WO2011030495A1 - 多結晶シリコン製造システム、多結晶シリコン製造装置および多結晶シリコンの製造方法 - Google Patents
多結晶シリコン製造システム、多結晶シリコン製造装置および多結晶シリコンの製造方法 Download PDFInfo
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02587—Structure
- H01L21/0259—Microstructure
- H01L21/02595—Microstructure polycrystalline
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/24—Deposition of silicon only
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4411—Cooling of the reaction chamber walls
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/46—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for heating the substrate
- C23C16/463—Cooling of the substrate
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02524—Group 14 semiconducting materials
- H01L21/02532—Silicon, silicon germanium, germanium
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02636—Selective deposition, e.g. simultaneous growth of mono- and non-monocrystalline semiconductor materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/02—Apparatus characterised by their chemically-resistant properties
- B01J2219/0204—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components
- B01J2219/0236—Metal based
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Definitions
- the present invention relates to a technique for producing polycrystalline silicon, and more particularly to a technique that enables efficient heat recovery from a refrigerant used for cooling a reactor and provision of high-purity polycrystalline silicon at the same time.
- Siemens method and fluidized bed reaction method are known as methods for producing high-purity polycrystalline silicon used as a raw material for single crystal silicon for semiconductor production.
- the Siemens method is a method in which a source gas containing chlorosilane is brought into contact with a heated silicon core wire, and polycrystalline silicon is grown on the surface of the silicon core wire by a CVD (Chemical Vapor Deposition) method.
- the fluidized bed reaction method is a method for obtaining granular polysilicon by supplying monosilane or trichlorosilane as raw materials and performing vapor deposition in a flowing gas.
- Patent Document 1 heat exchange is performed between a cooling medium used for cooling a steel reaction vessel (reactor) and a steam generator.
- a system for generating steam and reusing heat (so-called steam recovery) using the steam as a heating source is disclosed, such heat exchange between the cooling medium and the steam generator is used.
- the inner wall temperature of the reaction vessel must be raised to a certain level.
- Patent Document 1 exemplifies polyorganosiloxane as a cooling medium.
- the film heat transfer coefficient depends on thermal characteristics such as specific heat and thermal conductivity of polyorganosiloxane. Becomes relatively small, and when the polycrystalline silicon grows to have a large diameter, the inner wall surface of the steel reaction vessel reaches 400 ° C. or higher.
- the inner wall surface temperature of the steel reaction vessel reaches 400 ° C or higher, the inner wall surface of the reaction vessel in contact with the process gas obtained by diluting silicon source gas such as trichlorosilane with hydrogen gas is gradually corroded, and the steel constituting the inner wall surface
- impurity elements such as phosphorus, arsenic, boron, and aluminum contained in the steel are also released into the reaction atmosphere, but these impurity elements act as dopants in the polycrystalline silicon and resist. Affects the rate and greatly reduces the quality.
- Patent Document 2 discloses a technique for obtaining high-purity precipitated silicon by precipitating silicon in a reaction furnace made of a material that hardly releases outgas. ing.
- the reaction vessel has an inner wall made of a heat-resistant alloy containing 28% by weight or more of nickel.
- the above-mentioned “heat-resistant alloy containing nickel of 28% by weight or more” is used as Incoloy 800, Inconel 600. Inconel 601, Incoloy 825, Incoloy 801, Hastelloy B, Hastelloy C and the like are exemplified.
- polycrystalline silicon for semiconductor production is required to have extremely high purity, and in recent years, the total amount of dopant impurities is required to be 100 ppt (ppt ⁇ atomic) or less in terms of atomic ratio.
- ppt ⁇ atomic ppt ⁇ atomic
- low-temperature cooling water is used as a cooling medium, and the inner wall of the reactor is kept at a relatively low temperature. It is sufficient to grow polycrystalline silicon while maintaining the temperature, but with the conventional cooling method using low-temperature water, the temperature of the cooling water discharged from the reactor is less than 100 ° C, and steam is generated from water at this temperature. It is virtually impossible to efficiently recover the heat.
- a polycrystalline silicon production system of the present invention includes a reaction furnace for producing polycrystalline silicon, a refrigerant tank that stores a cooling medium, and a cooling medium that is supplied from the refrigerant tank to the reaction furnace. And a refrigerant circulation path for collecting the refrigerant in the refrigerant tank via a refrigerant flow path provided in the reactor, and an energy collecting unit for taking out a part of the cooling medium collected in the refrigerant tank for energy collection.
- a hot water having a temperature higher than the normal boiling point is used as a cooling medium supplied to the reaction furnace, steam obtained by vaporizing the hot water is taken out from the energy recovery unit, and the hot water is removed from the reaction furnace.
- the polycrystalline silicon is produced while the temperature inside the reactor is controlled to 400 ° C. or lower by circulating the reactor.
- a first pressure controller that depressurizes the hot water downstream from the reactor in the refrigerant circulation path;
- a second pressure control unit for controlling the pressure in the refrigerant tank, and the first pressure control unit reduces the pressure of the hot water to flush the hot water and generate steam.
- a system for cooling hot water can be mentioned.
- the temperature of the hot water is less than 200 ° C.
- the R value is 60% or more.
- the Cr content, the Ni content, and the Si content mass% of the first alloy material are [Cr]: 14.6 to 25.2 mass%, [Ni]: 19.6 to 77.5 mass%, [Si]: Within the range of 0.3 to 0.6% by mass.
- the furnace inner surface temperature is controlled to 370 ° C. or lower when polycrystalline silicon is deposited in the reaction furnace.
- a heat conductive layer made of a second alloy material having a higher thermal conductivity than the first alloy material is provided outside the furnace of the corrosion-resistant layer on the inner wall. Also good.
- the polycrystalline silicon manufacturing system of the present invention may have a configuration in which the coolant channel portion is provided outside the furnace of the inner wall.
- the refrigerant tank is provided with a liquid level control unit that detects the level of hot water stored in the refrigerant tank and replenishes the shortage. be able to.
- the polycrystalline silicon production system of the present invention can be configured such that a hot water supply pump is provided in a refrigerant circulation path for supplying a cooling medium from the refrigerant tank to the reactor.
- the polycrystalline silicon production system of the present invention is particularly effective for producing polycrystalline silicon having a dopant impurity total amount of 100 atom ppt or less.
- polycrystalline silicon can be obtained by supplying a silicon raw material gas in a state where the furnace inner surface temperature of the reaction furnace inner wall is controlled to less than 400 ° C.
- the method for producing polycrystalline silicon according to the present invention uses a steel type made of an alloy having a relational expression [Cr] + [Ni] ⁇ 1.5 [Si] of chromium, nickel, and silicon containing mass% of 40% or more.
- An inner wall surface of the reaction furnace in contact with the process gas is formed, and steam is generated while the inner wall surface of the reaction furnace is kept at 370 ° C. or lower during the growth of polycrystalline silicon.
- the polycrystalline silicon production apparatus includes a reaction furnace for producing polycrystalline silicon, and a refrigerant circulation path that cools the reaction furnace using hot water having a temperature higher than the standard boiling point.
- the hot water discharged from the furnace is flushed to generate steam.
- the hot water itself used as the cooling medium is reused as steam, it is possible to efficiently recover heat from the refrigerant used for cooling the reactor.
- the reactor is kept at a relatively high temperature using hot water as a cooling medium in order to generate steam, contamination of dopant impurities from the inner wall of the reactor when polycrystalline silicon is deposited in the reactor It can reduce and can obtain highly purified polycrystalline silicon.
- the inner wall surface temperature at the outlet side of the cooling medium immediately before the end of the polycrystalline silicon precipitation process and the dopant impurities incorporated into the polycrystalline silicon It is a figure which shows the relationship with a density
- FIG. 1 is a diagram for explaining a configuration example of a polycrystalline silicon manufacturing system according to the present invention.
- a polycrystalline silicon manufacturing system 100 for depositing polycrystalline silicon by a Siemens method is illustrated.
- the reaction furnace 10 is provided on the base plate 1, and a torii type silicon core wire 5 which is connected to the electrodes 2 a and 2 b at both ends and can be energized is set inside.
- a raw material gas such as trichlorosilane gas for depositing polycrystalline silicon, or a process gas such as nitrogen gas or hydrogen gas is supplied from the gas nozzle 3 into the reaction furnace 10 and heated by current supply from the electrodes 2a and 2b.
- Polycrystalline silicon 6 is deposited by vapor phase growth on the surface.
- Gas exhaust from the reaction furnace 10 is performed from the exhaust port 4.
- the furnace inner surface temperature is controlled to less than 400 ° C. by adjusting the flow rate of the cooling medium (hot water) 15 described later.
- Reference numeral 20 denotes a refrigerant tank that stores hot water 15 as a cooling medium, and the hot water 15 is supplied from the refrigerant tank 20 to the reaction furnace 10 from below by a hot water supply pump 21 provided in the refrigerant circulation path 24a. After passing through a refrigerant flow path 13 (described later) provided in the furnace 10, it is discharged from above the reaction furnace 10.
- the pressure of the hot water 15 discharged from above the reaction furnace 10 is detected by the first pressure control unit, that is, the pressure indicating controller PIC22 provided in the refrigerant circulation path 24b, and the opening degree of the control valve 23 is adjusted.
- the first pressure control unit that is, the pressure indicating controller PIC22 provided in the refrigerant circulation path 24b
- the opening degree of the control valve 23 is adjusted.
- the pressure in the refrigerant tank 20 that has risen with the generation of the steam is detected by the second pressure control unit, that is, the pressure indicating controller PIC31, and the steam is collected through the control valve 32. That is, a part of the cooling medium collected in the refrigerant tank 20 is taken out as steam and can be reused as a heat source for another use. Further, the temperature of the hot water supplied to the reactor 10 can be uniquely managed by the second pressure control unit, but should be managed using direct detection of the refrigerant temperature instead of the pressure control mechanism. You can also.
- the temperature inside the reaction furnace is the temperature of the hot water (pressure of the refrigerant tank 20) and the circulation amount, the amount of steam taken out, and the formation reaction of the polycrystalline silicon 6 in the reaction furnace 10. It can be calculated by heat balance calculation using the amount of energy added to perform, the thermal conductivity based on the structure and material of the reactor 10, the arrangement of the silicon core wire 5 arranged for the production of the polycrystalline silicon 6, etc.
- the target furnace inner surface temperature is set to 400 ° C. or lower, preferably 370 ° C. or lower, by controlling the pressure in the refrigerant tank and controlling the circulation amount of hot water as described above. be able to.
- the outlet temperature of the refrigerant channel is measured, the amount of energy removed from the temperature in the refrigerant tank and the amount of circulation is obtained, and the estimated value of the furnace inner surface temperature is calculated from the thermal conductivity based on the structure and material of the reactor.
- hot water having a temperature higher than the normal boiling point (100 ° C.) is used as the cooling medium supplied to the reaction furnace 10 for the following reason.
- the temperature of the cooling medium discharged from the reactor 10 is about 130 ° C.
- the temperature of the cooling medium is returned to about 100 ° C. by heat exchange between the cooling medium at that temperature and water.
- water is effective as a cooling medium because the film heat transfer coefficient can be very large.
- the temperature of the supplied water is 100 ° C. or lower
- the temperature of the water discharged from the reaction furnace 10 is at most about 120 ° C., and it is necessary to return to a temperature of 100 ° C. or lower for circulation use. From the viewpoint of steam recovery, it is not practical.
- hot water having a temperature exceeding the normal boiling point of water ie, 100 ° C.
- the reactor 10 when growing polycrystalline silicon by the Siemens method, if hot water at 125 ° C., for example, is supplied to the reactor 10 immediately before the end of the reaction when the polycrystalline silicon rod is enlarged, the reactor 10 The discharged hot water temperature was 141 ° C. At this time, the inner surface temperature of the reaction furnace is cooled to about 231 ° C. even at the hot water outlet end side where the temperature is highest, and can be sufficiently kept at 370 ° C. or less.
- the hot water discharged from the reactor 10 is 141 ° C.
- the hot water itself becomes steam when the hot water pressure is controlled (depressurized) and flushed, and between the cooling medium and the steam generator.
- the hot water pressure at a pressure exceeding the film temperature vapor pressure to prevent boiling of the hot water at the heat removal surface film of the reactor 10. This prevention of boiling is performed by the first pressure control valve 23. Further, the pressure indicating controller PIC31 and the control valve 32 for detecting the pressure in the refrigerant tank 20 control the pressure in the refrigerant tank 20, and thereby the temperature of hot water in the refrigerant tank 20 is controlled. .
- the liquid level height of the hot water 15 in the refrigerant tank 20 is detected by the level controller LIC41, and an amount corresponding to the hot water 15 lost by the steam recovery described above or a slight excess amount of pure water is supplied to the control valve. Replenish by adjusting the opening of 42.
- the hot water 15 in the refrigerant tank 20 is circulated to the reaction furnace 10 via the hot water supply pump 21.
- FIG. 2 is a cross-sectional view for explaining the structure of the wall portion of the reaction furnace 10 of the present invention.
- the cooling medium is disposed outside the furnace of the inner wall 11, that is, between the inner wall 11 inside the furnace and the outer wall 12 outside the furnace.
- the refrigerant flow passage 13 for circulating the hot water 15 is provided in a spiral shape, and the hot water 15 is supplied from the lower part of the reaction furnace 10 and discharged from the top.
- the inner wall 11 has a two-layer structure, and a corrosion-resistant layer 11a made of a highly corrosion-resistant alloy material is provided on the inner side of the furnace in contact with the corrosive process gas, and on the outer side (outer wall side) of the reactor 10
- the heat conduction layer 11b for efficiently conducting the heat from the inner wall surface to the cooling medium flow path 13 is provided.
- the heat conductive layer 11b is made of an alloy material having a higher thermal conductivity than the alloy material used for the corrosion resistant layer 11a.
- SB steel carbon steel for boilers and pressure vessels
- SGV steel for medium / normal temperature pressure vessels
- Carbon steel carbon steel
- the heat conductive layer 11b does not need to be limited to what consists of a single steel material, It is good also as what consists of a clad steel material which laminated
- the temperature and time were selected as 200 ° C. and 9 days as the first condition, and the temperature and time were selected as 300 ° C. and 9 days as the second condition, and corrosion experiments were performed under these first and second conditions.
- the temperature was set to 400 ° C. and 500 ° C., respectively, and the time was selected to be 19 days. Other than that, the corrosion test was performed again in the same procedure as described above.
- Table 1 and FIG. 3 summarize the results of the corrosion test under the above-described third condition (temperature 400 ° C., time: 19 days).
- Table 1 summarizes the specific composition of the alloy material (steel type) and the change in weight after the corrosion test.
- NAR is a registered trademark of Sumitomo Metal Industries, Ltd.
- Incoloy and Inconel are registered trademarks of Inco
- Hastelloy is a registered trademark of Highness Stellite
- Carpenter is a registered trademark of Carpenter.
- an alloy material having the R value of 40% or more is preferable, and a more preferable R value is 60% or more.
- a significant change in weight was observed as compared with the third condition.
- each reactor is made with SUS310S (R value: 41-46%) or Hastelloy® C (R value: 62% or more), which is a steel grade satisfying the condition of R value 40% or more, as an inner wall corrosion-resistant layer. Then, using these reactors, polycrystalline silicon was actually deposited, and an investigation was carried out to determine the temperature dependence of the dopant impurity concentration in the obtained polycrystalline silicon rod.
- FIG. 4 shows the inner wall surface temperature (horizontal axis) at the outlet side of the cooling medium immediately before the end of the polycrystalline silicon precipitation process for each reactor of the inner wall made of SUS310S or Hastelloy® C, which is a Cr—Ni—Si alloy material. It is a figure which shows the relationship with the dopant impurity density
- the total amount of dopant shown on the vertical axis is the total amount of dopant obtained by photoluminescence analysis, and specifically, the total content of phosphorus, arsenic, boron, and aluminum.
- the total amount of dopant in polycrystalline silicon is 100 ppt ⁇ atomic or less due to practical requirements for controlling resistivity during CZ single crystal growth or FZ single crystal growth used for semiconductor applications.
- the total amount of dopant in the polycrystalline silicon can be reduced to 100 ppt ⁇ atomic or less by keeping the temperature of the inner wall surface at 220 ° C. or lower.
- Hastelloy® C is used for the inner wall surface, the total amount of dopant in the polycrystalline silicon can be reduced to 100 ppt ⁇ atomic or less by keeping the temperature of the inner wall surface at 370 ° C. or lower.
- An alloy material having an R value defined by R [Cr] + [Ni] ⁇ 1.5 [Si] of 40% or more, which is preferable as a material for a corrosion resistant layer on the inner wall of a reactor for producing polycrystalline silicon Is shown in Table 2.
- the procedure for conducting the polycrystalline silicon precipitation reaction using the reactor of the present invention is generally as follows. First, the silicon core wire 5 is connected to the electrode 2, the reaction furnace 10 is placed in close contact with the base plate 1, and nitrogen gas is supplied from the gas nozzle 3 to replace the air in the reaction furnace 10 with nitrogen. Air and nitrogen in the reaction furnace 10 are exhausted from the exhaust port 4.
- the silicon core wire 5 is preheated to a temperature of 250 ° C. or higher so that the current can flow efficiently. Subsequently, a current is supplied from the electrode 2 to the silicon core wire 5 to heat the silicon core wire 5 to 900 ° C. or higher. Further, trichlorosilane gas is supplied as a raw material gas together with hydrogen gas, and polycrystalline silicon 6 is vapor-phase grown on the silicon core wire 5 in a temperature range of 900 ° C. or more and 1200 ° C. or less. Unreacted gas and by-product gas are discharged from the exhaust port 4.
- hot water 15 is supplied as a cooling medium to cool the reaction furnace 10.
- the pressure in the refrigerant tank 20 is maintained at 0.15 MPaG by the second pressure adjusting unit including the pressure indicating controller 31 and the pressure adjusting valve 32, thereby causing the reactor 10. Maintaining the temperature of the hot water 15 supplied to the reactor at 125 to 127 ° C. and maintaining the inner wall surface of the reactor 10 at 370 ° C. or less, a sufficient amount of refrigerant so that the reactor outlet temperature of the hot water does not exceed 200 ° C.
- the amount of hot water obtained from the heat balance calculation is supplied to the reactor by the refrigerant supply pump 21.
- the hot water 15 supplied as a cooling medium for cooling the reaction furnace 10 is set to a temperature range exceeding 100 ° C. and less than 200 ° C. exceeding the standard boiling point temperature, and the heat removal surface of the heat conduction layer 11b.
- the pressure adjustment valve 23 of the first pressure control unit controls the pressure to exceed the vapor pressure at the boundary film temperature.
- the pressure-controlled hot water 15 is supplied from below the reaction furnace 10 by the hot water supply pump 21 and cools the inner wall 11 through the cooling medium flow path 13 in contact with the heat conduction layer 11b, while the heat conduction layer 11b It is heated, heated up, and discharged from above the reactor 10.
- the source gas and current supply to the polycrystalline silicon 6 are stopped in this order, and the temperature in the reaction furnace 10 is lowered.
- the hot water 15 is switched to cold water, and the reaction furnace 10 is cooled to near room temperature.
- the reaction furnace 10 is opened to the atmosphere, and the grown polycrystalline silicon 6 is trimmed.
- the heat conduction layer 11b has an inner wall 11 of SB (boiler and pressure vessel carbon steel), and has two cooling medium channels 13, the cooling medium channel 13 While supplying hot water 15 of 125 ° C. to 127 ° C. at 72 m 3 / hr to both channels, the hot water pressure was controlled to 0.5 MPaG by the pressure indicating controller PIC22.
- the main raw material trichlorosilane gas was supplied while energizing and heating the silicon core wire 5 having a side of 7 mm square in a hydrogen atmosphere to about 1060 ° C., and the polycrystalline silicon 6 was grown to a diameter of about 120 mm in a growth time of about 80 hours. .
- the temperature of the hot water 15 discharged from the reaction furnace 10 was 129 ° C. at the start of energization and 141 ° C. at the end of the reaction.
- the results of heat transfer analysis at the start of energization and at the end of the reaction in the reactor were as shown in Table 3, and the surface temperature of the corrosion-resistant layer 11a on the hot water outlet end side was calculated to be 231 ° C at maximum.
- the pressure of the hot water 15 discharged from the reaction furnace 10 is maintained at 0.5 MPaG (hot water boiling temperature 158 ° C.) by the pressure indicating controller PIC 22 and does not boil in the cooling medium flow path 13 (heat This is because the surface temperature of the conductive layer channel side exceeds 152 ° C.). Further, by maintaining the pressure in the refrigerant tank 20 at 0.15 MPaG by the pressure indicating controller 31, the temperature of the hot water 15 supplied to the reactor 10 can be stably maintained at 125 to 127 ° C. and adjusted. Steam could be removed from the valve 32. Steam was recovered at 0.4 ton / hr at the beginning of the reaction and 3.5 ton / hr at the end of the reaction. This corresponds to a heat recovery of about 65% of the electric power input to the reactor 10.
- the hot water itself used as the cooling medium is reused as steam, it is possible to efficiently recover heat from the refrigerant used for cooling the reactor.
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Abstract
Description
実施例1
実施例2
2a、2b 電極
3 ガスノズル
4 排気口
5 シリコン芯線
6 多結晶シリコン
10 反応炉(反応容器)
11 内壁
11a 耐食層
11b 熱伝導層
12 外壁
13 冷却媒体流路
15 熱水
20 冷媒タンク
21 熱水供給ポンプ
22 圧力指示調節計
23 調節弁
24a、24b 冷媒循環経路
31 圧力指示調節計
32 調節弁
41 レベル調節計
42 調節弁
100 多結晶シリコン製造システム
Claims (15)
- 多結晶シリコン製造用の反応炉と、
冷却媒体を貯蔵する冷媒タンクと、
冷却媒体を前記冷媒タンクから前記反応炉に供給するとともに前記反応炉に設けられた冷媒流路部を経由して前記冷媒タンクに回収する冷媒循環経路と、
前記冷媒タンクに回収される冷却媒体の一部をエネルギー回収用として取り出すエネルギー回収部とを備え、
前記反応炉に供給される冷却媒体として標準沸点よりも高い温度の熱水が用いられ、
該熱水を気化させたスチームが前記エネルギー回収部より取り出され、
前記熱水を前記反応炉に循環させることにより前記反応炉の炉内側表面温度を400℃以下に制御しつつ多結晶シリコンの製造を行うことを特徴とする多結晶シリコン製造システム。 - 前記冷媒循環経路中の前記反応炉より下流側に、前記熱水を減圧する第1圧力制御部と、前記冷媒タンク内の圧力を制御する第2圧力制御部とをさらに備え、
前記第1圧力制御部で前記熱水の圧力を減圧することにより前記熱水をフラッシュさせてスチームを発生させると同時に前記熱水の冷却を行うことを特徴とする請求項1に記載の多結晶シリコン製造システム。 - 前記熱水の温度は200℃未満である請求項1又は2に記載の多結晶シリコン製造システム。
- 前記反応炉には、内壁の炉内表面側に、クロム(Cr)、ニッケル(Ni)、およびシリコン(Si)の含有質量%をそれぞれ[Cr]、[Ni]、および[Si]としたときに、R=[Cr]+[Ni]-1.5[Si]で定義付けられるR値が40%以上となる組成の第1の合金材料からなる耐食層が設けられている請求項1又は2に記載の多結晶シリコン製造システム。
- 前記R値が60%以上である、請求項4に記載の多結晶シリコン製造システム。
- 前記第1の合金材料のCr、Ni、およびSiの含有質量%はそれぞれ、[Cr]:14.6~25.2質量%、[Ni]:19.6~77.5質量%、[Si]:0.3~0.6質量%の範囲内にある、請求項4に記載の多結晶シリコン製造システム。
- 前記反応炉内で多結晶シリコンを析出させる際の炉内側表面温度が370℃以下に制御される、請求項4に記載の多結晶シリコン製造システム。
- 前記内壁の耐食層の炉外側に、前記第1の合金材料よりも高い熱伝導率の第2の合金材料からなる熱伝導層が設けられている、請求項4に記載の多結晶シリコン製造システム。
- 前記内壁の炉外側に前記冷媒流路部が設けられている、請求項4に記載の多結晶シリコン製造システム。
- 前記冷媒タンクには該冷媒タンク内に貯蔵されている熱水の液面を検知するとともに不足分を補充する液面制御部が設けられている請求項1又は2に記載の多結晶シリコン製造システム。
- 前記冷却媒体を前記冷媒タンクから前記反応炉に供給する前記冷媒循環経路内に熱水供給ポンプが設けられている請求項1又は2に記載の多結晶シリコン製造システム。
- 前記多結晶シリコン製造システムは、ドーパント不純物総量が100原子ppt以下である多結晶シリコンを製造するためのシステムである請求項1又は2に記載の多結晶シリコン製造システム。
- 請求項1又は2に記載の多結晶シリコン製造システムを用いた多結晶シリコンの製造方法であって、前記反応炉内壁の炉内側表面温度を400℃未満に制御した状態でシリコン原料ガスを供給し、多結晶シリコンを得ることを特徴とする多結晶シリコンの製造方法。
- クロム、ニッケル、シリコンの含有質量%の関係式[Cr]+[Ni]-1.5[Si]が40%以上の合金からなる鋼種によりプロセスガスに接する反応炉の内壁面を構成し、多結晶シリコンの成長中、前記反応炉の内壁面を370℃以下に保ちながらスチームを発生させることを特徴とする多結晶シリコンの製造方法。
- 多結晶シリコン製造用の反応炉と、標準沸点よりも高い温度の熱水を用いて反応炉を冷却する冷媒循環経路とを有し、前記反応炉から排出された前記熱水をフラッシュさせてスチームを発生させることを特徴とする多結晶シリコン製造装置。
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EP10815098.8A EP2479141B1 (en) | 2009-09-14 | 2010-07-20 | System for producing polycrystalline silicon, and process for producing polycrystalline silicon |
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EP2628532B1 (en) | 2019-08-28 |
JP5552284B2 (ja) | 2014-07-16 |
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