KR100805776B1 - Free falling type precursor feeding apparatus for inductive coupled plasma nano powder reactor - Google Patents

Abstract

An apparatus for supplying free falling type starting materials for mass-producing nano-powders is provided to supply and control uniformly and continuously solid metal powders, and select the powders in accordance with grain size of a raw material powder, thereby increasing the productivity the nano-powders. An apparatus for supplying free falling type starting materials for mass-producing nano-powders comprises a cover(14) consisting of a gas injection port for supplying gas for transferring solid metal powder, a vacuum port for connecting power source(10) for supplying power to a rotary motor(1) and a vacuum vent port(9) for vacuum; an outer housing(12), upper end connected to the cover, lower end connected to a corn-shaped powder transferring path(7) and having a vacuum bypass line(8) at the upper end circumferential one side to form a vacuum space; and an inner housing(13) which consists of a solid metal powder container(15) spaced apart from the inner center of the outer housing, an insulation portion(4) equipped at the upper end of the solid metal powder container for electrical insulation, a powder transferring shaft(2) equipped to include a powder transferring screw(2a) connected to the rotary motor to rotate in a circumferential direction regarding the powder transferring shaft in accordance with the rotation of the rotary motor, a corn-shaped powder receiver where solid metal powder from the solid metal powder container is supplied directly downward and stored, and a disc-shaped metal filter(5) which has a vibration motor(6) at a lower end portion to filter the solid metal powder transferred from the power receiver.

Description

Free falling type precursor feeding apparatus for inductive coupled plasma nano powder reactor}

1 is a cross-sectional view schematically showing a free-fall starting material supply apparatus for producing nanopowders using ICP according to the present invention;

2 is a cross-sectional view taken along the line A-A of FIG.

3 is a cross-sectional view taken along the line B-B in FIG.

<Explanation of symbols for the main parts of the drawings>

1: rotary motor 2: rotary shaft for powder transfer

2a: Screw for powder transfer 3: Concave powder receiver

4: insulation part 5: metal filter

6: vibrating motor 7: corrugated powder conveying furnace

8: vacuum bypass line 9: vacuum exhaust port

10: vacuum port for power connection 11: gas injection port

12: outer housing 13: inner housing

14: cover 15: solid metal powder container

16: Free fall starting material supply device for mass production of nano powder using ICP

The present invention relates to a free fall start material supply apparatus of a nano powder mass production apparatus using an inductive coupled plasma (ICP) using a high frequency coil (RF antenna), and a raw material using a rotating motor and a vibration motor. The present invention relates to a starting material supply device capable of uniformly and continuously supplying a solid metal powder.

The present society has made continuous leaps under the development of high technology. Since the mid 1900s, advanced industries such as electricity, electronics, and computers have led science and industry as the basis of the main industries, but now the limits of continuous development have met the direct demands of miniaturization, integration, and convenience. Indicates. Therefore, the need for a variety of new materials, shrinking processes and the technology to advance to the next generation is emerging more than ever.

Thus, for this reason, the biggest topic in science and industry at present is nano.

Nano is a unit representing one billionth, derived from the ancient Greek nanos (nanos), which means dwarf, and one nanometer (nm) is one millionth of a meter, about one-eighth of the thickness of the hair. It's about 10 atoms side by side.

Nanotechnology is a technology that takes advantage of new phenomena and properties that occur when the size of a material is approximately several-100 nm. The number-100 nm scale is an ultrafine technology at the molecular or atomic level.

Nano is a new paradigm that can be created in a variety of industries by exploring new areas of technology and fusion with existing industrial technologies, breaking away from the arithmetic definition of nanometers of only one billionth of a meter, and meeting the needs and understanding of existing technologies. It has become a basic substance across science and industry.

Therefore, the objective of the present invention is to develop a nano powder mass production apparatus that can create high added value industrially.

A characteristic of typical nanomaterials is the fact that their color changes with size in the nanoscale. In the case of optical properties, for example, Au is generally golden, but when it is 20 nm or less, the color turns red, and even a slight change in size changes color.

In addition, as all materials are broken down from large chunks to small chunks, the surface area of the whole material is rapidly increased, which makes nanomaterials unique.

In the case of chemical properties, for example, when TiO ₂ has a particle size of 20 μm or less, when it receives weak ultraviolet rays generated from a fluorescent lamp or an incandescent lamp, it has a sterilizing power, a self-cleaning power, and an anti-fog effect.

In addition, in the case of mechanical properties, the particles of the polycrystalline material have the same basic arrangement for each particle, but the direction is different, and the more grain boundaries per unit area existing between the particles and the particles, the stronger the mechanical properties tend to be.

However, contrary to general trends, nanomaterial particles show a sharp increase in strength in a specific grain size region, which does not seem to be common sense.

However, in view of the increase in mechanical strength when mixed with other composites, nanoparticles should be regarded as having excellent mechanical properties among the existing materials.

The results of the research on nanomaterials are still in their infancy, and since they show completely different characteristics from conventional common sense, we can only assume that the mechanical strength is excellent.

In the case of electromagnetic properties, semiconductors, magnetic metals, and nanoparticles exhibiting electronic properties are known to have a maximum magnetic property value of about 10 to 100 μm as they become smaller.

For example, it is known that spherical magnetic metal nanoparticles of very small and uniform size can be synthesized at the same time as their magnetic properties are maximized, and each of these particles can be used as one bit through their regular arrangement. These magnetic particles are a few μm in size and consist primarily of cobalt or an alloy of cobalt and platinum.

In general, the device for supplying the solid metal powder refers to a supply device for supplying the metal powder into the reactor to mass-produce the nano powder, and the solid metal powder supplied from the starting material supply device is introduced into the reactor.

The conventional starting material supply device is to supply the solid metal powder through a method such as a rotary motor, a vibration motor, a pressure difference, etc., the starting material supply device to supply a solid metal powder by operating the rotating motor and the vibration motor at the same time. It will be.

However, the conventional starting material supply device has a problem in that it is not possible to uniformly and continuously supply and control various types and various types of solid metal powders as it is limited to a method by a single method.

In addition, the conventional starting material supply device has a problem that the application is limited due to the adsorption phenomenon of the powder on the inner wall of the container filled with the powder and the temporary over-feeding of the powder.

Therefore, the starting material supply system in the nano powder mass production device serves as a uniform and continuous supply of starting material. This is not just a supply of starting material, but also directly related to the stability of the plasma and the yield of nanopowders, which indirectly can cause severe burns throughout the system.

If the starting material is supplied unevenly, the plasma generated at the lower end of the starting material is greatly changed due to the change in the supply amount of the starting material supplied to the inside, causing the plasma to shake, or excessive amount of starting material If supplied, the plasma may be turned off, which may cause very large damage to the entire nanopowder production apparatus.

Therefore, uniform supply of the solid metal powder, continuous supply and blocking of the starting material to such a nano powder mass production device is a function that must be added to the starting material supply device, which is a design element.

Currently, there is a method using a pressure difference as a method used in the starting material supply device, the supply method is very diverse and many methods are still under development.

This is because each of the physical and chemical properties of the starting material shows very different feed conditions depending on the conditions.

In the case of the method using the difference in pressure, for a simple example, the starting material of Au and Ag shows a significant difference in density compared to Ag for Au, the density of Au is 19.32g / cm 3, and the density of Ag is 10.50g / Cm 3.

If the starting material is supplied according to the method using the pressure difference, it may be possible to supply Ag, but due to the difference in density of the two metals, it is almost impossible to supply Au in the same state under the same conditions.

Therefore, in order to supply Au as Ag, a larger pressure difference should be given, which is a problem that cannot be used because this may have a great effect on the plasma generated at the lower end.

Accordingly, the present invention has been proposed to solve the above problems, and an object thereof is to limit the type and form of solid metal powder by using a rotating motor, a screw for conveying powder, a vibration motor, and a metal filter. It is possible to supply and adjust uniformly and continuously without using it, and to supply the solid metal powder filled in the powder filling container installed inside the vacuum container by the rotary motor and the powder conveying screw to the metal filter as the final supply port. And to block, and to supply the powder adsorbed on the inner wall of the filling container by using a screw for feeding, and also, by vibrating motor and metal filter to select the powder size according to the filter at the final supply of the solid metal powder It is to provide a starting material supply device for the production of nano-powder using ICP available.

Accordingly, the present invention for achieving the above object is a cover comprising a gas injection port for supplying the gas for transporting the solid metal powder, a vacuum port for connecting the power supply for supplying power to the rotary motor and a vacuum exhaust port for the vacuum; An outer housing connected to a cover at an upper end thereof, and connected to a powdered feed path at a lower end thereof, and having a vacuum bypass line at one side of the upper outer circumference thereof to form a vacuum space in a vacuum state; And a rotary metal connected to the solid metal powder container spaced apart from the inner center of the outer housing and provided in a vertical upward direction, an insulator provided at the top of the solid metal powder container for electrical insulation, and a rotating motor provided at the top center of the insulated part. Rotary shaft for conveying powder is provided to rotate in the circumferential direction with respect to the vertical downward direction according to the rotation of, the powdered powder receiver that is supplied and stored directly from the solid metal powder container is stored and the vibration motor is provided at the bottom And an inner housing made of a disk-shaped metal filter provided for filtering the solid metal powder conveyed from the mold powder receiver.

Due to the rotational movement of the rotary motor and the rotating shaft for transporting the powder, it is possible to prevent adsorption of the solid metal powder filled in the solid metal powder container.

A continuous supply of solid metal powder is possible due to the rotational movement of the rotating shaft for feeding the powder inside the bottom of the corrugated powder receiver.

It is characterized in that the supply of the solid metal powder can be selectively blocked due to the rotational movement of the rotating shaft for conveying the powder in the bottom of the corrugated powder receiver.

By vibrating the vibration motor, the metal filter is characterized in that the solid metal powder can be selected and supplied by size.

By vibrating the vibration motor, the metal filter is characterized in that the recollection of the sorted solid metal powder is possible.

Insulation is characterized in that it comprises a plate coated with an insulating material so that electrical insulation between the rotating motor, the inner housing and the outer housing is made.

The insulating material applied to the plate of the insulating portion is preferably characterized in that the Teflon material.

The solid metal powder container is preferably sealed to protect the solid metal powder filled therein.

The gas injection port is capable of protecting the gas for transporting the solid metal powder in the vacuum space above the outer housing.

It is characterized in that the uniform supply of the solid metal powder through the transfer efficiency and spiral movement of the solid metal powder through the powder-type powder conveying path.

The metal filter may be selectively formed in various sizes according to the grain size of the precursor powder supplied.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.

1 is a cross-sectional view schematically showing a free-fall starting material supply apparatus for mass production of nanoparticles using ICP according to the present invention, Figure 2 is a cross-sectional view of the line A of Figure 1, Figure 3 is a cross-sectional view of the line B of FIG.

As shown in Figures 1 to 3, the free fall starting material supply apparatus for mass production of nano-powders using ICP according to the present invention is a gas injection port 11, a rotary motor (1) for supplying a gas for transporting a solid metal powder The cover 14 having a vacuum port 10 for connecting power and a vacuum exhaust port 9 for vacuum is provided on the upper part.

In addition, an upper end is connected to the cover 14, and a lower end is connected to the cockle-shaped powder transfer path 7, and an outer space in which a vacuum bypass line 8 is provided at one outer circumference of the upper end forms a vacuum space in a vacuum state. The housing 12 is provided outside.

In addition, the solid metal powder container 15 is provided to have a predetermined height in the vertical upward direction from the inner center of the outer housing 12, and the insulating portion (4) provided on the top of the solid metal powder container 15 for electrical insulation And a screw for transport (2a) connected to the rotary motor (1) provided at the center of the upper end of the insulating portion (4) so as to rotate in the circumferential direction with respect to the vertical downward direction in accordance with the rotation of the rotary motor (1). Rotating shaft (2) for transporting the powder is provided to include, the solid metal powder is supplied from the solid metal powder container 15 is provided directly below the pin shaped powder receiver (3) and the vibration motor 6 is provided at the lower end And an inner housing 13 formed of a disk-shaped metal filter 5 provided for filtering the solid metal powder conveyed from the corrugated powder receiver 3.

The free fall starting material supply device for mass production of nano-powders using the ICP is a rotary motor (1) which is responsible for the initial transfer of the solid metal powder in the upper part around the powder-shaped receiver (3) in the outer housing (12). ) Is mounted above the insulator 4, and a disk-shaped metal filter 5 is provided at the bottom thereof, and a vibration motor 6 is mounted at the bottom thereof.

In addition, the transport gas supplied through the gas injection port 11 is transported through the corrugated powder transport path 7.

In addition, a vacuum exhaust port 9 is connected to an upper end of the outer housing 12, and a vacuum bypass line 8 is connected to one side of the outer housing 12.

Therefore, the free fall starting material supply device for mass production of nanoparticles using ICP according to the present invention is largely the starting material supply unit is the rotary motor (1), the screw for conveying powder (2a), the metal filter (5), the vibration motor (6) And the starting material filling part is composed of the solid metal powder container 15 in the inner housing 13, and the vacuum line is composed of the vacuum bypass line 8, the vacuum exhaust port 9, and the like.

The gas injection port 11 is involved in the gas.

The starting material supply part is equipped with a powder conveying screw (2a) from the supply region to the inner space of the inner housing 13 in which the starting material is filled in the rotating motor (1) to rotate to serve as a primary powder supply At the same time, it serves as a primary stopper of the powder.

Thereafter, the starting material supplied through the powder conveying screw 2a of the powder conveying rotating shaft 2 is seated on the metal filter 5 provided with the vibrating motor 6, and the vibrating motor 6 Starting material is uniformly supplied using the vibration of) and starting material larger than the voids of the metal filter 5 is not injected and exits to the side of the metal filter 5, so that the starting material is larger than the voids of the metal filter 5. Only materials with a small grain size or less can be supplied.

Therefore, the instantaneous shaking of the ICP generated during the supply of a material having a large particle size to the ICP may also be minimized, and stable supply and mass production of nano powder may be possible.

In addition, the powder transport rotary shaft 2 including the powder transport screw (2a) at the upper end is connected to the rotary motor (1) is connected to the space filled with the starting material is transported and filled with the powder at the same time It is possible to prevent the powder from being hardly compacted by pressure.

In addition, the starting material filling unit is formed by the gas and the vacuum in the vacuum space above the outer housing 12 to prevent the starting material from leaking due to the pressure difference when the starting material transport gas is injected and the initial vacuum is made. Due to the pressure difference, the starting material does not come out of the solid metal powder container 15, and the starting material injection capacity is about 500 g based on Au.

In addition, the vacuum line is vacuum in addition to the main vacuum line in order to create a smooth base vacuum state for the entire free-fall starting material supply apparatus for mass production of nano-powder using ICP according to the present invention, and at the same time the supply of the starting material can be blocked. When a vacuum line is initially created with a bypass line 8, the main vacuum line is locked and a vacuum can be made using the vacuum bypass line 8, and the supply of starting material after the hole is made. The vacuum bypass line 8 is closed and the starting material and the transport gas can be injected through the main vacuum line.

In addition, when vacuuming the free fall start material supply device for mass production of nanopowders using ICP, the vacuum may be destroyed without affecting the entire supply device 1 through the vacuum exhaust port 9.

Gas injected into the free fall start material supply device for mass production of nanopowders using ICP can also be injected with plasma reaction gas, argon gas and other kinds of gases. In other words, it serves to smoothly supply the starting material without stagnation in the middle of the supply line, and the gas can simultaneously cool the heat generated by the rotary motor 1 installed therein, thereby generating the vacuum. The cause of the failure of the rotary motor 1 by heat is cut off.

Since the insulating part 4 for electrical insulation may give an electric shock to the rotating motor 1 by the plasma induced when the plasma is generated, the upper end of the solid metal powder container 15 is made of Teflon material to block the electric shock. With a plate applied.

Hereinafter, the operating state of the free-fall start material supply apparatus for mass production of nanoparticles using ICP according to the present invention will be described.

First, after supplying raw material powder to the corrugated solid metal receiver 3, the upper space of the outer housing 12 forms an initial vacuum state through the vacuum bypass line 8.

Then, when the vacuum bypass line (8) is locked, the flow of vacuum exhaust and transfer gas is made through the compact powder conveying path (7).

As the rotary motor 1 operates, the powder transfer rotary shaft 2 rotates in the circumferential direction with respect to the vertically downward direction, thereby converting the solid metal powder in the powdered powder receiver 3 into the powdered powder. It is transferred to a disk-shaped metal filter (5) located at the bottom of the receiver (3).

Thereafter, the solid metal powder transferred to the metal filter 5 is freed into the corrugated powder conveying path 7 due to the vibration generated by the operation of the vibration motor 6 provided at the bottom of the metal filter 5. Dropped and transported to the reaction tube (not shown) of the nano-powder production apparatus using ICP.

In the structure of the free drop start material supply device for mass production of nanopowders using ICP according to the present invention, the screw 2a constituting the rotating shaft 2 for conveying the powder is a solid metal powder reaction tube (not shown) before the supply of the solid powder. C) has a stop function for preventing and blocking free fall into the inside, and the metal filter 5 forms a metal filter 5 having various pores according to the grain size of the raw material powder supplied. Optionally available.

As described above, the free-falling starting material supply device for mass production of nanoparticles using ICP according to the present invention can not only uniformly and continuously supply and control the solid metal powder, but also can be selected according to the size of the raw powder. There is an effect that can increase the production productivity of powder mass production.

In addition, by uniformly and continuously supplying the solid metal powder has an effect that can increase the stability of the entire nano-powder mass production apparatus using ICP.

Claims (12)

A cover comprising a gas injection port 11 for supplying a gas for transporting a solid metal powder, a vacuum port 10 for supplying power to the rotary motor 1, and a vacuum exhaust port 9 for vacuum ( 14); The upper housing is connected to the cover 14, the lower end is connected to the corrugated powder transport path (7), the outer housing is provided with a vacuum bypass line (8) on the outer peripheral side to form a vacuum space in a vacuum state ( 12); And A solid metal powder container 15 spaced apart from an inner center of the outer housing 12 in a vertical upward direction; an insulating portion 4 provided on an upper portion of the solid metal powder container 15 for electrical insulation; It is connected to the rotary motor (1) provided in the center of the upper end of the insulating portion (4) to include a screw for conveying powder (2a) to rotate in the circumferential direction with respect to the vertical down direction in accordance with the rotation of the rotary motor (1) Rotating shaft (2) for powder transport, the powdered powder receiver (3) that is supplied and stored directly from the solid metal powder container 15 and stored therein and the vibration motor (6) at the lower end is provided An inner housing (13) provided with a disk-shaped metal filter (5) provided for filtering the solid metal powder conveyed from the mold powder receiver (3); Free fall start material supply device for mass production of nanoparticles using ICP, characterized in that provided in the. The method of claim 1, wherein the adsorption of the solid metal powder filled in the solid metal powder container is prevented due to the rotational movement of the rotary motor 1 and the powder transporting shaft 2. Free fall starting material supply device for mass production of nano powder. The method of claim 1, wherein the supply of solid metal powder is possible due to the rotational movement of the rotating shaft (2) for transporting powder in the bottom of the pinch powder receiver 3 for mass production of nanoparticles using ICP Free fall starting material supply. The nanopowder using ICP according to claim 1, characterized in that the supply of solid metal powder can be selectively blocked due to the rotational movement of the rotating shaft 2 for transporting the powder inside the bottom of the corrugated powder receiver 3. Free fall starting material supply for mass production. According to claim 1, The metal filter (5) by vibrating the vibration motor (6) of the free fall starting material supply apparatus for mass production of nano-powder using ICP, characterized in that the solid metal powder can be selected and supplied by size. . According to claim 1 or 5, wherein the vibration of the vibration motor 6, the metal filter 5 is free for mass production of nano-powder using ICP, characterized in that the re-collection of the sorted solid metal powder is possible. Drop start material supply. 2. The insulating part (4) according to claim 1, characterized in that the insulating part (4) comprises a plate coated with an insulating material so that electrical insulation between the rotary motor (1), the inner housing (13) and the outer housing (12) is achieved. Free fall start material supply apparatus for mass-producing nanoparticles using ICP which are used. 8. The apparatus of claim 7, wherein the insulating material applied to the plate of the insulating part (4) is made of Teflon material. The apparatus of claim 1, wherein the solid metal powder container (15) is hermetically sealed to protect the solid metal powder filled therein. The method of claim 1, wherein the gas injection port 11 can protect the gas for transporting the solid metal powder in the upper vacuum space of the outer housing 12, characterized in that the supply of free-fall starting material for the production of nano-powder using ICP Device. The method of claim 1, wherein the free powder for mass production of nanoparticles using ICP, characterized in that uniform supply of the solid metal powder through the transfer efficiency and the spiral movement of the solid metal powder through the powdered powder conveying path (7). Drop start material supply. The apparatus of claim 1, wherein the metal filter (5) can be selectively formed in various sizes according to the grain size of the powder to be supplied.

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