KR101724359B1 - Method of manufacturing of silicon nanopowder and Apparatus of manufacturing of silicon nanopowder - Google Patents
Method of manufacturing of silicon nanopowder and Apparatus of manufacturing of silicon nanopowder Download PDFInfo
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- KR101724359B1 KR101724359B1 KR1020160044203A KR20160044203A KR101724359B1 KR 101724359 B1 KR101724359 B1 KR 101724359B1 KR 1020160044203 A KR1020160044203 A KR 1020160044203A KR 20160044203 A KR20160044203 A KR 20160044203A KR 101724359 B1 KR101724359 B1 KR 101724359B1
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- gas
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0894—Processes carried out in the presence of a plasma
- B01J2219/0896—Cold plasma
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
Description
The present invention relates to a method for producing silicon nano powder and an RF thermal plasma apparatus for producing silicon nano powder.
Due to the rapid growth of the semiconductor industry and the demand for solar cells, the silicon wafer industry is also steadily growing. In such semiconductor and wafer manufacturing processes, silicon wafer wastes are generated, most of which can not be recycled and landfilled. Methods of recovering and recycling such abandoned silicon wastes as useful resources are being researched.
Examples of the method for producing the silicon nano powder include a solid phase synthesis method, a liquid phase synthesis method, and a vapor phase synthesis method. The gas phase synthesis method is the most preferred because it has a high reaction rate, a very simple process and high purity particles. Particularly, the gas phase synthesis process using RF thermal plasma can synthesize silicon nano powder in a short period of time, and is advantageous in that vaporization is easy, yield is good, and process conditions are easily controlled by using a high temperature plasma.
Plasma consists of charged particles and neutral particles, and is divided into thermal plasma or cold plasma depending on the activation method and activation energy. Thermal plasma is an ionized gas composed of electrons, ions, atoms and molecules, and is a state of a fourth material with an ultra-high temperature and high heat capacity ranging from several thousand to tens of thousands of K.
Typical methods of generating thermal plasma are plasma generating a DC or AC arc discharge and RF plasma using a radio frequency (RF) magnetic field. RF thermal plasma is the most suitable device for obtaining nanoparticles on a large scale with high purity. The RF thermal plasma system can prevent oxidation of the product by blocking contact with the external environment, especially oxygen. In addition, since a discharge occurs without an electrode, it is possible to obtain a material of high purity.
The RF thermal plasma apparatus is a device for generating a plasma. Generally, the RF plasma plasma apparatus generates a plasma. A raw material supply part for supplying raw materials into the torch, a reaction chamber for providing a reaction space, and a particle collecting part.
[Prior Art Literature]
[Patent Literature]
Korean Patent Laid-Open Publication No. 10-2016-0009817 (2016.01.27)
It is an object of the present invention to provide a method for producing silicon nano powder and an RF thermal plasma apparatus for producing silicon nano powder which are capable of finding optimal cooling gas injection position and flow rate conditions and selectively producing particle sizes under these conditions.
A method of manufacturing a silicon nano powder according to an embodiment of the present invention includes: (1) generating an RF thermal plasma by supplying an RF thermal plasma generating gas to an RF thermal plasma apparatus; (Step 2) of injecting a cooling gas through a cooling device in a direction opposite to the feeding direction of the RF thermal plasma generating gas of the step 1; And supplying the silicon raw material powder to the RF thermal plasma generated in the step 1 to vaporize and cool the silicon raw material powder (step 3); .
The flow rate of the cooling gas in the
The distance between the nozzle of the cooling device for supplying the cooling gas in the
The cooling gas in the
The thermal plasma generating gas in step 1 may be hydrogen and argon.
The silicon raw material powder of step 3 may be obtained by grinding the defective product generated in the production of the silicon wiper.
The diameter of the silicon raw material powder in the step 3 may be 38 탆 or less.
Further, an RF thermal plasma apparatus according to an embodiment of the present invention includes a torch for generating a thermal plasma; A reactor extending in a flow direction of the thermal plasma generated in the torch; A raw material supply device for injecting the silicon raw material powder into the generated thermal plasma; And a cooling device for injecting a cooling gas in an opposite direction to the direction in which the plasma generating gas is injected.
The method for producing silicon nano powder according to the embodiment of the present invention and the RF thermal plasma apparatus for producing silicon nano powder are characterized in that cooling gas is injected in the direction opposite to the plasma gas to increase the cooling effect and the gasification rate, And the injection position can be adjusted to form small and uniform nano-sized particles.
Figure 1 shows an RF thermal plasma apparatus.
Figure 2 shows a cooling device.
3 shows an XRD pattern of a silicon raw material powder.
4 shows an XRD pattern of a silicon nano powder.
5 to 7 are SEM photographs of silicon nano powders produced according to the use of hydrogen gas and cooling apparatus.
8 to 12 are SEM photographs of silicon nano powders produced according to an embodiment of the present invention.
13 to 15 are SEM photographs of silicon nano powders produced according to the use of hydrogen gas and cooling apparatus.
16 to 18 show the particle size distribution of the silicon nano powder produced according to whether or not the hydrogen gas and the cooling device are used.
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings. However, the embodiments of the present invention can be modified into various other forms, and the scope of the present invention is not limited to the embodiments described below. Further, the embodiments of the present invention are provided to more fully explain the present invention to those skilled in the art. Accordingly, the shapes and sizes of the elements in the drawings may be exaggerated for clarity of description, and the elements denoted by the same reference numerals in the drawings are the same elements. In the drawings, like reference numerals are used throughout the drawings. In addition, "including" an element throughout the specification does not exclude other elements unless specifically stated to the contrary.
A method of manufacturing a silicon nano powder according to an embodiment of the present invention includes: (1) generating an RF thermal plasma by supplying an RF thermal plasma generating gas to an RF thermal plasma apparatus; (Step 2) of injecting a cooling gas through a cooling device in a direction opposite to the feeding direction of the RF thermal plasma generating gas of the step 1; And supplying the silicon raw material powder to the RF thermal plasma generated in the step 1 to vaporize and cool the silicon raw material powder (step 3); .
Hereinafter, a method for producing silicon nano powder according to an embodiment of the present invention will be described in detail for each step.
First, in the method for producing silicon nano powder according to an embodiment of the present invention, step 1 is a step of generating a RF thermal plasma by supplying a thermal plasma generating gas to a thermal plasma apparatus.
The RF
The
A center gas is introduced into the confinement tube, and a sheath gas is introduced between the confinement tube and the induction coil to prevent the powder from being adsorbed.
The sheath gas may be a mixture of argon gas and hydrogen gas, the flow rate of the argon gas may be 50 L / min, and the flow rate of the hydrogen gas may be 10 L / min. The center gas may be argon gas and the flow rate may be 20 L / min.
The diameter of the torch outlet is preferably larger than the nozzle diameter of the torch to regulate the plasma velocity so that the silicon raw material powder is vaporized.
The
In the RF thermal plasma according to the present invention, a magnetic field formed by the current flowing through the induction coil is generated, and an electric field formed around the magnetic field can be formed by accelerating electrons and ionizing due to continuous collision of accelerated atoms.
Next, in the method for producing silicon nano powder according to the present invention, the
The
The cooling gas in the
Next, in the method of manufacturing the silicon nano powder according to the present invention, step 3 is a step of supplying the silicon raw material powder to the RF thermal plasma generated in step 1 and vaporizing and cooling it.
Specifically, the supply of the silicon raw material powder in the step 3 is preferably performed in the direction of generating the thermal plasma in the step 1, and the silicon raw material powder having a high specific heat can be effectively vaporized. When the silicon raw material powder is supplied in the direction of generating the thermal plasma, the injected raw material powder stays relatively long in the high temperature region along the flow of the high temperature plasma, so that complete vaporization can occur. At this time, an inert gas such as argon gas may be used as a carrier gas to supply the silicon raw material powder.
The silicon raw material powder injected through the carrier gas inlet in the raw material supply device is obtained by pulverizing a defective product generated in the course of production of a silicon wafer and has a diameter of 25 to 50 탆, preferably 38 탆, and an injection speed of 0.5 to 2 g / min, preferably 1 g / min. The injected silicon raw material powder is vaporized while passing through a high-temperature thermal plasma region formed in the reactor, and rapidly cooled by the injected cooling gas.
The
In order to prevent the oxidation of silicon due to the inflow of air into the reactor, it is preferable to perform the reaction in a closed state. The
The silicon raw material powder vaporized by the thermal plasma is quenched by the cooling gas in the inner wall of the
In addition, the cooling gas injected in the direction opposite to the thermal plasma generating gas through the cooling device forms turbulence in the plasma flow to increase the time for residence in the high temperature plasma region by recycling the silicon raw material powder to increase the rate of vaporization .
The generated silicon nano powder can be collected through the
Thus, the silicon nano powder according to the present invention can be produced.
An RF thermal plasma apparatus according to an embodiment of the present invention will be described.
An RF thermal plasma apparatus for producing silicon nano powder according to an embodiment of the present invention includes a torch for generating RF thermal plasma; A reactor extending in a flow direction of the thermal plasma generated in the torch; A raw material supply device for injecting the silicon raw material powder into the generated thermal plasma; And a cooling device for injecting a cooling gas in a direction opposite to the direction of the plasma generating gas.
The flow rate of the cooling gas injected from the cooling device may be 70 L / min.
The distance between the nozzle of the cooling device and the outlet of the torch may be 350 mm.
The cooling device may inject a cooling gas toward the center of the thermal plasma region.
The thermal plasma generating gas injected into the torch of the RF thermal plasma apparatus may be hydrogen and argon.
The silicon raw material powder to be injected into the raw material supply device may be obtained by grinding a defective product generated during the production of the silicon wafer.
The diameter of the silicon raw material powder injected into the raw material supply device may be 38 탆 or less.
Figure 1 shows an RF thermal plasma apparatus for the production of silicon nano powder.
Referring to FIG. 1, an RF
Referring to FIG. 1, the
Referring to FIG. 1, the
The
The heat insulating tube of the
FIG. 2 is an enlarged view of the
Referring to FIG. 2, the
The present invention is characterized in that the size of the silicon nano powder is controlled by adjusting the gap between the nozzle of the
Hereinafter, the present invention will be described in more detail with reference to the following Examples and Experimental Examples.
However, the following examples and experimental examples are intended to illustrate the contents of the present invention, but the scope of the invention is not limited by the examples and the experimental examples.
In this experiment, a 4 MHz, 30 kW RF thermal plasma system (PL-35, TEKNA Plasma Systems) was used to generate high temperature thermal plasma.
≪ Example 1 > Preparation of silicon nano powder 1
Step 1: Step of generating RF thermal plasma
Argon (Ar) was supplied as an RF thermal plasma generating gas to the torch of the RF thermal plasma apparatus shown in FIG. 1, and thermal plasma was generated under the operating conditions shown in Table 1 below.
Step 2: Cooling gas injection step
The cooling gas was injected through the cooling device in the direction opposite to the feeding direction of the RF thermal plasma generating gas in the step 1. The flow rate of the cooling gas was 45 L / min. At this time, the distance between the torch outlet and the cooling device nozzle was 150 mm.
Step 3: Supplying the silicon raw material powder and vaporizing and cooling it
The silicon raw material powder was supplied through the raw material supply device provided at one side of the torch of the thermal plasma apparatus of step 1 to vaporize and cool the silicon raw material powder. The flow rate of the carrier gas was 5 L / min.
≪ Example 2 > Preparation of
Silicon nanocrystals were prepared in the same manner as in Example 1, except that the RF thermal plasma generating gas was a mixed gas of argon and hydrogen under the same operating conditions as in Table 1 below.
Hydrogen: 10 L / min
≪ Example 3 > Preparation of silicon nano powder 3
In the same manner as in Example 2, except that the flow rate of the cooling gas was 30 L / min under the operating conditions shown in Table 3 below in
Hydrogen: 10 L / min
≪ Example 4 > Preparation of
In the same manner as in Example 2 except that the flow rate of the cooling gas was 50 L / min and the distance between the outlet of the torch and the cooling device nozzle was 350 mm under the operating conditions shown in Table 4 below in the
Hydrogen: 10 L / min
≪ Example 5 > Preparation of
In the same manner as in Example 2 except that the flow rate of the cooling gas was 70 L / min and the distance between the outlet of the torch and the cooling device nozzle was 350 mm under the operating conditions shown in Table 5 below in
Hydrogen: 10 L / min
≪ Example 6 > Preparation of
Example 2 was carried out in the same manner as in Example 2 except that the flow rate of the cooling gas was 70 L / min and the distance between the outlet of the torch and the cooling device nozzle was 250 mm under the operating conditions shown in Table 6 below To prepare a silicon nano powder.
Hydrogen: 10 L / min
≪ Example 7 > Preparation of silicon nano powder 7
Example 2 was carried out in the same manner as in Example 2 except that the flow rate of the cooling gas was 70 L / min under the operating conditions shown in Table 7 below, and the distance between the outlet of the torch and the cooling device nozzle was 150 mm To prepare a silicon nano powder.
Hydrogen: 10 L / min
≪ Comparative Example 1 &
Step 1: Step of generating RF thermal plasma
Argon and hydrogen were supplied to the torch of the thermal plasma apparatus shown in FIG. 1 as an RF thermal plasma generating gas, and thermal plasma was generated under the operating conditions shown in Table 8 below.
Step 2: Silicon powder feed and vaporization step
The silicon raw material powder was supplied through the raw material supply device provided at one side of the torch of the thermal plasma apparatus of step 1 to vaporize the silicon raw material powder.
Step 3: The silicon raw material powder vaporized in
Hydrogen: 10 L / min
<Experimental Example 1> SEM analysis
The silicon nano powders prepared in Examples 1 to 3 were observed by SEM and the results are shown in FIGS. 5 to 7. FIG.
As shown in FIGS. 5 and 7, it can be seen that relatively large non-vaporized particles remained, unlike in FIG. 6 where hydrogen gas and a cooling device were used at the same time.
<Experimental Example 2> Surface area analysis
The surface area and the converted particle size of the silicon nano powder prepared in Examples 1 and 2 and Comparative Example 1 are shown in Table 9.
The converted particle size (D eq ) in Table 9 can be obtained through the formula (1).
[Equation 1]
In the formula (1), SSA is the surface area of the powder particles, and rho is the density of silicon.
The surface area of the particles was the largest in Example 2 using the hydrogen gas and the cooling device together, and it was confirmed that the converted particle diameters were also the smallest. From the results of the analysis, it was confirmed that when the rate of vaporization is low and relatively large particles exist at a high ratio, the surface area becomes smaller and the converted particle size increases.
<Experimental Example 3> SEM analysis
The silicon nano powders prepared in Examples 3 to 7 were observed by SEM and are shown in Figs. 8 to 12. Fig.
It was confirmed that more particles were vaporized in FIG. 8 to FIG. 10, and large particles in FIG. 10 were remarkably reduced. 11 and 12 show that a large number of large and large particles are observed in comparison with FIG. 10, indicating that the rate of vaporization is lowered. It was confirmed that the vaporization was most favorable in Example 5 and nanoparticle formation was most excellent.
<Experimental Example 4>
The silicon nano powders prepared in Examples 3 to 7 were observed with an SEM and magnified to a high magnification (x100,000). The results are shown in Figs. 13 to 15. Fig.
SEM photographs showed that the size of silicon nanoparticles decreased as the flow rate of cooling gas increased at the same interval.
<Experimental Example 5>
The particle size distributions of the silicon nano powders prepared in Examples 4 to 6 are shown in Figs.
As the flow rate of the cooling gas increases, the particle size distribution becomes uniform.
<Experimental Example 6>
The average particle sizes of the silicon nano powders prepared in Examples 4 to 6 are shown in Table 10.
It was confirmed that particles having the smallest size and the smallest size distribution were produced in Example 5.
The present invention is not limited to the above-described embodiment and the accompanying drawings, but is intended to be limited by the appended claims. It will be apparent to those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. something to do.
100: RF thermal plasma device
110: Torch
120: Power supply
130: Reactor
140: Feeding device
150: plasma generating gas supply device
160: Cooling unit
161:
162: Holder
163: Cooling gas inlet
164: cooling gas outlet
165: Cooling water inlet
166: Cooling water outlet
170: connection tube
180: Cyclone
191: Bag filter
192: Vacuum pump
Claims (8)
(Step 2) of injecting a cooling gas through a cooling device in a direction opposite to the feeding direction of the RF thermal plasma generating gas of the step 1; And
(Step 3) of supplying the silicon raw material powder to the RF thermal plasma generated in the step 1 and vaporizing and cooling the silicon raw material powder,
Wherein the flow rate of the cooling gas in step 2 is 65 to 75 L / min, and the distance between the nozzle of the cooling device in step 2 and the outlet of the torch is 300 to 400 mm.
Wherein the cooling gas of step 2 is injected toward the center of the plasma region generated in step 1.
Wherein the thermal plasma generating gas in step (1) is hydrogen and argon.
Wherein the silicon raw material powder of step 3 is obtained by grinding a defective product generated in the course of producing a silicon wafer.
Wherein the diameter of the pulverized silicon raw material powder is 38 占 퐉 or less.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200056073A (en) | 2018-11-14 | 2020-05-22 | 주식회사 멘도타 | Manufacturing apparatus and manufacturing method of nanopowder using DC arc plasma and apparatus for manufacturing the same |
| KR20230046641A (en) * | 2021-09-30 | 2023-04-06 | 충북대학교 산학협력단 | Method for preparing silicon nano-sized powder from waste solar panel |
| KR20230064982A (en) | 2021-11-04 | 2023-05-11 | 김태윤 | Method for manufacturing multi-composite nanopowder using transfer arc plasma and multi-composite nanopowder prepared by the same method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002253953A (en) * | 2001-02-28 | 2002-09-10 | C I Kasei Co Ltd | Apparatus and method of manufacturing ultrafine particle |
| KR100828102B1 (en) * | 2006-12-22 | 2008-05-08 | 주식회사 포스코 | Method and apparatus for silicon powder production |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002253953A (en) * | 2001-02-28 | 2002-09-10 | C I Kasei Co Ltd | Apparatus and method of manufacturing ultrafine particle |
| KR100828102B1 (en) * | 2006-12-22 | 2008-05-08 | 주식회사 포스코 | Method and apparatus for silicon powder production |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200056073A (en) | 2018-11-14 | 2020-05-22 | 주식회사 멘도타 | Manufacturing apparatus and manufacturing method of nanopowder using DC arc plasma and apparatus for manufacturing the same |
| KR20230046641A (en) * | 2021-09-30 | 2023-04-06 | 충북대학교 산학협력단 | Method for preparing silicon nano-sized powder from waste solar panel |
| KR102592579B1 (en) * | 2021-09-30 | 2023-10-23 | 충북대학교 산학협력단 | Method for preparing silicon nano-sized powder from waste solar panel |
| KR20230064982A (en) | 2021-11-04 | 2023-05-11 | 김태윤 | Method for manufacturing multi-composite nanopowder using transfer arc plasma and multi-composite nanopowder prepared by the same method |
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