JP2009167022A - Apparatus for producing silicon - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an apparatus for producing silicon capable of improving the efficiency of a reduction reaction so as to improve the yield of silicon and improving the separation recovery efficiency of the produced silicon and the produced gas as well, without causing complication in equipment configurations. <P>SOLUTION: The apparatus for producing silicon is equipped with a zinc feed pipe which communicates a silicon compound gas to a reaction vessel 10 and supplies zinc gas from a first zinc supply port 40a into the reaction vessel in ejecting to a second ejecting direction, a flow straightening member 20 which is installed in the reaction vessel and allows the silicon compound gas ejected from a silicon compound supply port in the first ejecting direction to flow from the upstream side to the downstream side in the reaction vessel while the zinc gas ejected from the first zinc supply port to the second zinc supply port is deviated, and a discharge pipe 10b which is installed at the downstream side of the flow straightening member in the reaction vessel and discharges a reaction product gas containing silicon outside the reaction vessel. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to a silicon manufacturing apparatus, and more particularly to a silicon manufacturing apparatus provided with a rectifying member that controls the flow of a raw material gas in a reaction vessel.

  In recent years, the production method of obtaining high purity silicon by reducing silicon tetrachloride with zinc by the so-called zinc reduction method is that the equipment is compact and consumes little energy, and high purity silicon of 6-nine or more can be obtained. Therefore, it has been attracting attention as a method for producing silicon for solar cells, for which demand is expected to increase rapidly in the future.

  In the silicon production technology using such a zinc reduction method, a reaction vessel and an evaporation tank that are maintained at a predetermined temperature are provided, and the temperature of the zinc gas gasified in the evaporation tank is controlled through a gas supply pipe. The thing of the structure supplied to a reaction furnace is proposed (refer patent documents 1 to 3).

Furthermore, in the silicon production technology using the zinc reduction method, a structure in which the seed silicon is separately supplied to the reactor to grow the produced silicon greatly in order to improve the separation efficiency from the reaction product gas and improve the yield. Have been proposed (see Patent Documents 4 and 5).
JP 2002-234719 A Japanese Patent Laid-Open No. 2004-210594 JP 2004-284935 A JP 2003-95633 A JP 2003-342016 A

  However, according to the study of the present inventors, in the first place, in the zinc reduction method, the molecular weight of zinc chloride is 136.4 with respect to the atomic weight of silicon of 28.1, and two molecules of chloride per one silicon atom. Since zinc is produced, that is, zinc chloride is produced at a yield of about 10 times the yield of silicon, silicon is improved while improving the separation and recovery efficiency of silicon and product gas by the reduction reaction. Although the establishment of a manufacturing technique for improving the yield of the metal is cited as an important issue, the silicon manufacturing technique using the zinc reduction method in Patent Documents 1 to 5 eliminates the complexity of the apparatus configuration. From the viewpoint of improving the efficiency of the reduction reaction for improving the yield of silicon and at the same time improving the separation and recovery efficiency of the produced silicon and the produced gas. It is believed that there is room for improvement.

  Specifically, according to further studies by the present inventors, in the configurations of Patent Documents 1 to 3, in order to further improve the reduction reaction efficiency, for example, the reaction from the evaporation tank without condensing gasified zinc It is necessary to adopt a configuration for supplying to the furnace. To this end, it is necessary to separately add a heater for heating the zinc gas supply unit from the evaporation tank to the reactor, and the apparatus configuration is complicated. It will become.

  In addition, in the configurations of Patent Documents 4 and 5, although it is intended to improve the yield of silicon while improving the separation efficiency between silicon and product gas, a seed crystal is separately supplied to the reactor. Therefore, it is difficult to recover the silicon deposited and deposited on the inner surface of the reaction vessel. There is a limit in improving the recovery rate.

  The present invention has been made in view of such circumstances, and improves the efficiency of the reduction reaction for improving the yield of silicon while eliminating the complexity of the apparatus configuration, and at the same time, separation of the generated silicon and the generated gas. An object of the present invention is to provide a silicon manufacturing apparatus capable of improving the recovery efficiency.

  In order to achieve the above object, in the first aspect, the present invention communicates with a reaction vessel and the reaction vessel, and allows silicon compound gas to flow into the reaction vessel from the silicon compound supply port in the first discharge direction. A silicon compound supply pipe that is supplied while being discharged, a zinc supply pipe that communicates with the reaction vessel and supplies zinc gas while being discharged from the first zinc supply port into the reaction vessel in the second discharge direction; Silicon provided in the reaction vessel and discharged from the silicon compound supply port in the first discharge direction while deflecting zinc gas discharged from the first zinc supply port in the second discharge direction A rectifying member that allows the compound gas to flow from the upstream side to the downstream side in the reaction vessel; and a reaction product gas that is provided on the downstream side of the rectification member in the reaction vessel and that contains silicon. A discharge pipe for output, a silicon manufacturing apparatus comprising a.

  Moreover, in addition to this 1st aspect, this invention is a cylindrical member with which the said reaction container is a cylindrical member, and the said rectification | straightening member is accommodated in the said cylindrical member of the said reaction container, and has a surrounding wall. It is assumed that there is a second aspect.

  Moreover, this invention makes it the 3rd aspect that the said cylindrical member which comprises the said baffle member is a cylindrical member in addition to this 2nd aspect.

  Moreover, in addition to this 2nd aspect, this invention is that the said cylindrical member which comprises the said rectification | straightening member is a hollow truncated cone member with a diameter decreasing toward the downstream from the upstream in the said reaction container. The fourth aspect is assumed.

  Further, in addition to any one of the second to fourth aspects, the present invention provides a fifth aspect in which the silicon compound supply port is disposed facing the region surrounded by the peripheral wall of the rectifying member. And

  In addition to any one of the second to fourth aspects of the present invention, the silicon compound supply port is arranged in the region surrounded by the peripheral wall of the rectifying member as a sixth aspect. To do.

  Moreover, this invention makes it a 7th aspect to arrange | position the said 1st zinc supply port corresponding to the said surrounding wall of the said baffle member in addition to the situation in any one of this 2nd to 6th.

  Further, in addition to the seventh aspect, the present invention has an eighth aspect in which the first zinc supply port is disposed to face an upstream portion of the peripheral wall of the rectifying member.

  Further, according to the present invention, in addition to any one of the second to sixth aspects, the zinc supply pipe is further arranged on the upstream side in the reaction vessel with respect to the first zinc supply port. A ninth aspect is that the second zinc supply port is disposed upstream of the silicon compound supply port.

  Further, according to the present invention, in addition to any one of the second to sixth aspects, the rectifying member is arranged on the upstream side in the reaction vessel and the first rectifying member arranged on the downstream side in the reaction vessel. And the zinc supply pipe further has a second zinc supply port arranged on the upstream side of the reaction vessel with respect to the first zinc supply port, The first zinc supply port is disposed corresponding to the peripheral wall of the first rectifying member, and the second zinc supply port is disposed corresponding to the peripheral wall of the second rectifying member. The tenth aspect is assumed.

  According to the present invention, in addition to the tenth aspect, the silicon compound supply port is disposed on the first silicon compound supply port disposed on the downstream side in the reaction vessel and on the upstream side in the reaction vessel. A second silicon compound port, wherein the first silicon compound supply port is disposed in the region surrounded by the peripheral wall of the first rectifying member, and the second silicon compound supply port is In the eleventh aspect, the second straightening member is disposed in the region surrounded by the peripheral wall.

  According to the first aspect of the present invention, the first discharge from the silicon compound supply port is performed while deflecting the zinc gas provided in the reaction vessel and discharged from the first zinc supply port in the second discharge direction. By providing a rectifying member that allows the silicon compound gas discharged in the direction to flow from the upstream side to the downstream side in the reaction vessel, the flow of the silicon compound gas is not disturbed unnecessarily. Zinc gas can be flowed into the reaction vessel, reducing the complexity of the equipment configuration, improving the efficiency of the reduction reaction to improve the yield of silicon, and simultaneously separating and recovering the generated silicon and the generated gas Efficiency can also be improved.

  According to the second aspect of the present invention, the rectifying member is a cylindrical member that is accommodated in the cylindrical member of the reaction vessel and has a peripheral wall, so that the second zinc gas can be more reliably supplied from the first zinc supply port. The silicon compound gas discharged in the first discharge direction from the silicon compound supply port is allowed to flow from the upstream side to the downstream side in the reaction vessel while deflecting the zinc gas discharged in the discharge direction. it can.

  According to the third aspect of the present invention, the rectifying member is a cylindrical member, so that the zinc gas discharged from the first zinc supply port in the second discharge direction can be more reliably deflected with a simple configuration. However, the silicon compound gas discharged from the silicon compound supply port in the first discharge direction can be allowed to flow from the upstream side to the downstream side in the reaction vessel.

  According to the fourth aspect of the present invention, the flow of the silicon compound gas passing through the flow straightening member is obtained by making the flow straightening member a hollow truncated cone member whose diameter decreases from the upstream side toward the downstream side in the reaction vessel. As a result, a larger pressure gradient is generated so that the flow of the deflected zinc gas is directed from the upstream to the downstream while increasing the flow velocity, thereby making the silicon compound gas and the zinc gas more smooth and reliable. Can be made to flow downstream to be combined, and a reduction reaction between the silicon compound gas and the zinc gas can be generated more efficiently.

  According to the fifth aspect of the present invention, the silicon compound supply port is disposed facing the region surrounded by the peripheral wall of the rectifying member, so that the silicon compound gas is surely surrounded by the peripheral wall of the rectifying member. The area can be passed primarily.

  According to the sixth aspect of the present invention, the silicon compound supply port is disposed in the region surrounded by the peripheral wall of the rectifying member, so that the silicon compound is not affected unnecessarily by the flow of zinc gas. The gas can be mainly passed through the region surrounded by the peripheral wall of the rectifying member more reliably.

  According to the seventh aspect of the present invention, the first zinc supply port is disposed corresponding to the peripheral wall of the rectifying member, so that the zinc can be reliably produced without unnecessarily affecting the flow of the silicon compound gas. The gas flow can be deflected.

  According to the eighth aspect of the present invention, the first zinc supply port is disposed to face the upstream portion of the peripheral wall of the rectifying member, so that the flow of the silicon compound gas is not adversely affected. By applying a pressure due to the pressure gradient generated around the peripheral wall to the flow of the zinc gas to be deflected, the zinc gas can flow more reliably from the upstream side to the downstream side to be merged with the flow of the silicon compound gas.

  According to the ninth aspect of the present invention, the zinc supply pipe further has a second zinc supply port arranged on the upstream side in the reaction vessel with respect to the first zinc supply port. By disposing the zinc supply port on the upstream side of the silicon compound supply port, the flow of the zinc compound discharged from the second zinc supply port does not unnecessarily affect the flow of the silicon compound gas. A sufficient amount of zinc gas from upstream to downstream can be rapidly supplied into the reaction vessel.

  According to a tenth aspect of the present invention, the rectifying member includes a first rectifying member disposed on the downstream side in the reaction vessel, and a second rectifying member disposed on the upstream side in the reaction vessel, The zinc supply pipe further has a second zinc supply port disposed upstream of the first zinc supply port in the reaction vessel, and the first zinc supply port is connected to the first rectifying member. When the second zinc supply port is disposed corresponding to the peripheral wall and is disposed corresponding to the peripheral wall of the second rectifying member, a plurality of zinc supply ports are provided to supply a sufficient amount of zinc gas. Even so, the flow of zinc gas can be reliably deflected.

  According to the eleventh aspect of the present invention, the silicon compound supply port has a first silicon compound supply port arranged on the downstream side in the reaction vessel and a second silicon compound supply port arranged on the upstream side in the reaction vessel. The first silicon compound supply port is disposed in a region surrounded by the peripheral wall of the first rectifying member, and the second silicon compound supply port is surrounded by the peripheral wall of the second rectifying member. By disposing in the closed area, a plurality of silicon compound supply ports can be provided to rapidly supply a sufficient amount of silicon compound gas from upstream to downstream into the reaction vessel, and the silicon compound gas can be reliably supplied to the rectifying member. The area surrounded by the peripheral wall can be passed mainly.

  Hereinafter, a silicon manufacturing apparatus according to an embodiment of the present invention will be described in detail with reference to the drawings as appropriate. In the figure, the x-axis, y-axis, and z-axis form a three-axis orthogonal coordinate system, and the z-axis is a vertical direction in which gravity works in the negative direction. In addition, the positive direction side of the z-axis may be referred to as the downstream side, and the negative direction side of the z-axis may be referred to as the upstream side as appropriate.

(First embodiment)
First, the silicon manufacturing apparatus according to the first embodiment of the present invention will be described in detail with reference to FIGS.

  FIG. 1 is a schematic partial cross-sectional view of a silicon manufacturing apparatus in the present embodiment. 2 is an enlarged sectional view taken along line AA in FIG. 1, and FIG. 3 is an enlarged sectional view taken along line BB in FIG.

  As shown in FIG. 1, the silicon manufacturing apparatus 1 in this embodiment includes a reaction vessel 10 in which a silicon compound contained in a silicon compound gas and zinc contained in a zinc gas cause a reduction reaction. The reaction vessel 10 is made of quartz glass, and is a cylindrical member that houses a rectifying member 20 therein and has a main body portion 10a that forms a peripheral wall around a central axis C parallel to the z axis. A silicon compound supply pipe 30 for supplying a silicon compound gas is connected to the upstream end of the main body 10a, and the downstream end of the main body 10a of the reaction vessel 10 is generated by a reduction reaction. A discharge pipe 10b for discharging the produced product such as silicon to the outside is communicated. In addition, the main body 10a is connected to a first zinc supply pipe 40 and a second zinc supply pipe 50 that both supply zinc gas therein, and a sufficient amount of zinc gas is contained in the reaction vessel 10. Is supplied quickly.

  The rectifying member 20 is made of ceramic, and is a cylindrical member that is disposed coaxially with the central axis C of the reaction vessel 10 and has a peripheral wall 20a surrounding the axis. The rectifying member 20 is supported by the main body 10 a of the reaction vessel 10 by the support member M. The coaxiality between the central axis of the rectifying member 20 and the central axis C of the reaction vessel 10 is not strict. That is, the silicon compound gas can flow at a predetermined flow rate from the upstream side to the downstream side of the main body portion 10a through the internal region surrounded by the peripheral wall 20a, and the zinc gas can be supplied to the peripheral wall 20a. If the arrangement can be deflected, the central axis of the rectifying member 20 does not necessarily have to be arranged coaxially with the central axis C of the reaction vessel 10. It doesn't matter.

  The silicon compound supply pipe 30 is made of quartz glass, extends coaxially with the central axis C of the reaction vessel 10 in the main body portion 10a of the reaction vessel 10, and has a silicon compound supply port 30a in the main body portion 10a. From the silicon compound supply port 30a, silicon compound gas is discharged into the main body 10a along the silicon compound discharge direction S1 which is the direction of the central axis C. The silicon compound supply pipe 30 communicates with the silicon compound introduction pipe 34 via the connecting member 32 outside the main body 10 a of the reaction vessel 10. The silicon compound introduction pipe 34 is connected to a silicon compound gas source (not shown). Such a silicon compound gas source may store not only the silicon compound gas but also the carrier gas so as to increase the discharge pressure of the silicon compound gas discharged from the silicon compound supply port 30a. May be introduced into the silicon compound supply pipe 30 or the silicon compound introduction pipe 34 by providing a separate carrier gas source. The silicon compound is typically silicon tetrachloride. The silicon compound discharge direction S1 with respect to the silicon compound gas is typically a direction parallel to the central axis C, but is not limited, and can flow the silicon compound gas from the upstream side to the downstream side. For example, the direction may intersect the central axis C.

  The first zinc supply pipe 40 and the second zinc supply pipe 50 are both made of quartz glass and are arranged symmetrically with respect to the central axis C of the reaction vessel 10 so that the first zinc supply tube 40 and the second zinc supply tube 50 are arranged with respect to the peripheral wall of the main body 10a of the reaction vessel 10. Thus, the first zinc supply port 40a and the second zinc supply port 50a communicate with each other about the central axis C in an axisymmetric manner. The first zinc supply port 40a is arranged on the upstream side of the silicon compound supply port 30a with respect to the peripheral wall of the main body 10a, and the second zinc supply port 50a is on the downstream side of the silicon compound supply port 30a. The main body 10a is disposed with respect to the peripheral wall. Further, zinc gas is discharged from the first zinc supply port 40a along the first zinc supply direction S2, which is a direction orthogonal to the central axis C, and from the second zinc supply port 50a, zinc gas is discharged. Are discharged along a second zinc discharge direction S3 that is orthogonal to the central axis C and is opposite to the first zinc discharge direction S2. In this example, two zinc supply pipes each having one zinc supply port are provided on the axial object with different axial positions, but if the amount of zinc gas can be sufficiently secured, the arrangement and number Is not limited, for example, one zinc supply pipe may have a plurality of zinc supply ports, or a plurality of zinc supply ports are arranged at appropriate intervals in the same axial position. It doesn't matter. In addition, the first zinc supply direction S2 and the second zinc discharge direction S3 related to the zinc gas are typically orthogonal to the silicon compound discharge direction S1 related to the silicon compound gas, but are limited. Instead, the direction may be the direction from the upstream side to the downstream side while facing the silicon compound discharge direction S1.

  The first zinc supply pipe 40 has an extending part 40b extending in parallel with the central axis C of the reaction vessel 10 from the first zinc supply port 40a, and the extending part 40b is connected via a connecting member 42. , Communicated with the first zinc introduction pipe 44. The second zinc supply pipe 50 has an extending portion 50 b extending from the second zinc supply port 50 a in parallel to the central axis C of the reaction vessel 10, and the extending portion 50 b is connected via a connecting member 52. , Communicated with the second zinc introduction pipe 54. The first zinc introduction pipe 44 and the second zinc introduction pipe 54 are each connected to a molten zinc source (not shown). Further, in order to increase the discharge pressure of the zinc gas discharged from the first zinc supply port 40a and the second zinc supply port 50a, a separate carrier gas source is provided, and the first zinc supply pipe 40 and the second zinc gas supply port 40a are provided. Each carrier gas may be introduced into the zinc supply pipe 50.

  Further, the periphery of the main body portion 10a forming the peripheral wall of the reaction vessel 10, the extended portion 40b of the first zinc supply pipe 40, and the extended portion 50b of the second zinc supply pipe 50 is cylindrical so as to surround them. A heating device 60 is provided. The heating device 60 has a boiling point (930 ° C.) or higher of molten zinc or solid zinc respectively supplied to the extending part 40b of the first zinc supply pipe 40 and the extending part 50b of the second zinc supply pipe 50. To generate zinc gas, and the silicon compound gas and zinc gas supplied into the main body 10a are heated to promote a reduction reaction therebetween.

  Here, the arrangement relationship between the rectifying member 20, the silicon compound supply pipe 30, the first zinc supply pipe 40, and the second zinc supply pipe 50, and the flow of the discharged silicon compound gas and zinc gas are described in detail. Explained.

  In the arrangement relationship between the rectifying member 20 and the silicon compound supply pipe 30, the silicon compound supply port 30a of the silicon compound supply pipe 30 is surrounded by the peripheral wall 20a of the rectification member 20, as shown in detail in FIGS. It is located on the upstream side of the rectifying member 20 so as to face the internal region. Here, the rectifying member 20 and the silicon compound supply pipe 30 are arranged coaxially with the central axis C of the reaction vessel 10, and the silicon compound gas is discharged from the silicon compound supply port 30a in the direction of the central axis C. Along the direction S1, the main body 10a of the reaction vessel 10 is discharged from the upstream side to the downstream side at a predetermined discharge pressure and flows so as to flow through the main body portion 10a and be discharged from the discharge pipe 10b. The silicon compound gas thus flowed flows with a predetermined flow velocity distribution from the upstream side to the downstream side of the main body 10a mainly through the internal region surrounded by the peripheral wall 20a of the rectifying member 20. Furthermore, due to the flow of the silicon compound gas discharged in this way and flowing from the upstream side to the downstream side, a pressure gradient in which the pressure decreases from the upstream side to the downstream side occurs in the main body portion 10a, for example, Even in the region between the peripheral wall 20a and the main body portion 10a facing it and the downstream region thereof, a pressure gradient is generated in which the pressure decreases from the upstream side toward the downstream side.

  In the arrangement relationship between the rectifying member 20 and the first zinc supply pipe 40, as shown in detail in FIGS. 2 and 3, the first zinc supply port 40a of the first zinc supply pipe 40 is connected to the rectifying member 20. Considering the pressure gradient from the upstream side to the downstream side in the region between the peripheral wall 20a and the region between the peripheral wall 20a and the main body 10a of the reaction vessel 10 facing the peripheral wall 20a and the downstream region, the first The zinc supply port 40a is disposed at a position closer to the upstream end 20c than the downstream end 20b of the peripheral wall 20a with respect to the peripheral wall 20a. With this configuration, the zinc gas is predetermined in the main body portion 10a of the reaction vessel 10 along the first zinc discharge direction S2 that is a direction orthogonal to the central axis C of the reaction vessel 10 from the first zinc supply port 40a. Since the discharged zinc gas is discharged at the discharge pressure of the rectifying member 20, the flow rate distribution of the silicon compound gas flowing at a predetermined flow rate from the upstream side toward the downstream side in the inner region surrounded by the peripheral wall 20a of the rectifying member 20 is substantially reduced. Without being affected by the surrounding wall 20a. Specifically, the discharged zinc gas is deflected upstream and downstream by the peripheral wall 20a in the cross section shown in FIG. 1, and around the central axis C so as to surround the peripheral wall 20a in the cross section shown in FIG. Is deflected clockwise and counterclockwise. Here, since the zinc supply port 40a is disposed at a position near the upstream end 20c with respect to the peripheral wall 20a, in the discharged zinc gas, the region between the peripheral wall 20a and the main body portion 10a facing the area or In the downstream region, the flow from the upstream side to the downstream side is mainly received by the pressure due to the pressure gradient from the upstream side to the downstream side. Thus, the zinc gas traveling from the upstream side to the downstream side passes through the internal region surrounded by the peripheral wall 20a of the rectifying member 20, and the silicon compound gas flowing at a predetermined flow rate from the upstream side to the downstream side. , Mainly at the downstream side of the rectifying member 20.

  In the arrangement relationship between the rectifying member 20 and the second zinc supply pipe 50, as shown in detail in FIGS. 2 and 3, the second zinc supply port 50a of the second zinc supply pipe 50 is connected to the silicon compound supply pipe. 30 is located opposite. Here, a predetermined amount of zinc gas enters the main body 10a of the reaction vessel 10 along the second zinc discharge direction S3 that is a direction orthogonal to the central axis C of the reaction vessel 10 from the second zinc supply port 50a. It is discharged at the discharge pressure. The discharged zinc gas is a pressure due to a pressure gradient in which the pressure decreases from the upstream side to the downstream side caused by the flow from the upstream side to the downstream side of the silicon compound gas discharged from the silicon compound supply port 30a. In response, the flow proceeds from the upstream side toward the downstream side. The zinc gas traveling from the upstream side to the downstream side as described above merges with the silicon compound gas discharged from the silicon compound supply port 30a, and mainly passes through the internal region surrounded by the peripheral wall 20a of the rectifying member 20. It flows downstream, and also joins with the zinc gas discharged from the first zinc supply port 40a and flowing mainly between the peripheral wall 20a and the main body portion 10a facing it.

  Therefore, the silicon compound gas and the zinc gas that are sequentially joined in this way are mixed diffusively downstream of the rectifying member 20 and cause a reduction reaction to produce silicon powder and zinc chloride that are aggregates of silicon particles. Further, the silicon powder and zinc chloride generated flow toward the discharge pipe 10b of the reaction vessel 10 on the downstream side, and the generated silicon powder and zinc chloride receive the discharge pressure due to the pressure in the main body 10a of the reaction vessel 10 and are discharged from the discharge pipe 10b. It is discharged out of the main body 10a. The silicon powder and zinc chloride discharged from the discharge pipe 10b are separated by a separation / recovery device (not shown), and silicon is selectively recovered.

  Next, a silicon manufacturing method using the silicon manufacturing apparatus in the present embodiment having the above configuration will be described in detail. The series of steps in the manufacturing method are not shown in the figure, but are controlled in accordance with a predetermined program while referring to detection values, databases, and the like obtained from detectors that require a controller. Of course, manual processes may be mixed if necessary.

  First, the heating device 60 heats the reaction vessel 10, the extended portion 40 b of the first zinc supply tube 40, and the extended portion 50 b of the second zinc supply tube 50, while heating the first zinc supply tube 40 and the first zinc supply tube 40. Molten zinc or solid zinc is supplied to the second zinc supply pipe 50, and the molten zinc is heated to the boiling point or more in the extending portion 40b and the extending portion 50b to be gasified to generate zinc gas. The generated zinc gas flows from the first zinc supply port 40a along the first zinc discharge direction S2, which is a direction orthogonal to the central axis C of the reaction vessel 10, and from the second zinc supply port 50a to the reaction vessel. 10 is discharged into the main body 10a of the reaction vessel 10 at a predetermined discharge pressure along a second zinc discharge direction S3 which is a direction orthogonal to the central axis C of the ten.

  At the same time, the silicon compound gas has a predetermined discharge pressure from the upstream side to the downstream side in the main body 10a of the reaction vessel 10 along the silicon compound discharge direction S1 that is the direction of the central axis C from the silicon compound supply port 30a. Is discharged. The silicon compound gas discharged in this way flows with a predetermined flow velocity distribution from the upstream side to the downstream side of the main body 10a mainly through the internal region surrounded by the peripheral wall 20a of the rectifying member 20. In 10a, a pressure gradient is generated in which the pressure decreases from the upstream side toward the downstream side, and the region between the peripheral wall 20a and the main body portion 10a opposed to the peripheral wall 20a and the downstream region are also downstream from the upstream side. A pressure gradient is created in which the pressure decreases towards the.

  Here, the zinc gas discharged into the main body portion 10a of the reaction vessel 10 from the second zinc supply port 50a on the upstream side is upstream due to the pressure gradient generated from the upstream side to the downstream side of the main body portion 10a. It becomes the flow which goes to the downstream side. The zinc gas traveling from the upstream side to the downstream side as described above merges with the silicon compound gas discharged from the silicon compound supply port 30a, and mainly passes through the internal region surrounded by the peripheral wall 20a of the rectifying member 20. Flows downstream.

  Furthermore, the zinc gas discharged into the main body 10a of the reaction vessel 10 from the first zinc supply port 40a on the downstream side is directed from the upstream side toward the downstream side in the internal region surrounded by the peripheral wall 20a of the rectifying member 20. Without substantially affecting the flow velocity distribution of the silicon compound gas flowing at a predetermined flow velocity, while flowing around the circumferential wall 20a around the z axis, between the upstream side and the downstream side, such as between the circumferential wall 20a and the body portion 10a facing it. In response to the pressure gradient due to the pressure, the flow from the upstream side toward the downstream side is mainly deflected by the peripheral wall 20a.

  Thus, the silicon compound gas that flows at a predetermined flow rate from the upstream side to the downstream side mainly through the internal region surrounded by the peripheral wall 20a of the rectifying member 20, mainly between the peripheral wall 20a and the main body portion 10a facing it. The zinc gas that flows from the upstream side to the downstream side via the air and the zinc gas that flows mainly from the upstream side to the downstream side via the internal region surrounded by the peripheral wall 20a of the rectifying member 20 are mainly the rectifying member. 20, while being mixed and diffusively mixed, a reduction reaction is caused to generate silicon powder and zinc chloride, which are aggregates of silicon particles, and further toward the discharge pipe 10 b of the reaction vessel 10 on the downstream side. And flow.

  The silicon powder and zinc chloride thus generated are discharged from the discharge pipe 10b to the outside of the main body 10a under the discharge pressure due to the pressure in the main body 10a of the reaction vessel 10, and are discharged by an appropriate separation and recovery device. The silicon can be selectively recovered to obtain silicon, and the zinc chloride is further sent to a reprocessing apparatus or the like (not shown).

  Therefore, according to the above configuration, while deflecting the zinc gas provided in the reaction vessel and discharged from the first zinc supply port in the second discharge direction, from the silicon compound supply port in the first discharge direction. A silicon compound gas that substantially regulates the flow rate of the gas flow in the reaction vessel with a simple configuration of providing a flow regulating member that allows the discharged silicon compound gas to flow from the upstream side toward the downstream side in the reaction vessel. Zinc gas can be flowed into the reaction vessel without unnecessarily affecting the flow of the gas, improving the efficiency of the reduction reaction to improve the yield of silicon while eliminating the complexity of the apparatus configuration, At the same time, the separation and recovery efficiency between the generated silicon and the generated gas can be improved.

  Further, the rectifying member is a cylindrical member that is accommodated in the cylindrical member of the reaction vessel and has a peripheral wall, so that the zinc gas discharged more reliably from the first zinc supply port in the second discharge direction. The silicon compound gas discharged from the silicon compound supply port in the first discharge direction can be allowed to flow from the upstream side to the downstream side in the reaction vessel. More specifically, by using a cylindrical member as the rectifying member, the silicon compound is supplied while deflecting the zinc gas discharged in the second discharge direction from the first zinc supply port more reliably with a simple configuration. The silicon compound gas discharged from the mouth in the first discharge direction can be allowed to flow from the upstream side toward the downstream side in the reaction vessel without being affected unnecessarily.

  In addition, since the silicon compound supply port faces the region surrounded by the peripheral wall of the rectifying member, the silicon compound gas can be surely passed mainly through the region surrounded by the peripheral wall of the rectifying member.

  In addition, since the first zinc supply port is arranged corresponding to the peripheral wall of the rectifying member, the flow of zinc gas can be reliably deflected. More specifically, the first zinc supply port is disposed opposite to the upstream side portion of the peripheral wall of the rectifying member, so that the pressure due to the pressure gradient generated around the peripheral wall is generated in the flow of the deflected zinc gas. By acting, the zinc gas can flow more reliably from the upstream side to the downstream side, and can be merged with the flow of the silicon compound gas.

  The zinc supply pipe further has a second zinc supply port arranged on the upstream side of the reaction vessel with respect to the first zinc supply port, and the second zinc supply port is configured to supply a silicon compound. By disposing upstream of the port, the flow of zinc gas discharged from the second zinc supply port does not unnecessarily affect the flow of the silicon compound gas and extends from upstream to downstream in the reaction vessel. A sufficient amount of zinc gas can be supplied quickly.

(Second Embodiment)
Next, a silicon manufacturing apparatus according to the second embodiment of the present invention will be described in detail with reference to FIGS.

  FIG. 4 is a schematic partial cross-sectional view of the silicon manufacturing apparatus in the present embodiment. FIG. 5 is an enlarged cross-sectional view taken along line CC in FIG. 4, and FIG. 6 is an enlarged cross-sectional view taken along line DD in FIG.

  As shown in FIGS. 4 to 6, the silicon manufacturing apparatus 2 of the present embodiment is different from the silicon manufacturing apparatus 1 of the first embodiment in that the rectifying member 20 is changed to a rectifying member 70. And the remaining configuration is the same. Therefore, in the present embodiment, description will be made by paying attention to such differences, and the same components will be denoted by the same reference numerals, and description thereof will be simplified or omitted as appropriate.

  The rectifying member 70 of the present embodiment is made of quartz or ceramic, is disposed coaxially with the central axis C of the reaction vessel 10, and is supported by the main body 10 a of the reaction vessel 10 by the support member M. 1, the peripheral wall 70 a surrounding the axis is a hollow truncated cone member having a truncated cone shape whose diameter decreases from the upstream side to the downstream side in the reaction vessel 10. Is different. Note that the first zinc supply port 40a is disposed closer to the upstream end 70c than the downstream end 70b of the peripheral wall 70a with respect to the peripheral wall 70a, as in the first embodiment. is there.

  By adopting the hollow truncated cone member as the rectifying member 70 in this way, the upstream side into the main body portion 10a of the reaction vessel 10 along the silicon compound discharge direction S1 that is the direction of the central axis C from the silicon compound supply port 30a. When the silicon compound gas discharged at a predetermined discharge pressure from the downstream to the downstream flows mainly from the upstream side to the downstream side of the main body 10a through the internal region surrounded by the peripheral wall 70a, the upstream side The flow is restricted by the peripheral wall 70a having a truncated cone shape whose diameter decreases from the side toward the downstream side, and the flow rate of the silicon compound gas increases on the downstream side of the rectifying member 70.

  Further, due to the flow of the silicon compound gas thus discharged, the pressure decreases from the upstream side to the downstream side in the region between the peripheral wall 70a and the main body portion 10a facing the peripheral wall 70a and the downstream region thereof. The pressure gradient also increases. Here, the first zinc supply port 40a discharges at a predetermined discharge pressure into the main body portion 10a of the reaction vessel 10 along the first zinc discharge direction S4 which is a direction orthogonal to the central axis C of the reaction vessel 10. In the cross section shown in FIG. 4, the zinc gas is deflected upstream and downstream by the peripheral wall 70a, and in the cross section shown in FIG. 6, it rotates clockwise and counterclockwise around the central axis C so as to surround the peripheral wall 70a. However, in the discharged zinc gas, the pressure gradient from the upstream side to the downstream side between the peripheral wall 70a and the main body portion 10a facing it and in the downstream region becomes larger. The main flow is from the downstream side to the upstream side at a higher flow velocity under a large pressure. Further, since the zinc gas traveling from the downstream side to the upstream side flows along the circumferential wall 70a having a truncated cone shape whose diameter decreases from the upstream side to the downstream side in this way, the interior surrounded by the circumferential wall 70a. The silicon compound gas flowing at a predetermined flow rate from the upstream side to the downstream side via the region is more smoothly merged on the downstream side of the rectifying member 70.

  Therefore, also in the present embodiment, the silicon compound gas that flows at a predetermined flow rate from the upstream side to the downstream side mainly through the internal region surrounded by the peripheral wall 70a of the rectifying member 70, mainly the peripheral wall 70a and the main body facing it. Zinc gas flowing from the upstream side toward the downstream side via the portion 10a, and zinc gas flowing mainly from the upstream side toward the downstream side via the internal region surrounded by the peripheral wall 70a of the rectifying member 70 Is discharged from the discharge pipe 10b of the reaction vessel 10 on the further downstream side, while joining mainly on the downstream side of the rectifying member 70 to generate a reduction reaction to generate silicon powder and zinc chloride as an aggregate of silicon particles, Silicon can be selectively recovered to obtain silicon.

Therefore, according to the above configuration, the flow of the silicon compound gas passing through the flow straightening member is narrowed by making the flow straightening member a hollow truncated cone member whose diameter decreases from the upstream side to the downstream side in the reaction vessel. As a result, the flow rate of the zinc gas is increased and a pressure gradient is applied to the flow of the deflected zinc gas from upstream to downstream, so that the silicon compound gas and the zinc gas can flow more smoothly and reliably downstream. Thus, the reduction reaction between the silicon compound gas and the zinc gas can be generated more efficiently.
(Third embodiment)
Next, a silicon manufacturing apparatus according to the third embodiment of the present invention will be described in detail with reference to FIGS.

  FIG. 7 is a schematic partial cross-sectional view of the silicon manufacturing apparatus in the present embodiment. FIG. 8 is an enlarged cross-sectional view taken along line EE in FIG. 7, and reference numerals and the like are parenthesized for convenience, and an enlarged cross-sectional view taken along line FF in FIG. 7 is also shown. 9 is an enlarged sectional view taken along line GG in FIG. 7, and FIG. 10 is an enlarged sectional view taken along line HH in FIG.

  As shown in FIGS. 7 to 10, in the silicon manufacturing apparatus 3 of the present embodiment, the downstream side of the silicon manufacturing apparatus 2 of the second embodiment instead of the single silicon compound supply pipe 30. A plurality of silicon compound supply pipes, that is, one silicon compound supply pipe 80 and an upstream second silicon compound supply pipe 90 are changed to communicate with the upstream end of the main body 10a of the reaction vessel 10, and further In addition to the downstream rectifying member (first rectifying member) 70, an upstream rectifying member (second rectifying member) 100 is added, and the remaining configuration is the same. . Therefore, in the present embodiment, description will be made by paying attention to such differences, and the same components will be denoted by the same reference numerals, and description thereof will be simplified or omitted as appropriate.

  The upstream rectifying member 100 has the same configuration and arrangement as the downstream rectifying member 70 except that it is disposed on the upstream side, is made of quartz or ceramic, and has a central axis C of the reaction vessel 10. A peripheral wall 100a that is coaxially arranged and surrounds the axis thereof is a hollow truncated cone member having a truncated cone shape whose diameter decreases from the upstream side to the downstream side in the reaction vessel 10. It is supported by the main body 10a.

  The first silicon compound supply pipe 80 on the downstream side and the second silicon compound supply pipe 90 on the upstream side are both made of quartz glass, and the central axis C of the reaction vessel 10 is set in the main body portion 10a of the reaction vessel 10. The main body 10a extends in contact with each other so as to sandwich the downstream silicon compound supply port (first silicon compound supply port) 80a and the upstream silicon compound supply port (second silicon compound supply port) 90a. Respectively. From the downstream silicon compound supply port 80a, silicon compound gas is discharged into the main body 10a along the silicon compound discharge direction S5 which is the direction of the central axis C, and from the upstream silicon compound supply port 90a, the silicon compound gas is discharged. The gas is discharged into the main body 10a along the silicon compound discharge direction S6 which is the direction of the central axis C, and a sufficient amount of silicon compound gas is rapidly supplied into the reaction vessel 10. Further, the silicon compound supply pipes 80 and 90 are connected to a silicon compound gas source (not shown) via the connecting members 82 and 92 outside the main body 10a of the reaction vessel 10, respectively. 84 and 94. The silicon compound introduction pipe 34 is connected to a silicon compound gas source (not shown). Such a silicon compound gas source may store a carrier gas so as to be freely supplied, or the carrier gas may be provided with a separate carrier gas source.

  Here, regarding the arrangement relationship between the rectifying members 70 and 80, the silicon compound supply pipes 80 and 90, the first zinc supply pipe 40 and the second zinc supply pipe 50, and the discharged silicon compound gas and zinc gas The flow will be described in detail.

  In the positional relationship between the rectifying member 70 and the first silicon compound supply pipe 80, as shown in detail in FIGS. 8 and 9, the first silicon compound supply port 80a of the first silicon compound supply pipe 80 is rectified. It is substantially different from the configuration of the second embodiment that the member 70 is located in the inner region surrounded by the peripheral wall 70a. In this embodiment, the rectifying member 70 is deviated in the positive direction of the x-axis by a distance corresponding to the radius of the pipe, but the deviation amount is a minute amount with respect to the rectifying member 70. There is no real need to consider here. Here, the silicon compound gas flows upstream into the main body 10a of the reaction vessel 10 along the silicon compound discharge direction S5 which is the direction of the central axis C from the silicon compound supply 80a in the inner region surrounded by the peripheral wall 70a. Since the discharged silicon compound gas is discharged at a predetermined discharge pressure from the downstream side to the downstream side, the discharged silicon compound gas more reliably passes through the inner region surrounded by the peripheral wall 70a of the rectifying member 70, and is upstream of the main body 10a. From the bottom to the downstream side with a predetermined flow velocity distribution. Of course, due to the flow of the silicon compound gas discharged in this manner, a pressure gradient in which the pressure decreases from the upstream side toward the downstream side occurs in the main body portion 10a, and the peripheral wall 80a and the main body facing it. A pressure gradient in which the pressure decreases from the upstream side toward the downstream side also occurs between the portion 10a. Further, this arrangement relationship is the same in the arrangement relationship between the rectifying member 80 and the second silicon compound supply pipe 90, as shown in detail in FIGS.

  The arrangement relationship between the rectifying member 70 and the first zinc supply pipe 40 is not different from that in the second embodiment, but the first silicon compound supply port 80a of the first silicon compound supply pipe 80 is provided. Since the zinc gas is discharged from the first zinc supply port 40a, the silicon compound gas is discharged from the first silicon compound supply port 80a because it is located in the inner region surrounded by the peripheral wall 70a of the flow regulating member 70. There is substantially no unnecessary interference with the discharge, the first zinc supply port 40a is positioned to face the peripheral wall 70a of the rectifying member 70, and the first silicon compound supply port 80a is the peripheral wall 70a of the rectifying member 70. The relative positional relationship can be freely set within the condition that it is located within the inner region surrounded by. Further, as shown in detail in FIGS. 8 and 10, such an arrangement relationship is an arrangement relationship between the rectifying member 80 and the second zinc supply pipe 50, or between the second zinc supply port 50 a and the silicon compound supply port 90 a. The same applies to the arrangement relationship.

  Therefore, in the present embodiment, the silicon compound gas that flows from the upstream side toward the downstream side mainly through only the internal region surrounded by the peripheral wall 70a of the rectifying member 70, the internal portion surrounded by the peripheral wall 100a of the rectifying member 100 The silicon compound gas that flows from the upstream side toward the downstream side sequentially through the region and the inner region surrounded by the peripheral wall 70a of the flow regulating member 70, mainly through the space between the peripheral wall 70a and the main body portion 10a facing it. Zinc gas flowing from the side toward the downstream side, and mainly from the upstream side to the downstream side via the internal region surrounded by the peripheral wall 70a of the rectifying member 70 via the space between the peripheral wall 100a and the main body 10a facing it. The zinc gas that flows toward the gas mainly joins at the downstream side of the rectifying member 70 and causes a reduction reaction to generate silicon powder and zinc chloride that are aggregates of silicon particles. While, it is possible to further discharged from the discharge pipe 10b of the reaction vessel 10 on the downstream side, the silicon is selectively collected to obtain silicon.

  Therefore, according to the above configuration, the rectifying member includes the first rectifying member disposed on the downstream side in the reaction vessel and the second rectifying member disposed on the upstream side in the reaction vessel, and supplies zinc. The tube further has a second zinc supply port disposed upstream of the first zinc supply port in the reaction vessel, and the first zinc supply port is formed on the peripheral wall of the first rectifying member. The second zinc supply port is disposed in correspondence with the peripheral wall of the second rectifying member, thereby providing a plurality of zinc supply ports to supply a sufficient amount of zinc gas. However, the flow of zinc gas can be reliably deflected.

  The silicon compound supply port includes a first silicon compound supply port disposed on the downstream side in the reaction vessel and a second silicon compound port disposed on the upstream side in the reaction vessel, and the first silicon compound supply port The compound supply port is disposed in a region surrounded by the peripheral wall of the first rectifying member, and the second silicon compound supply port is disposed in a region surrounded by the peripheral wall of the second rectifying member. By providing a plurality of silicon compound supply ports, a sufficient amount of silicon compound gas from upstream to downstream can be expedited in the reaction vessel, and the silicon compound gas surely passes mainly through the region surrounded by the peripheral wall of the rectifying member. Can be made.

  In the present invention, the type, arrangement, number, and the like of the members are not limited to the above-described embodiments, and the components depart from the gist of the invention, such as appropriately replacing the constituent elements with those having the same operational effects. Of course, it can be appropriately changed within the range not to be.

  As described above, in the present invention, the efficiency of the reduction reaction for improving the yield of silicon is improved while eliminating the complexity of the apparatus configuration, and at the same time, the separation and recovery efficiency between the generated silicon and the generated gas is improved. The present invention provides a silicon manufacturing apparatus that can be improved, and is expected to be able to manufacture silicon materials for various electronic devices because of its general-purpose universal character.

1 is a schematic partial cross-sectional view of a silicon manufacturing apparatus according to a first embodiment of the present invention. It is an expanded sectional view by the AA line of FIG. It is an expanded sectional view by the BB line of FIG. It is a schematic partial cross section figure of the silicon manufacturing apparatus in the 2nd Embodiment of this invention. It is an expanded sectional view by the CC line of FIG. It is an expanded sectional view by the DD line of FIG. It is a schematic partial cross section figure of the silicon manufacturing apparatus in the 3rd Embodiment of this invention. It is an expanded sectional view by the EE line of FIG. 7, and attaches | subjects the code | symbol etc. for convenience, and also shows the expanded sectional view by the FF line of FIG. It is an expanded sectional view by the GG line of FIG. It is an expanded sectional view by the HH line of FIG.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ......... Silicon manufacturing apparatus 10 ......... Reaction container 10a ...... Main body part 10b ...... Discharge pipe 20 ......... Rectifying member 20a ...... Perimeter wall 20b ...... Downstream end 20c ...... Upstream end 30 ......... Silicon compound Supply pipe 30a …… Silicon compound supply port 32 ………… Connecting member 34 ………… Silicon compound introduction tube 40 ………… First zinc supply tube 40a …… First zinc supply port 40b …… Extension portion 44… …… First zinc introduction pipe 50 ............ Second zinc supply pipe 50 a ...... Second zinc supply port 50 b ...... Extended portion 54 ............ Second zinc introduction pipe 60 ............ Heating device 2 ………… Silicon manufacturing device 70 ………… Rectifying member 70a …… Peripheral wall 70b …… Downstream end 70c …… Upstream end 3 ………… Silicon manufacturing device 80 ………… First silicon compound supply pipe 80a …… No. 1 silicon compound supply port 82... Connection member 84. ... Silicon compound introduction pipe 90 ......... Second silicon compound supply pipe 90a ... Second silicon compound supply port 92 ...... Connecting member 94 ......... Silicon compound introduction pipe 100 ... Rectifying member 100a ... Peripheral wall 100b ... Downstream end 100c ... Upstream end

Claims (11)

A reaction vessel;
A silicon compound supply pipe that communicates with the reaction vessel and supplies silicon compound gas from the silicon compound supply port into the reaction vessel while being discharged in a first discharge direction;
A zinc supply pipe that communicates with the reaction vessel and supplies zinc gas while being discharged from the first zinc supply port into the reaction vessel in the second discharge direction;
Silicon provided in the reaction vessel and discharged from the silicon compound supply port in the first discharge direction while deflecting zinc gas discharged from the first zinc supply port in the second discharge direction A rectifying member that allows the compound gas to flow from the upstream side toward the downstream side in the reaction vessel;
A discharge pipe provided on the downstream side of the flow straightening member in the reaction vessel, for discharging a reaction product gas containing silicon out of the reaction vessel;
A silicon manufacturing apparatus comprising:   2. The silicon manufacturing apparatus according to claim 1, wherein the reaction container is a cylindrical member, and the rectifying member is a cylindrical member housed in the cylindrical member of the reaction container and having a peripheral wall.   The silicon manufacturing apparatus according to claim 2, wherein the cylindrical member constituting the rectifying member is a cylindrical member.   The silicon manufacturing apparatus according to claim 2, wherein the cylindrical member constituting the rectifying member is a hollow truncated cone member whose diameter decreases from the upstream side to the downstream side in the reaction vessel.   5. The silicon manufacturing apparatus according to claim 2, wherein the silicon compound supply port is arranged facing the region surrounded by the peripheral wall of the rectifying member.   5. The silicon manufacturing apparatus according to claim 2, wherein the silicon compound supply port is disposed in the region surrounded by the peripheral wall of the rectifying member.   The silicon manufacturing apparatus according to claim 2, wherein the first zinc supply port is disposed corresponding to the peripheral wall of the rectifying member.   The silicon manufacturing apparatus according to claim 7, wherein the first zinc supply port is disposed to face an upstream portion of the peripheral wall of the rectifying member.   The zinc supply pipe further has a second zinc supply port arranged on the upstream side of the reaction vessel with respect to the first zinc supply port, and the second zinc supply port The silicon manufacturing apparatus according to claim 2, which is disposed upstream of the compound supply port.   The rectifying member includes a first rectifying member disposed on the downstream side in the reaction vessel, and a second rectifying member disposed on the upstream side in the reaction vessel, and the zinc supply pipe further includes The first zinc supply port has a second zinc supply port arranged on the upstream side of the reaction vessel, and the first zinc supply port corresponds to the peripheral wall of the first rectifying member. The silicon manufacturing apparatus according to claim 2, wherein the second zinc supply port is disposed corresponding to a peripheral wall of the second rectifying member.   The silicon compound supply port includes a first silicon compound supply port disposed on the downstream side in the reaction vessel and a second silicon compound port disposed on the upstream side in the reaction vessel, and the first The silicon compound supply port is disposed in the region surrounded by the peripheral wall of the first rectifying member, and the second silicon compound supply port is surrounded by the peripheral wall of the second rectifying member. The silicon manufacturing apparatus according to claim 10, which is disposed in the region.

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