the vaporized raw material.
The method of claim 5,
The atmosphere gas is a continuous manufacturing method of nano-powder using a transfer type thermal plasma, characterized in that is supplied using a flow controller between the crucible and the transfer film.
According to claim 1,
The vaporization step,
A method of continuously producing nanopowder using a transferable thermal plasma, further comprising a coating layer forming process of forming a coating layer on the surface of the raw material vaporized in the vaporization step by supplying a coating gas between the crucible and the transfer film. .
According to claim 1,
The nano-powder forming step,
A cooling water circulation process for circulating cooling water on both sides of the transfer film; And
A method for continuously manufacturing nanopowders using a transfer-type thermal plasma, comprising: a surface temperature control process of cooling the surface of the transfer film using a cooling plate.
According to claim 1,
The packaging step,
A method for continuously manufacturing nanopowders using a transportable thermal plasma, characterized in that the nanopowders are vacuum-packed by a predetermined amount in a packaging container using a load cell.
According to claim 1,
The raw material supply step, vaporization step and nano-powder forming step is a continuous manufacturing method of nano-powder using a transfer type thermal plasma, characterized in that is continuously performed for a set time.

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