KR20160123655A - Fluidized bed reactor for manufacturing granular polycrystalline silicon - Google Patents
Fluidized bed reactor for manufacturing granular polycrystalline silicon Download PDFInfo
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- KR20160123655A KR20160123655A KR1020150053976A KR20150053976A KR20160123655A KR 20160123655 A KR20160123655 A KR 20160123655A KR 1020150053976 A KR1020150053976 A KR 1020150053976A KR 20150053976 A KR20150053976 A KR 20150053976A KR 20160123655 A KR20160123655 A KR 20160123655A
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1845—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with particles moving upwards while fluidised
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1836—Heating and cooling the reactor
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
- C30B31/06—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor by contacting with diffusion material in the gaseous state
- C30B31/10—Reaction chambers; Selection of materials therefor
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Abstract
Description
The present invention relates to a fluidized bed reactor which can be used to produce polycrystalline silicon (hereinafter referred to as 'particulate polysilicon').
Polysilicon is a basic raw material for the photovoltaic industry and the semiconductor industry, and the demand for the polysilicon is rapidly increasing with the development of the relevant industrial field in recent years.
Polysilicon is mainly manufactured by a method of precipitating a silicon element on a silicon surface through thermal decomposition and / or hydrogen reduction reaction of a silicon-containing source gas. Typically, Siemens method using a bell-jar type reactor, a method using a fluidized bed reactor may be mentioned as an example.
Among them, the Siemens method is a conventional method of depositing silicon on the surface of a silicon rod provided in a bell-shaped reactor, in which the surface area required for the deposition of silicon is limited and the diameter of the silicon rod increases due to the deposition reaction Therefore, a continuous process is impossible. In addition, the Siemens method has a limitation in productivity because the power consumption per unit weight of the produced polysilicon is large.
A method using a fluidized bed reactor is a method of growing a seed by precipitating silicon on the surface of a polysilicon seed heated at a high temperature by pyrolysis of a raw material gas. The method using a fluidized bed reactor has advantages in that the surface area of the seed in which the precipitation reaction of silicon can occur is large, silicon can be precipitated at a relatively low temperature, the post-treatment process is simple, and the production efficiency is superior to that of the Siemens method .
1 is a cross-sectional view schematically showing the structure of a conventional fluidized bed reactor for producing polysilicon. In a conventional fluidized bed reactor, a heating means for heating the polysilicon seed is provided outside the reactor as shown in Fig. 1 (a) or inside the reactor as shown in Fig. 1 (b).
However, when the size of the reactor is increased, the temperature difference between the wall surface of the reactor and the center of the reactor becomes large, as shown in FIG. 1 (a) . In order to overcome these limitations, the method of changing the reaction conditions is applied, but the decrease of the production efficiency due to the increase of the side reaction is still pointed out as a problem.
The internal heating system as shown in FIG. 1 (b) can reduce the temperature difference in the reactor as compared with the external heating system. However, such an internal heating method has a problem that the polysilicon particles may be contaminated and the possibility of abnormal shut-down in the reactor is relatively high, resulting in poor quality and productivity of the polysilicon.
The present invention provides a fluidized bed reactor for producing particulate polysilicon capable of improving productivity and increasing production scale while solving the conventional problems (unevenness of temperature in the reactor, contamination of polysilicon, etc.) due to the heating method of the reactor .
According to the present invention,
A
And a
The
The
The
According to the present invention, the
The fluidized bed reactor for producing the particulate polysilicon includes a seed supply unit for supplying a silicon seed to an inner space of the
The fluidized bed reactor for producing a particulate polysilicon may include an etching gas injection unit disposed on one side wall of the
The fluidized bed reactor for producing particulate polysilicon according to the present invention solves the conventional problems due to the heating method of the reactor (unevenness of the temperature in the reactor depending on the external heating system, contamination of the polysilicon with the internal heating system and instability of the process operation) . Furthermore, the reactor according to the present invention can provide a uniform heating environment even when expansion of the reactor is required to increase the production scale, which is advantageous for improving the productivity and increasing the production scale.
1 is a cross-sectional view schematically showing the structure of a conventional fluidized bed reactor for producing polysilicon.
2 is a cross-sectional view schematically showing the structure of a fluidized bed reactor for producing polysilicon according to an embodiment of the present invention.
3 and 4 are perspective views schematically showing a structure of a fluidized bed reactor for producing polysilicon according to an embodiment of the present invention.
Hereinafter, a fluidized bed reactor for producing a particulate polysilicon according to an embodiment of the present invention will be described in detail.
Prior to that, unless explicitly stated throughout the description, the terminology is merely to refer to any embodiment, and is not intended to limit the invention.
And, the singular forms used in the specification include plural forms unless the phrases expressly mean the opposite. Also, as used herein, the term " comprises " embodies certain features, areas, integers, steps, operations, elements and / or components, It does not exclude the existence or addition of a group.
And, terms including ordinals such as "first" or "second" in the present specification can be used to describe various elements, but the elements are not limited by the terms. The term including the ordinal number is used only for the purpose of distinguishing one element from another. For example, without departing from the scope of the present invention, the first component may also be referred to as a second component, and similarly, the second component may also be referred to as a first component.
On the other hand, according to the study of the present inventors, in a fluidized bed reactor for producing a particulate polysilicon, when the fluidized bed formed in the lower part of the reaction chamber is divided into a plurality of partition walls and each of the divided areas is heated externally, It is possible to increase the productivity of the polysilicon. Through the improved heating method, unevenness of the temperature in the reactor according to the conventional external heating method and pollution of the polysilicon according to the conventional internal heating method and instability of the process operation can be easily solved. Further, the improved heating system provided by the present invention enables the achievement of equal heating efficiency by increasing the number of divided regions even when expansion of the reactor scale is required to increase the production scale. Accordingly, the reactor of the present invention, to which such an improved heating system is applied, has an advantage of being able to improve productivity and advantageously increase the production scale.
According to one embodiment of the invention,
A
And a
The
The
The
Referring to FIG. 2, the fluidized bed reactor according to the present invention includes a
The
The
The
The
The
Particularly, the
Specifically, the
The
As described above, the fluidized bed reactor has a plurality of reaction spaces which are individually heated, so that uniform heating of the reaction space is possible as compared with the external heating type reactor for one reaction space as shown in FIG. 1 (a) . The improved heating system can adjust the number of
The fluidized bed reactor for producing the particulate polysilicon includes a seed supply unit for supplying a silicon seed to the inner space of the
Here, the source gas supply unit for supplying the silicon-containing source gas into the
The fluidized bed reactor for producing a particulate polysilicon may include an etching gas injection unit disposed on one side wall of the
Each of the parts constituting the fluidized bed reactor described above may be made of a metal material such as carbon steel, stainless steel or other alloy steel. The inside of each part may be formed with a protective film made of a material such as metal, organic polymer, or ceramic. In addition, a common member such as a gasket, a sealing member, or the like may be applied to each portion where the respective portions are connected.
The production of the particulate polysilicon using the fluidized bed reactor may include supplying fluidized gas to the lower end of the fluidized bed reactor filled with the silicon seed particles to form a fluidized bed of the silicon seed particles; Supplying a silicon-containing material gas to the fluidized bed to deposit silicon on the surface of the silicon seed particle in contact with the material gas; And injecting an etching gas through one side wall of the fluidized bed reactor.
In the fluidized bed formation step of the silicon seed, the silicon seed can be prepared by pulverizing and classifying a high purity polysilicon mass. The particle diameter of the silicon seed may be determined in a range suitable for fluidization of the particles such as a minimum fluidization speed and is preferably 10 to 500 占 퐉 or 100 to 500 占 퐉 or 100 to 350 占 퐉 or 150 to 350 占 퐉 or 150 To 300 [mu] m.
The prepared silicon seed is supplied in an appropriate amount to the reaction chamber of the fluidized bed reactor, and the supplied silicon seed is supported by the gas distributor. When fluidized gas is supplied to the lower end of the fluidized bed reactor, a fluidized bed of the silicon seed is formed. Here, as the fluidizing gas, a conventional one may be used, and hydrogen, nitrogen, argon, helium, or a mixed gas thereof may be used as a non-limiting example. At this time, the charging amount of the fluidizing gas may be determined in consideration of the particle diameter of the silicon seed, the minimum fluidization speed, and the like, and may be adjusted within a range from 1 to 10 times the minimum fluidization speed.
The fluidized bed of the silicon seed can be formed simultaneously with heating or before and after heating. Through heating of the fluidized bed, the temperature of the silicon seed rises to a temperature at which silicon can be deposited on its surface. Here, the heating temperature of the fluidized bed may be adjusted according to the composition of the silicon-containing source gas, and preferably 600 to 800 ° C. And, the heating of the fluidized bed can be carried out under atmospheric pressure or higher pressure conditions (pressure of 1 to 10 bar as a non-limitative example).
On the other hand, in the step of supplying silicon-containing source gas to deposit silicon,
The silicon-containing source gas may include at least one compound selected from the group consisting of monosilane (SiH 4 ), silicate silicate (SiH 2 Cl 2 ), trichlorosilane (SiHCl 3 ), and tetrachlorosilane (SiCl 4 ) ; Considering the efficiency of the precipitation reaction, monosilane gas can be preferably used. The silicon-containing source gas may further contain at least one component selected from the group consisting of hydrogen, nitrogen, argon, and helium, if necessary.
The silicon-containing source gas supplied to the fluidized bed is pyrolyzed at the surface of the silicon seed (for example, SiH 4 ↔ Si + 2H 2 ), and as a result, silicon is precipitated on the surface of the silicon seed.
Due to the precipitation of silicon, the silicon seed gradually decreases in fluidity as the particle size gradually increases, and gradually sinks to the lower portion of the fluidized bed. By observing the state of the particles sinking to the bottom of the fluidized bed, the appropriate size of the polysilicon particles can be recovered to the outside of the reactor. That is, the manufacturing method of the embodiment may further include discharging the particulate polysilicon formed by the precipitation of the silicon. Then, a new silicon seed is filled in the reactor, and the above-described processes are repeated to obtain the particulate polysilicon.
Here, the pyrolysis of the silicon-containing source gas and the deposition of silicon can be classified into two detailed reactions as follows.
(Formula 1) SiH 4? SiH 2 + H 2
(Formula 2) SiH 2 ? Si + H 2
Silane (SiH 2 ) generated in a heterogeneous reaction with silicon-containing source gas and silicon seed is highly reactive and is mostly deposited on the surface of silicon seed and pyrolyzed to precipitate silicon.
However, the silane (SiH 2 ) not in contact with the silicon seed can be obtained by a homogeneous reaction with the monosilane (SiH 4 ) contained in the silicon-containing source gas, as shown in the following formulas 3 to 5, Si n +1 H 2n +4 , n is an integer of 1 or more).
(Formula 3) SiH 4 + SiH 2 ↔ Si 2 H 6
(Formula 4) Si 2 H 6 + SiH 2 ↔ Si 3 H 8
(Formula 5) Si 3 H 8 + SiH 2 ↔ Si 4 H 10
...
(Formula 6) Si n H 2n + 2 + SiH 2 ↔ Si n +1 H 2n +4
The silicon fine powder is mainly formed in a region where no solid phase is present, that is, in a bubble phase or an upper portion of the fluidized bed, and is formed when supersaturation or pressure increases due to a high concentration of silicon- .
However, the silicon fine powder is not substantially involved in the growth of the silicon seed. That is, since the reaction rate of the silane compound (Si n H 2n +2 ) is faster than the rate of the decomposition reaction, the silicon fine powder (Si n +1 H 2n +4 ) is decomposed in the uniform reaction, . In the non-uniform reaction in which the silicon fine powder can come into contact with the silicon seed, the silicon fine powder is deposited on the silicon seed by a scavenging effect, but the amount is only about 10% of the total silicon fine powder.
The silicon fine powder is a crystalline silicon particle having a particle diameter of several to several tens of micrometers. When mixed with a silicon seed, the silicon fine powder adversely affects the flow characteristics of the silicon seed and is agglomerated and immersed in the reactor, A fouling phenomenon may be induced.
In addition, when the silicon fine powder is deposited on the silicon seed by the cleaning effect in the non-uniform reaction system, the surface of the silicon seed becomes non-uniform. In such a non-uniform surface or a void formed by the silicon seed, Hydrogen gas remains. When polysilicon particles having residual hydrogen gas are used in the process of producing an ingot, defects due to the generation of bubbles are generated during the formation of the silicon single crystal by the Czochralski method, which may adversely affect the quality of the silicon wafer.
Therefore, in order to ensure stable operation and to produce a high-quality polysilicon, it is required to remove the silicon fine powder. In order to solve the problems caused by the silicon fine powder, various methods such as a method of putting a quenching gas on the upper part of the fluidized bed, a method of lowering the silicon concentration of the raw material gas, a post- For example, a heat treatment at a temperature of 1000 DEG C or higher or chemical etching, etc.), and the like have been proposed. However, the methods proposed so far have limitations in that the production cost is increased or the process is complicated and the productivity is lowered.
Further, in order to remove the silicon deposits deposited on the wall surface of the fluidized bed reactor, a method has been proposed in which the introduction of the silicon-containing source gas is stopped and the etching gas is introduced through the lower end of the reactor while the polysilicon particles are recovered. However, the silicon deposit is a by-product which is grown by deposition of the silicon-containing source gas on the wall surface of the reactor, and the generation mechanism is different from that of the silicon derivative formed in the reaction region. Therefore, this method can not effectively remove the silicon fine particles formed in the reaction zone of the fluidized bed reactor. Further, in the above method, after the completion of the silicon precipitation step, the post-treatment step is separately performed in a state in which the inside of the reactor is empty, so continuous operation is impossible and thus it is difficult to apply to the mass production of polysilicon.
According to the present invention, as the etching gas is injected through one side wall of the fluidized bed reactor separately from the supply of the silicon-containing source gas, the silicon fine particles can be removed simultaneously with the precipitation of silicon to the silicon seed Do. That is, unlike the conventional methods in which the supply of the silicon-containing source gas must be stopped during the introduction of the etching gas, the method using the reactor as described above is advantageous in that the introduction of the etching gas does not hinder the silicon deposition efficiency or fluidity, The etching gas can be injected even in a state where the etching gas is being injected.
Further, it is possible to inject the etching gas at a required concentration even in the upper portion of the fluidized bed as well as the inside of the fluidized bed, thereby enabling a more efficient process operation. Furthermore, according to this method, since the etching gas is injected through one side wall of the fluidized bed reactor, corrosion of the gas distributor provided at the lower end of the fluidized bed reactor can be prevented.
In the present invention, the etching gas may be a compound capable of forming a silane-type compound by reacting with the silicon fine powder (Si n +1 H 2n +4 , where n is an integer of 1 or more), preferably hydrogen chloride (HCl), chlorine (Cl 2 ), or a mixed gas thereof. For example, when hydrogen chloride is used as the etching gas, the silicon fine powder may be reduced in size or removed by the following reaction.
(Formula 7) Si + 3HCl? SiHCl 3 + H 2
(Equation 8) Si + 4HCl → SiCl 4 + 2H 2
(Equation 9) Si + 2HCl → SiH 2 Cl 2
(Formula 10) Si + H 2 + HCl → SiH 3 Cl
In the above formulas 7 to 10, the reactions of the formulas 7 and 8 mainly occur. Among them, the reaction of Equation 7 is a strong exothermic reaction in which trichlorosilane (SiHCl 3 ) is formed. Therefore, the reaction takes place mainly at 300 ° C or lower, and the reaction of Equation 8 can occur at 300 ° C or higher. The reaction of the equation (7) mainly takes place at the upper part of the fluidized bed, and the reaction of the equation (8) can occur mainly inside the fluidized bed.
Therefore, in the present invention, the etching gas is introduced into the fluidized bed of the silicon seed, the upper part of the fluidized bed, or the upper part of the fluidized bed and the upper part of the fluidized bed through at least one injection nozzle provided on one side wall of the fluidized bed reactor Can be sprayed. The effect of the etching gas injection can be maximized by controlling the injection position of the etching gas through the one side wall of the fluidized bed reactor or by controlling the amount of the etching gas injected at each position.
Here, the injection timing of the etching gas may be determined according to the progress of the silicon deposition step. That is, since the fluidized bed reactor is normally closed, it is difficult to visually confirm the generation of silicon fine powder. However, in the process of fluidizing the silicon seed, a pressure difference (a pressure difference of about 0.5 bar, for example) is formed inside and on the fluidized bed of the silicon seed. The pressure difference is increased due to the formation of silicon fine powder Can be grasped. Therefore, the etching gas may be injected from a time point when the pressure difference tends to increase with the passage of the silicon deposition step.
The etching gas may be continuously injected through one side wall of the fluidized bed reactor while the silicon deposition reaction proceeds. However, since the etching gas and the silicon fine powder have good reactivity, it is advantageous in terms of efficiency of continuous operation to inject the etching gas periodically or intermittently.
The injection of the etching gas may be performed at a temperature of 300 to 800 DEG C or 500 to 700 DEG C and a pressure of 1 to 20 bar or 1 to 10 bar.
Further, according to the present invention, the etching gas may be injected so that chlorine is contained in an amount of 50 to 90 mol% based on silicon atoms contained in the silicon fine powder (Si n +1 H 2n +4 , n being an integer of 1 or more) . That is, it is preferable that the etching gas is injected so as to contain at least 50 mol% of chlorine with respect to the silicon atoms contained in the silicon fine powder so that the effect of the etching gas injection can be exhibited. However, when the etching gas is injected in an excessive amount, the growth of the silicon seed can be suppressed, and corrosion of the gas distributor can be caused. Therefore, it is preferable that the etching gas is injected so as to contain not more than 90 mol% of chlorine with respect to the silicon atoms contained in the silicon fine powder.
And, for example, if the etching gas is injected into the fluidized bed, the non-uniform deposition surface of the silicon seed can be more effectively removed, but if the concentration is excessive, the deposition rate of silicon to the silicon seed can be reduced . Therefore, it is preferable that the concentration of the etching gas is appropriately adjusted within the above-described range according to the position where the etching gas is injected (that is, the inside of the fluidized bed, the top of the fluidized bed, or the inside of the fluidized bed and the top of the fluidized bed) .
Meanwhile, the waste gas treatment step is a step of recovering and treating a silane gas (see the above formulas 7 to 10), hydrogen gas, and unreacted etching gas generated by the reaction of the silicon fine powder and the etching gas. That is, the waste gas recovered to the upper part of the fluidized bed reactor is difficult to be separated by the column because it contains hydrogen (b.p. about -252.degree. C.) and hydrogen chloride (b.p. Therefore, it is preferable to place an etching gas reduction reactor at the rear end of the fluidized bed reactor to convert the etching gas into a silane gas as shown in the following formulas 11 and 12.
(Formula 11) HCl + SiH 2 Cl 2 → SiHCl 3 + H 2
(Formula 12) HCl + SiHCl 3 ? SiCl 4 + H 2
And, the silane gas and the hydrogen gas can be separated through the column. The separated hydrogen gas can be recovered as high purity hydrogen gas through the adsorption column and recycled to the fluidized bed reactor. And, the separated silane gas can be regenerated through various processes, some of which can be recycled to the fluidized bed reactor.
100: Base plate
200: reaction chamber
210: first body part
215: reaction tube
217:
220: second body part
230: Head portion
Claims (3)
And a reaction chamber 200 having a first body part 210, a second body part 220 and a head part 230 which are sequentially connected to the base plate 100 to form one internal space and;
The first body part 210 includes a plurality of reaction tubes 215 spaced radially from the base plate 100 to provide a plurality of reaction spaces connected to the second body part 220, And a plurality of heating units (217) surrounding at least a part of an outer peripheral surface of the reaction tube (215), respectively;
The second body part 220 provides one reaction space connected to the reaction tube 215 of the first body part 210, respectively;
The head portion 230 seals the upper portion of the reaction chamber 200 and has a larger diameter than the second body portion 220.
The heating unit (217) surrounds the entire outer peripheral surface of the reaction tube (215).
The fluidized bed reactor for producing a particulate polysilicon,
A seed supply unit for supplying a silicon seed to the inner space of the reaction chamber 200,
A raw material gas supply unit for supplying a silicon-containing material gas to the internal space of the reaction chamber 200,
A fluidized gas supply unit connected to a lower portion of the base plate 100 to supply a gas for fluidizing the silicon seed,
A gas distributor for supporting the silicon seed and distributing the fluidized gas to the inner space of the reaction chamber 200, and a porous plate for partitioning the base plate 100 and the first body 210,
A polysilicon particle recovery unit for recovering polysilicon particles connected to a lower portion of the base plate 100,
And a fluidized-bed reactor for producing particulate polysilicon.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020150053976A KR20160123655A (en) | 2015-04-16 | 2015-04-16 | Fluidized bed reactor for manufacturing granular polycrystalline silicon |
| US15/549,759 US10518237B2 (en) | 2015-04-01 | 2016-03-24 | Gas distribution unit for fluidized bed reactor system, fluidized bed reactor system having the gas distribution unit, and method for preparing granular polycrystalline silicon using the fluidized bed reactor system |
| PCT/KR2016/002990 WO2016159568A1 (en) | 2015-04-01 | 2016-03-24 | Gas distribution device for fluidised-bed reactor system, fluidised-bed reactor system comprising gas distribution device, and method for preparing granular polysilicon using fluidised-bed reactor system |
| JP2017548414A JP6448816B2 (en) | 2015-04-01 | 2016-03-24 | Gas distributor for fluidized bed reactor system, fluidized bed reactor system including the gas distributor, and method for producing particulate polysilicon using the fluidized bed reactor system |
| CN201680019913.5A CN107438479B (en) | 2015-04-01 | 2016-03-24 | Gas distribution unit for fluidized bed reactor system, fluidized bed reactor system having the same, and method for preparing granular polycrystalline silicon using the fluidized bed reactor system |
| EP16773349.2A EP3278872B1 (en) | 2015-04-01 | 2016-03-24 | Method for preparing granular polysilicon using a fluidised-bed reactor system |
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| KR1020150053976A KR20160123655A (en) | 2015-04-16 | 2015-04-16 | Fluidized bed reactor for manufacturing granular polycrystalline silicon |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5382412A (en) | 1992-10-16 | 1995-01-17 | Korea Research Institute Of Chemical Technology | Fluidized bed reactor heated by microwaves |
| US6827786B2 (en) | 2000-12-26 | 2004-12-07 | Stephen M Lord | Machine for production of granular silicon |
-
2015
- 2015-04-16 KR KR1020150053976A patent/KR20160123655A/en not_active Application Discontinuation
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5382412A (en) | 1992-10-16 | 1995-01-17 | Korea Research Institute Of Chemical Technology | Fluidized bed reactor heated by microwaves |
| US6827786B2 (en) | 2000-12-26 | 2004-12-07 | Stephen M Lord | Machine for production of granular silicon |
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