TWI671421B - Silicon deposition reactor with bottom seal arrangement - Google Patents

Silicon deposition reactor with bottom seal arrangement Download PDF

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TWI671421B
TWI671421B TW104120874A TW104120874A TWI671421B TW I671421 B TWI671421 B TW I671421B TW 104120874 A TW104120874 A TW 104120874A TW 104120874 A TW104120874 A TW 104120874A TW I671421 B TWI671421 B TW I671421B
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ring
gasket
seal
sealing ring
chamber
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TW201623671A (en
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麥可V 史潘格勒
馬修J 米勒
傑佛瑞A 漢森
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大陸商陝西有色天宏瑞科矽材料有限責任公司
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    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1818Feeding of the fluidising gas
    • B01J8/1827Feeding of the fluidising gas the fluidising gas being a reactant
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1836Heating and cooling the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1872Details of the fluidised bed reactor
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    • C01B33/027Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
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    • C01B33/027Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
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    • C01B33/035Preparation 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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    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical 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
    • C23C16/4401Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
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    • C23COATING 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
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    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • C23C16/4401Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
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    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical 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
    • C23C16/4417Methods specially adapted for coating powder
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    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical 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
    • C23C16/442Chemical 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 using fluidised bed process
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B15/00Fluidised-bed furnaces; Other furnaces using or treating finely-divided materials in dispersion
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B15/00Fluidised-bed furnaces; Other furnaces using or treating finely-divided materials in dispersion
    • F27B15/02Details, accessories, or equipment peculiar to furnaces of these types
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F27B15/00Fluidised-bed furnaces; Other furnaces using or treating finely-divided materials in dispersion
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    • F27B15/04Casings; Supports therefor
    • F27B15/06Arrangements of linings
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B15/00Fluidised-bed furnaces; Other furnaces using or treating finely-divided materials in dispersion
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F27B15/09Arrangements of devices for discharging
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B01J2208/00017Controlling the temperature
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Abstract

本發明揭示用於生產高純度有矽塗層顆粒的流化床反應器系統。一容器具有:一外殼體;一絕緣層,其位在該外殼體內側;一同心圓的內殼體,其位在該外殼體內側;以及一同心圓的襯墊,其被定位在該內殼體內側並且定義一反應器腔室。該內殼體與襯墊藉由一O型環密封配置一起在它們的底部處被密封,用以防止該反應器腔室中的氣體進入介於該內殼體與該襯墊之間的空間。一中央入口噴嘴會在該反應器腔室之中產生一垂直羽狀氣體。 The invention discloses a fluidized bed reactor system for producing high-purity silicon-coated particles. A container has: an outer shell; an insulating layer positioned inside the outer shell; a concentric inner shell positioned inside the outer shell; and a concentric gasket positioned inside the outer shell The inside of the housing and defines a reactor chamber. The inner shell and the gasket are sealed together at their bottoms by an O-ring seal arrangement to prevent gas in the reactor chamber from entering the space between the inner shell and the gasket . A central inlet nozzle produces a vertical plume of gas in the reactor chamber.

Description

具有底部密封配置的矽沉積反應器 Silicon deposition reactor with bottom sealed configuration

本揭示內容和用於熱分解流化床(fluidized bed)中的矽承載氣體的反應器有關,以便產生有矽塗層的顆粒(silicon-coated particles)。 The present disclosure relates to a reactor for thermally decomposing a silicon-bearing gas in a fluidized bed in order to generate silicon-coated particles.

【相關申請案交叉參考】[Cross Reference for Related Applications]

本發明主張2014年12月31日提申的美國臨時申請案第62/099,057號的權利,本文以引用的方式將其完整併入。 The present invention claims the right of US Provisional Application No. 62 / 099,057 filed on December 31, 2014, which is incorporated herein by reference in its entirety.

流化床中的矽承載氣體的熱分解係一種產生用於光伏特與半導體產業的多晶矽的引人注目的製程,因為其卓越的質量與熱量傳輸、大沉積表面、以及連續性生產的關係。相較於西門子式的反應器(Siemens-type reactor),該流化床反應器以小額的能量消耗提供明顯較高的生產速率。該流化床反應器能夠為連續性並且高自動化,以便大幅減少人力成本。 Thermal decomposition of a silicon-bearing gas in a fluidized bed is an attractive process for producing polycrystalline silicon for the photovoltaic and semiconductor industries due to its superior quality in relation to heat transfer, large deposition surfaces, and continuous production. Compared to a Siemens-type reactor, the fluidized-bed reactor provides a significantly higher production rate with a small amount of energy consumption. The fluidized bed reactor can be continuous and highly automated in order to significantly reduce labor costs.

其中一種此類的流化床反應器已在WO2011063007 A2中說明過並且顯示在圖1中。於該反應器中,一內殼體大致上垂直延伸穿過反應器並且大致上為具有大致上圓形剖面的圓柱形。一位在該內殼體內側的襯墊大致上垂直延伸穿過反應器並且同樣大致上為具有大致上圓形剖面的 圓柱形。該襯墊定義該反應器腔室並且保護該內殼體避免受到有矽塗層的顆粒的磨擦破壞。該襯墊係由經過選擇避免污染該些矽顆粒的一或多種材料所構成。因此,該襯墊會保護該流化床中的晶種顆粒與產物顆粒,避免受到內殼體材料及/或容器壁部材料的污染。 One such fluidized bed reactor has been described in WO2011063007 A2 and is shown in FIG. 1. In the reactor, an inner shell extends substantially vertically through the reactor and is substantially cylindrical with a substantially circular cross section. A gasket on the inside of the inner casing extends substantially vertically through the reactor and is also generally of a generally circular cross-section. Cylindrical. The gasket defines the reactor chamber and protects the inner casing from abrasion damage by silicon-coated particles. The pad is composed of one or more materials selected to avoid contamination of the silicon particles. Therefore, the gasket will protect the seed particles and product particles in the fluidized bed from being contaminated by the inner shell material and / or the container wall material.

WO2011063007 A2的內殼體與襯墊藉由一間隙而分開,使得一圓柱形形狀的環狀空間被提供在該內殼體與該襯墊之間。一密封會被提供在該內殼體的底部,用以避免氣體與顆粒狀材料從反應腔室進入該空間。 The inner shell and the gasket of WO2011063007 A2 are separated by a gap, so that a cylindrical annular space is provided between the inner shell and the gasket. A seal is provided at the bottom of the inner housing to prevent gases and particulate materials from entering the space from the reaction chamber.

因為該內殼體與該襯墊係由具有不同熱膨脹係數的不同材料製成的關係,並且因為在該反應器的操作期間反應腔室中的氣體壓力不同於該內殼體與該襯墊之間的空間中的氣體壓力的關係,所以,會有問題發生。 Because the inner casing and the gasket are made of different materials having different thermal expansion coefficients, and because the gas pressure in the reaction chamber during operation of the reactor is different from that of the inner casing and the gasket There is a relationship between the pressure of the gas in the space, so there will be problems.

此系統中的一特殊問題為介於該內殼體與該襯墊之間的密封不發生作用。於此系統中,一典型的密封配置為一位在兩個平坦的水平金屬表面之間的扁平墊圈。此配置會有問題,因為該墊圈僅藉由平坦表面之間的磨擦力被固定在正確的地方。流體床反應器會在操作其間產生龐大的振動。因此,當振動與壓力突波造成該反應器底部的部件在附近偏移時,該扁平墊圈會慢慢地滑出該兩個平坦的金屬表面之間。 A special problem in this system is that the seal between the inner casing and the gasket is ineffective. In this system, a typical seal configuration is a flat washer between two flat horizontal metal surfaces. This configuration can be problematic because the gasket is held in place only by friction between the flat surfaces. Fluid bed reactors generate large vibrations during operation. Therefore, when vibration and pressure surges cause the components at the bottom of the reactor to shift in the vicinity, the flat gasket will slowly slide out between the two flat metal surfaces.

還有另一個問題係,當某個製程翻倒時,一扁平墊圈的朝內邊緣表面會直接接觸該反應器腔室內部的矽顆粒。該墊圈會因直接接觸熱的矽顆粒而過熱並且故障。一旦一扁平墊圈的的最內側區域故障並且脫落時,該些熱的矽顆粒會作用於下一層並且最後會「燒穿(burn through)」整個墊圈,從而破壞密封的完整性。這同樣會影響產物品質。一些斷裂的墊圈 材料會進入該反應器腔室並且污染其中所含的矽顆粒。 Another problem is that when a certain process is turned over, the inner edge surface of a flat gasket will directly contact the silicon particles inside the reactor chamber. The gasket can overheat and fail due to direct contact with hot silicon particles. Once the innermost area of a flat gasket fails and comes off, the hot silicon particles will act on the next layer and eventually "burn through" the entire gasket, thereby destroying the integrity of the seal. This also affects product quality. Some broken washers Material enters the reactor chamber and contaminates the silicon particles contained therein.

因此,本領域需要一種能夠於出現在用於沉積矽的流化床反應器之中的條件下一個有效運作的密封配置。 Therefore, what is needed in the art is a sealed configuration that can operate effectively under the conditions that occur in a fluidized bed reactor for silicon deposition.

本發明揭示用於生產高純度有矽塗層顆粒的流化床反應器系統。該些流化床反應器系統包含一襯墊,其係由會最小化該流化床中的顆粒污染的材料所構成。於該反應器中,一內殼體大致上垂直延伸穿過反應器並且大致上為具有大致上圓形剖面的圓柱形。一位在該內殼體內側的襯墊大致上垂直延伸穿過反應器並且同樣大致上為具有大致上圓形剖面的圓柱形。該襯墊定義該反應器腔室並且保護該內殼體避免受到因接觸有矽塗層的顆粒所造成的磨擦破壞。 The invention discloses a fluidized bed reactor system for producing high-purity silicon-coated particles. The fluidized bed reactor systems include a liner composed of a material that will minimize particulate contamination in the fluidized bed. In the reactor, an inner shell extends substantially vertically through the reactor and is substantially cylindrical with a substantially circular cross section. A gasket inside the inner casing extends substantially vertically through the reactor and is also generally cylindrical with a generally circular cross-section. The gasket defines the reactor chamber and protects the inner casing from abrasion damage caused by contact with particles coated with silicon.

其中一種系統包括一容器,其具有:一外殼體;一絕緣層,其鄰接該外殼體的一內表面;一大致上圓柱形的內殼體,其位在該絕緣層內側並且被定位在複數個加熱器內側。優點係,該內殼體係由一高溫合金製成。一大致上圓柱形的襯墊位在該內殼體裡面,有一圓柱形形狀的環狀空間被提供在該內殼體與該襯墊之間。該襯墊定義一反應腔室,該反應腔室含有複數個晶種顆粒及/或有矽塗層的顆粒。該襯墊可以由非污染的材料製成,其包含,但是並不限制於:石英、矽、低鎳合金、高溫合金、鈷合金、氮化矽、石墨、碳化矽、鉬、或是鉬合金。 One system includes a container having: an outer shell; an insulating layer abutting an inner surface of the outer shell; and a generally cylindrical inner shell positioned inside the insulating layer and positioned in a plurality Heater inside. The advantage is that the inner casing is made of a high temperature alloy. A substantially cylindrical gasket is positioned inside the inner casing, and a cylindrical annular space is provided between the inner casing and the gasket. The pad defines a reaction chamber containing a plurality of seed particles and / or silicon-coated particles. The gasket can be made of non-contaminating materials, including but not limited to: quartz, silicon, low nickel alloy, high temperature alloy, cobalt alloy, silicon nitride, graphite, silicon carbide, molybdenum, or molybdenum alloy .

內殼體與襯墊的底端表面皆被支撐在該反應器的底部附近。一支撐裝配件包含多個器件,它們被排列成用以密封介於該內殼體與襯墊之間的空間的底部,以便阻隔氣體和顆粒材料進入該空間。該裝配件 的優點係在相鄰的鋼製反應器部件的相向表面之間包含一或更多個O型環。每一個O型環被容納在一定義在一鋼製反應器部件的水平表面之中的環狀通道或溝槽之中。O型環位在定義該反應器腔室的(多個)表面的某個徑向朝外距離處,使得位在該腔室內側的熱矽顆粒不會碰觸到該些O型環。因此,該些矽顆粒不會因接觸到O型環而有任何污染。此O型環的完整性會被維持,因為該些熱顆粒無法碰觸該O型環,因為該些鋼製部件會吸收大部分的熱並且將其向外傳導。優點係,O型環被提供在一位於該內殼體與該襯墊之間的鋼製密封環的上方表面與下方表面處。該鋼製密封環會幫助散熱。因為每一個O型環皆位在一環狀溝槽之中,所以,該O型環無法滑出正確的位置。 Both the inner shell and the bottom surface of the gasket are supported near the bottom of the reactor. A support assembly includes a plurality of devices that are arranged to seal the bottom of a space interposed between the inner case and the gasket so as to block gas and particulate material from entering the space. The assembly The advantage is that one or more O-rings are included between facing surfaces of adjacent steel reactor components. Each O-ring is housed in an annular channel or groove defined in the horizontal surface of a steel reactor component. The O-ring is located at a certain radially outward distance defining the surface (s) of the reactor chamber, so that the hot silicon particles located inside the chamber will not touch the O-rings. Therefore, the silicon particles will not be contaminated by contact with the O-ring. The integrity of the O-ring is maintained because the hot particles cannot touch the O-ring because the steel components absorb most of the heat and conduct it outward. The advantage is that the O-ring is provided at an upper surface and a lower surface of a steel seal ring located between the inner casing and the gasket. This steel sealing ring helps dissipate heat. Because each O-ring is located in an annular groove, the O-ring cannot slide out of the correct position.

該系統進一步包含一反應氣體入口噴嘴,一或更多個入口用於流化氣體,例如,複數個流化噴嘴,以及至少一出口用於矽產物移除。 The system further includes a reactive gas inlet nozzle, one or more inlets for fluidizing the gas, for example, a plurality of fluidizing nozzles, and at least one outlet for silicon product removal.

前面的發明內容可以參考隨附的圖式從下面的詳細說明中更清楚的瞭解。 The foregoing summary may be more clearly understood from the following detailed description with reference to the accompanying drawings.

A1‧‧‧中央軸 A 1 ‧‧‧ central axis

10‧‧‧流化床反應器 10‧‧‧ fluidized bed reactor

12‧‧‧容器 12‧‧‧ container

15‧‧‧反應器腔室 15‧‧‧ reactor chamber

20‧‧‧入口噴嘴 20‧‧‧ inlet nozzle

22‧‧‧中央路徑 22‧‧‧ Central Path

24‧‧‧環狀路徑 24‧‧‧ circular path

40‧‧‧流化氣體噴嘴 40‧‧‧ fluidized gas nozzle

50‧‧‧取樣噴嘴 50‧‧‧Sampling nozzle

60‧‧‧壓力噴嘴 60‧‧‧pressure nozzle

70‧‧‧淨化氣體/冷卻氣體噴嘴 70‧‧‧Purge gas / cooling gas nozzle

72‧‧‧淨化氣體/冷卻氣體噴嘴 72‧‧‧Purge gas / cooling gas nozzle

80‧‧‧外殼體 80‧‧‧ outer shell

90‧‧‧內部床加熱器 90‧‧‧ Internal Bed Heater

100‧‧‧加熱器 100‧‧‧ heater

110‧‧‧晶種噴嘴 110‧‧‧ seed nozzle

120‧‧‧產物出口 120‧‧‧ product export

130‧‧‧絕緣層 130‧‧‧ Insulation

140‧‧‧內殼體 140‧‧‧Inner shell

141‧‧‧外表面 141‧‧‧outer surface

142‧‧‧內表面 142‧‧‧Inner surface

150‧‧‧襯墊 150‧‧‧ cushion

151‧‧‧內表面 151‧‧‧Inner surface

152‧‧‧表面 152‧‧‧ surface

154‧‧‧環狀底部表面 154‧‧‧Circular bottom surface

160‧‧‧內殼體膨脹裝置 160‧‧‧Inner shell expansion device

165‧‧‧膨脹彈簧 165‧‧‧Expansion spring

170‧‧‧基底 170‧‧‧ substrate

172‧‧‧頂部頭部 172‧‧‧Top head

180‧‧‧羽狀氣體 180‧‧‧feather gas

220‧‧‧下方密封支撐環 220‧‧‧ bottom seal support ring

230‧‧‧上方密封環 230‧‧‧upper seal ring

240‧‧‧環狀空間 240‧‧‧ annular space

241‧‧‧膨脹支撐體部件 241‧‧‧Expansion support body parts

242‧‧‧膨脹支撐體部件 242‧‧‧ Expansion support body parts

260‧‧‧外緣表面 260‧‧‧ outer edge surface

262‧‧‧內緣表面 262‧‧‧Inner edge surface

264‧‧‧中央開口 264‧‧‧Central opening

270‧‧‧上方部分 270‧‧‧upper

272‧‧‧下方部分 272‧‧‧below

274‧‧‧凸緣 274‧‧‧ flange

276‧‧‧突出表面 276‧‧‧ protruding surface

280‧‧‧密封環 280‧‧‧seal ring

282‧‧‧環狀內緣表面 282‧‧‧Circular inner edge surface

284‧‧‧開口 284‧‧‧ opening

285‧‧‧環狀頂部表面 285‧‧‧ annular top surface

286‧‧‧環狀底部表面 286‧‧‧ annular bottom surface

288‧‧‧圓形通道 288‧‧‧circular channel

290‧‧‧O型環 290‧‧‧O-ring

294‧‧‧環狀上方墊圈 294‧‧‧Ring ring washer

296‧‧‧環狀下方墊圈 296‧‧‧Ring under washer

300‧‧‧中間環 300‧‧‧ Middle Ring

304‧‧‧頂部表面 304‧‧‧Top surface

308‧‧‧開口通道 308‧‧‧open channel

310‧‧‧O型環 310‧‧‧O-ring

圖1所示的係一流化床反應器的概略剖面正視圖。 A schematic cross-sectional front view of the systemized bed reactor shown in FIG. 1.

圖2所示的係一流化床反應器的一部分的放大概略剖面正視圖,圖中描繪一外殼體、一絕緣層、一具有一內殼體膨脹裝置的內殼體、以及一襯墊。 An enlarged schematic cross-sectional front view of a portion of a systemized bed reactor shown in FIG. 2 depicts an outer shell, an insulating layer, an inner shell having an inner shell expansion device, and a gasket.

圖3所示的係圖2所示的流化床反應器的一部分的放大部分概略剖面正視圖,其描繪用於該內殼體與該襯墊的底部支撐系統的細節。 FIG. 3 is an enlarged partial schematic cross-sectional front view of a portion of the fluidized bed reactor shown in FIG. 2, which depicts details of a bottom support system for the inner casing and the liner.

圖4所示的係沿著圖3的直線4-4所獲得的部分剖視圖。 FIG. 4 is a partial cross-sectional view taken along line 4-4 of FIG. 3.

本文中揭示用於形成多晶矽的流化床反應器系統,其藉由熱分解一矽承載氣體並且將矽沉積在已流化的矽顆粒或是其它晶種顆粒(舉例來說,矽土顆粒、石墨顆粒、或石英顆粒)上。 A fluidized bed reactor system for forming polycrystalline silicon is disclosed herein, which thermally decomposes a silicon-bearing gas and deposits silicon on fluidized silicon particles or other seed particles (for example, silica particles, Graphite particles, or quartz particles).

有矽塗層的顆粒會藉由在一反應器腔室裡面熱分解一矽承載氣體並且在該腔室中的一流化床裡面將矽沉積在顆粒上。一開始,該沉積係在小型的晶種顆粒上。沉積會繼續進行,直到顆粒被成長至適合商業用途的大小為止,隨之,該些已成長的顆粒便會被取得。 The silicon-coated particles thermally decompose a silicon-bearing gas in a reactor chamber and deposit silicon on the particles in a first-class bed in the chamber. Initially, the deposition was on small seed particles. Deposition continues until the particles are grown to a size suitable for commercial use, and the grown particles are then obtained.

晶種顆粒可能有適合被矽塗佈的任何所希望的組成物。合宜的組成物不會熔化或蒸發,並且不會於出現在該反應器腔室中的條件下分解或是進行化學反應。合宜的晶種顆粒組成物的範例包含,但是並不限制於:矽、矽土、石墨、以及石英。 The seed particles may have any desired composition suitable for being coated with silicon. Convenient compositions do not melt or evaporate, and do not decompose or undergo a chemical reaction under the conditions present in the reactor chamber. Examples of suitable seed particle compositions include, but are not limited to: silicon, silica, graphite, and quartz.

矽會藉由分解選擇自由下面所組成的群之中的矽承載氣體而被沉積在該些顆粒上:矽烷(SiH4)、二矽烷(Si2H6)、較高階的矽烷(SinH2n+2)、二氯化矽烷(SiH2Cl2)、三氯化矽烷(SiHCl3)、四氯化矽(SiCl4)、二溴化矽烷(SiH2Br2)、三溴化矽烷(SiHBr3)、四溴化矽(SiBr4)、二碘化矽烷(SiH2I2)、三碘化矽烷(SiHI3)、四碘化矽(SiI4)、以及它們的混合物。該矽承載氣體可以與一或更多種含鹵素的氣體混合,含鹵素的氣體如由下面所組成的群之中的任一者的定義:氯氣(Cl2)、氯化氫(HCl)、溴氣(Br2)、溴化氫(HBr)、碘(I2)、碘化氫(HI)、以及它們的混合物。該矽承載氣體亦可以與一或更多種其它氣體混合,其包含氫氣(H2)或是選擇自下面的一或更多種惰性氣體:氮氣(N2)、 氦氣(He)、氬氣(Ar)、以及氖氣(Ne)。於特殊的實施例中,該矽承載氣體為矽烷,並且矽烷會與氫氣混合。 Silicon is deposited on these particles by decomposing the silicon-bearing gas in the group consisting of the following free choices: silane (SiH 4 ), disilane (Si 2 H 6 ), higher order silane (Si n H 2n + 2 ), silicon dichloride (SiH 2 Cl 2 ), silicon trichloride (SiHCl 3 ), silicon tetrachloride (SiCl 4 ), silicon dibromide (SiH 2 Br 2 ), silicon bromide (SiH 2 SiHBr 3 ), silicon tetrabromide (SiBr 4 ), silicon diiodide (SiH 2 I 2 ), silicon triiodide (SiHI 3 ), silicon tetraiodide (SiI 4 ), and mixtures thereof. The silicon-bearing gas may be mixed with one or more halogen-containing gases, as defined by any one of the following groups: chlorine (Cl 2 ), hydrogen chloride (HCl), bromine (Br 2 ), hydrogen bromide (HBr), iodine (I 2 ), hydrogen iodide (HI), and mixtures thereof. The silicon carrier gas can also be mixed with one or more other gases, including hydrogen (H 2 ) or one or more inert gases selected from the following: nitrogen (N 2 ), helium (He), argon Gas (Ar), and neon gas (Ne). In a special embodiment, the silicon carrier gas is silane, and the silane is mixed with hydrogen.

該矽承載氣體以及任何伴隨的氫氣、含鹵素的氣體、及/或惰性氣體會被引進一流化床反應器的中央腔室之中並且於該腔室裡面被熱分解,用以產生沉積在該腔室內部的晶種顆粒上的矽。 The silicon-bearing gas and any accompanying hydrogen, halogen-containing gas, and / or inert gas will be introduced into the central chamber of a first-class chemical bed reactor and thermally decomposed inside the chamber to produce a deposit on Silicon on seed particles inside the chamber.

圖1所示的係一有產物塗層的顆粒的流化床反應器10的通用結構。圖1的反應器雷同於WO2011063007 A2的反應器,其特別適用於藉由矽烷的熱分解所產生的矽產物。該反應器10包含一容器12,其從一基底170處大致上垂直地延伸至一頂部頭部172,該容器12有一垂直中央軸A1,並且可以在不同的高度有不同的剖面尺寸。圖1中所示的反應器有不同剖面尺寸的五個區域I至V。 The general structure of a fluidized bed reactor 10 shown in FIG. 1 is a product-coated particle. The reactor of FIG. 1 is similar to the reactor of WO2011063007 A2, which is particularly suitable for silicon products produced by thermal decomposition of silane. The reactor 10 includes a container 12 that extends substantially vertically from a base 170 to a top head 172. The container 12 has a vertical central axis A 1 and can have different cross-sectional dimensions at different heights. The reactor shown in Fig. 1 has five zones I to V of different cross-sectional dimensions.

反應器10有一外殼體80。一或更多個加熱器100於區域IV中被定位在外殼體80內側。於某些系統中,加熱器100為輻射加熱器。該反應器10還可以包含一內部床加熱器90。一絕緣層130被定位在外殼體80的內表面中。該絕緣層130熱絕緣外殼體80與輻射加熱器100。 The reactor 10 has an outer casing 80. One or more heaters 100 are positioned inside the outer casing 80 in the region IV. In some systems, the heater 100 is a radiant heater. The reactor 10 may also include an internal bed heater 90. An insulating layer 130 is positioned in the inner surface of the outer case 80. The insulating layer 130 thermally insulates the outer casing 80 and the radiant heater 100.

一內殼體140垂直延伸貫穿反應器10的區域II至V。圖中所示的內殼體大致上為具有大致上圓形剖面的圓柱形。該內殼體能夠由能夠耐受反應器10裡面的條件並且非常適用於被用來將熱傳輸至該流化床之中的高溫的任何合宜材料所構成。因為在該內殼體的內部與外部的壓力雷同,所以,該內殼體能夠很薄。於某些系統中,該內殼體的厚度為5mm至10mm,例如,6mm至8mm。 An inner shell 140 extends vertically through regions II to V of the reactor 10. The inner case shown in the figure is substantially cylindrical with a substantially circular cross section. The inner casing can be composed of any suitable material that can withstand the conditions inside the reactor 10 and is well suited to the high temperatures used to transfer heat into the fluidized bed. Since the pressure inside and outside the inner casing are the same, the inner casing can be thin. In some systems, the thickness of the inner casing is 5 mm to 10 mm, for example, 6 mm to 8 mm.

一可被移除的襯墊150被定位在該內殼體140裡面,位在和 該內殼體140的內表面142相隔一小距離處。圖中所示的襯墊150大致上為圓柱形,具有大致上圓形的剖面,內殼體140有同圓心,大致上垂直延伸貫穿區域II至V。襯墊150有一內表面151,其至少部分定義一反應器腔室15。 A removable pad 150 is positioned inside the inner case 140 between the and The inner surfaces 142 of the inner casing 140 are separated by a small distance. The gasket 150 shown in the figure is substantially cylindrical and has a substantially circular cross-section. The inner shell 140 has a concentric center and extends substantially vertically through the regions II to V. The liner 150 has an inner surface 151 which at least partially defines a reactor chamber 15.

襯墊150可圍阻該流化床並且將其與該反應器的其它器件分離。明確地說,襯墊150保護內殼體140,使其不會受到該流化床中的有矽塗層的顆粒以及晶種顆粒的磨擦,並且保護該些顆粒避免受到內殼體材料及/或容器壁部材料的污染。 The liner 150 may enclose the fluidized bed and separate it from other components of the reactor. Specifically, the gasket 150 protects the inner shell 140 from the friction of the silicon-coated particles and seed particles in the fluidized bed, and protects these particles from the inner shell material and / Or contamination of the container wall material.

襯墊150係由所構成經過選擇不會污染該些顆粒的材料所構成,並且較佳的係,由能夠承受1600℉(870℃)的溫度並且維持穩定性的材料所製成。適用於襯墊150的材料包含,但是並不限制於非污染的材料,其包含,但是並不限制於:石英、矽、低鎳合金、高溫合金、鈷合金、氮化矽、石墨、碳化矽、鉬、或是鉬合金。於特殊的系統中,該襯墊係由碳化矽、鉬、或是鉬合金所構成。碳化矽的優點係具有2.2-2.4x10-6/℉或者3.9-4.0x10-6/℃的低熱膨脹係數。 The pad 150 is made of a material selected not to contaminate the particles, and is preferably made of a material capable of withstanding a temperature of 1600 ° F (870 ° C) and maintaining stability. Suitable materials for the pad 150 include, but are not limited to, non-contaminating materials, which include, but are not limited to: quartz, silicon, low nickel alloy, high temperature alloy, cobalt alloy, silicon nitride, graphite, silicon carbide , Molybdenum, or molybdenum alloy. In special systems, the gasket is made of silicon carbide, molybdenum, or a molybdenum alloy. The advantage of silicon carbide is that it has a low thermal expansion coefficient of 2.2-2.4x10-6 / ° F or 3.9-4.0x10-6 / ° C.

圖2所示的係一改良的反應器系統的結構的外殼體80至其襯墊150,其包含一改良底部密封。該絕緣層130被設置在外殼體80旁邊並且被支撐在一下方密封支撐環220與一上方密封環230之間。該內殼體140被定位在該絕緣層130的內側並且受到下方密封支撐環220的支撐。該內殼體140有一外表面141與一內表面142。圖中所示的表面141、142有同圓心並且大致上為圓柱形,該內殼體140中該些表面叉開的底部部分除外。襯墊150被定位在該內殼體140的內側。在該內殼體140與襯墊150之間有 一窄的間隙,舉例來說,如圖中水平測得為1.5mm,以便允許水平熱膨脹。由於該間隙的關係,在該底部密封與該內殼體140的頂部之間存在一環狀空間240。於圖中所示的實施例中,該環狀空間240的側邊界係由圓形圓柱體的兩個垂直延伸的同心圓表面142、152所定義。該底部密封裝配件的各種器件共同提供一從該內殼體140延伸至該襯墊150的密封,用以阻隔氣體從反應器腔室15的底部進入介於該內殼體140與該襯墊150之間的空間240之中。 The outer shell 80 to the gasket 150 of the structure of a modified reactor system shown in FIG. 2 includes a modified bottom seal. The insulating layer 130 is disposed beside the outer casing 80 and is supported between a lower seal support ring 220 and an upper seal ring 230. The inner case 140 is positioned on the inner side of the insulating layer 130 and is supported by the lower sealing support ring 220. The inner casing 140 has an outer surface 141 and an inner surface 142. The surfaces 141 and 142 shown in the figure have concentric circles and are substantially cylindrical, except for the bottom portions of the inner shell 140 where the surfaces diverge. The pad 150 is positioned inside the inner case 140. There is a space between the inner case 140 and the pad 150 A narrow gap, for example, measured 1.5 mm horizontally in the figure to allow horizontal thermal expansion. Due to the gap, there is an annular space 240 between the bottom seal and the top of the inner case 140. In the embodiment shown in the figure, the side boundary of the annular space 240 is defined by two vertically extending concentric circular surfaces 142, 152 of a circular cylinder. The various components of the bottom seal assembly collectively provide a seal extending from the inner shell 140 to the gasket 150 to block gas from the bottom of the reactor chamber 15 from entering between the inner shell 140 and the gasket 150 between 240 and 240.

外殼體80、內殼體140、以及下方密封支撐環220中的每一者皆由適合耐受和加熱該流化床與冷卻該產物相關聯的溫度梯度的材料所構成。合宜的材料包含,但是並不限制於:奧氏體不銹鋼;高溫金屬合金,例如,INCOLOY®合金、INCONEL®合金;以及鈷合金,舉例來說,RENE®41。 Each of the outer casing 80, the inner casing 140, and the lower sealing support ring 220 is composed of a material suitable for withstanding and heating the temperature gradient associated with cooling the product with the fluidized bed. Suitable materials include, but are not limited to: austenitic stainless steel; high temperature metal alloys, such as INCOLOY ® alloys, INCONEL ® alloys; and cobalt alloys, for example, RENE ® 41.

多個輻射加熱器(圖中並未顯示)可以被設置在絕緣層130與內殼體140之間。 A plurality of radiant heaters (not shown) may be disposed between the insulating layer 130 and the inner case 140.

一膨脹接合系統包含一內殼體膨脹裝置160,其從該內殼體140的上方表面處向上延伸。內殼體膨脹裝置160能夠壓縮而在反應器10的操作期間允許該內殼體140的垂直熱膨脹。 An expansion joint system includes an inner casing expansion device 160 that extends upward from an upper surface of the inner casing 140. The inner casing expansion device 160 is capable of being compressed to allow vertical thermal expansion of the inner casing 140 during operation of the reactor 10.

圖中所示的內殼體膨脹裝置160延伸在該內殼體140與一膨脹支撐體之間。該膨脹支撐體包含部件241、242,它們牢牢地附接至上方密封環230。該膨脹接合系統會適應於該反應器的內殼體140與外殼體80的差異膨脹。圖中所示的內殼體膨脹裝置160為一大致上圓柱形的彈簧式裝置,其內徑雷同於內殼體140的內徑。該內殼體膨脹裝置160被配置成用以於內殼體140上施加向下壓力。於特定的系統中,該內殼體膨脹裝置160 為由扁線或波形彈簧所製成的螺旋線圈,也就是,由於金屬線中有波浪狀的扁線所製成的圓柱形堆疊。 The inner casing expansion device 160 shown in the figure extends between the inner casing 140 and an expansion support. The expansion support contains components 241, 242, which are firmly attached to the upper seal ring 230. The expansion joint system is adapted to the differential expansion of the inner shell 140 and the outer shell 80 of the reactor. The inner casing expansion device 160 shown in the figure is a substantially cylindrical spring-type device, and its inner diameter is the same as the inner diameter of the inner casing 140. The inner casing expansion device 160 is configured to apply a downward pressure on the inner casing 140. In a particular system, the inner casing expansion device 160 It is a spiral coil made of a flat wire or a wave spring, that is, a cylindrical stack made of wavy flat wires in a metal wire.

當該反應器裡面的溫度升高時,該內殼體140會膨脹並且內殼體膨脹裝置160會被向上推擠並且壓縮。當冷卻時,該內殼體140會收縮並且內殼體膨脹裝置160會擴展。內殼體膨脹裝置160還會於內殼體140上施加壓力。視情況,一膨脹彈簧165可被提供於該襯墊150上方,以便適應於該襯墊的熱膨脹。 When the temperature inside the reactor rises, the inner shell 140 will expand and the inner shell expansion device 160 will be pushed upward and compressed. When cooled, the inner casing 140 will shrink and the inner casing expansion device 160 will expand. The inner casing expansion device 160 also applies pressure on the inner casing 140. Optionally, an expansion spring 165 may be provided above the pad 150 to accommodate the thermal expansion of the pad.

內殼體140與襯墊150的下方末端部分受到支撐與密封,使得氣體不會從該流化床處流至介於該內殼體與該襯墊之間的環狀空間240之中。襯墊150有一環狀底部表面154,其被研磨為光滑且平坦以便幫助形成一良好的底部密封。於圖中所示的系統中,襯墊150的底部表面154大致上水平延伸。 The lower end portions of the inner casing 140 and the gasket 150 are supported and sealed, so that gas does not flow from the fluidized bed into the annular space 240 between the inner casing and the gasket. The gasket 150 has an annular bottom surface 154 that is ground to be smooth and flat to help form a good bottom seal. In the system shown in the figure, the bottom surface 154 of the pad 150 extends substantially horizontally.

圖3更詳細地顯示圖2的底部密封配置。於圖中所示的配置中,該襯墊150受到該內殼體140支撐並且一或更多個墊圈被提供在該襯墊150與該內殼體140之間,以便提供一氣密式密封。一支撐部件(例如,圖中所示的下方密封支撐環220)為環狀形狀,在基底170上方的某個高度處被附接至外殼體80,從該外殼體80處以凸緣的方式向內延伸,並且支撐該內殼體140。該下方密封支撐環220有一外緣表面260與一內緣表面262,該外緣表面260面向該外殼體80並且該內緣表面262定義一大致上垂直延伸的中央開口264,表示在圖4之中,貫穿該下方密封支撐環220。該內殼體140有一上方部分270與一下方部分272。圖中所示的下方部分272有一座落在該密封支撐環220上的扁平底部表面。該下方部分272包含一凸緣274,其 相對於該上方部分270徑向向內突出,該凸緣274有一大致上水平、面朝上的突出表面276。襯墊150受到該突出表面276的支撐。於圖3中所示的有利配置中,內殼體140的下方部分272從水平處測量厚於上方部分270。下方部分272的較大厚度提供該內殼體140一較寬廣的基底座落在該密封支撐環220上。優點係,該下方部分272夠厚,使得該內殼體140的基底能夠定義鑽孔以接收螺栓,或者能夠支撐短釘以便將該內殼體固定至該容器,例如,固定至密封支撐環220。於圖中所示的系統中,該外表面141朝內殼體140的底部向外開展,用以提供額外的厚度。 FIG. 3 shows the bottom seal configuration of FIG. 2 in more detail. In the configuration shown in the figure, the gasket 150 is supported by the inner casing 140 and one or more gaskets are provided between the gasket 150 and the inner casing 140 to provide an air-tight seal. A support member (for example, the lower seal support ring 220 shown in the figure) is ring-shaped, and is attached to the outer casing 80 at a height above the base 170, and is flanged from the outer casing 80 toward It extends inwardly and supports the inner case 140. The lower sealing support ring 220 has an outer edge surface 260 and an inner edge surface 262. The outer edge surface 260 faces the outer casing 80 and the inner edge surface 262 defines a central opening 264 extending substantially vertically, as shown in FIG. In the middle, the lower support ring 220 is penetrated. The inner case 140 has an upper portion 270 and a lower portion 272. The lower portion 272 shown in the figure has a flat bottom surface that falls on the sealing support ring 220. The lower portion 272 includes a flange 274, which Radially inwardly protruding from the upper portion 270, the flange 274 has a generally horizontal, upwardly-facing protruding surface 276. The pad 150 is supported by the protruding surface 276. In the advantageous configuration shown in FIG. 3, the lower portion 272 of the inner case 140 is thicker than the upper portion 270 as measured from the horizontal. The larger thickness of the lower portion 272 provides a wider base of the inner shell 140 to fall on the sealing support ring 220. The advantage is that the lower portion 272 is thick enough so that the base of the inner casing 140 can define a drilled hole to receive bolts, or can support short nails to secure the inner casing to the container, for example, to a sealing support ring 220 . In the system shown in the figure, the outer surface 141 extends outward toward the bottom of the inner shell 140 to provide additional thickness.

於圖中所示的系統中,一環狀部件被連接至內殼體140,用以為襯墊150提供支撐。圖中所示的該環狀部件為一密封環280,其位在該襯墊150與該突出表面276之間,該密封環280受到該突出表面276的支撐並且該襯墊150受到該密封環280的支撐。該密封環280有一環狀頂部表面285與一環狀底部表面286,兩個表面大致上為扁平並且大致上水平延伸。該密封環280還具有一環狀內緣表面282,其定義一大致上垂直延伸的開口284,表示在圖4之中,貫穿密封環280。該密封環280可以為鐵素體不銹鋼(ferritic stainless steel),例如,410級的不銹鋼。 In the system shown in the figure, a ring-shaped member is connected to the inner case 140 to provide support for the pad 150. The annular member shown in the figure is a sealing ring 280 between the gasket 150 and the protruding surface 276. The sealing ring 280 is supported by the protruding surface 276 and the gasket 150 is received by the sealing ring. 280 support. The sealing ring 280 has a ring-shaped top surface 285 and a ring-shaped bottom surface 286. The two surfaces are substantially flat and extend substantially horizontally. The sealing ring 280 also has an annular inner edge surface 282 which defines an opening 284 extending substantially vertically, and is shown in FIG. 4 and penetrates the sealing ring 280. The sealing ring 280 may be ferritic stainless steel, for example, 410 grade stainless steel.

密封環280的頂部表面285定義至少一環狀向上的開口通道。在圖3至4中所示的系統中,該頂部表面285定義一圓形通道288。一O型環290,有時候亦稱為「上方O型環」,被提供在該環狀向上的開口通道288之中。該O型環扣接位在該O型環上方與下方的表面,用以形成一介於該些表面之間的密封。於替代例中,複數條通道會被提供在頂部表面285之中;複數個O型環會被提供在襯墊150與密封環280之間。該O型環 290可以由任何合宜的材料所製成。明確地說,O型環290可以為中空核心的不銹鋼,或者,可以為一全氟彈性體材料,例如,DuPontTM Kalrez®全氟彈性體(FFKM)。 The top surface 285 of the sealing ring 280 defines at least one annular upward open channel. In the system shown in FIGS. 3 to 4, the top surface 285 defines a circular channel 288. An O-ring 290, sometimes referred to as an "upper O-ring", is provided in the annular upwardly-opening channel 288. The O-ring buckle is located on the surface above and below the O-ring to form a seal between the surfaces. In the alternative, a plurality of channels may be provided in the top surface 285; a plurality of O-rings may be provided between the gasket 150 and the sealing ring 280. The O-ring 290 may be made of any suitable material. In particular, O-ring 290 may be a stainless steel hollow core, or may be a perfluoro elastomeric material, e.g., DuPont TM Kalrez ® perfluoroelastomer (FFKM).

該系統還可以包含一環狀的中間環300,在圖3中會清楚看見。圖中所示的中間環300位在密封環280與突出表面276之間,該中間環300受到該突出表面276的支撐並且該密封環280受到該中間環300的支撐。圖中所示的中間環有一頂部表面304,其定義至少一環狀向上的開口通道308。一O型環310,有時候亦稱為「下方O型環」,被提供在該些環狀向上的開口通道308的一或更多者之中。該O型環扣接位在該O型環上方與下方的表面,用以形成一介於該些表面之間的密封。於圖3至4的實施例中,一O型環310被提供在一通道308之中。於替代例中,複數條通道308會被提供;複數個O型環會被提供。該O型環310可以由聚合物所製成,例如,DuPontTM Viton®含氟彈性體,或者,可以為一全氟彈性體材料,例如,DuPontTM Kalrez®全氟彈性體(FFKM)。 The system may also include a ring-shaped intermediate ring 300, which will be clearly seen in FIG. The intermediate ring 300 shown in the figure is located between the sealing ring 280 and the protruding surface 276. The intermediate ring 300 is supported by the protruding surface 276 and the sealing ring 280 is supported by the intermediate ring 300. The intermediate ring shown in the figure has a top surface 304 which defines at least one annular upwardly-opening channel 308. An O-ring 310, sometimes also referred to as a "lower O-ring", is provided in one or more of the annular upward opening channels 308. The O-ring buckle is located on the surface above and below the O-ring to form a seal between the surfaces. In the embodiments of FIGS. 3 to 4, an O-ring 310 is provided in a channel 308. In the alternative, a plurality of channels 308 may be provided; a plurality of O-rings may be provided. The O-ring 310 may be made from a polymer, e.g., DuPont TM Viton ® fluoroelastomers, or may be a perfluoro elastomeric material, e.g., DuPont TM Kalrez ® perfluoroelastomer (FFKM).

於圖中所示的實施例中,一環狀上方墊圈294位在密封環280與襯墊150之間,主要用以保護該O型環不會受到肇因於接觸襯墊150的下方表面154的磨損。一環狀下方墊圈296位在密封環280與突出表面276之間。明確地說,環狀上方墊圈294位在密封環280的頂部表面285與襯墊150之間;環狀下方墊圈296位在密封環280的底部表面286與突出表面276之間。此些墊圈通常為非必要並且可以省略。但是,墊圈294、296中的一或兩者可於必要時被提供。該些墊圈可以由石墨材料所製成,例如,GRAFOIL®撓性石墨墊圈材料,其有充分的剛性使得該些墊圈不會在反應器 的操作期間往旁邊滑動。於沒有上方墊圈294的系統中,襯墊150的下方表面154座落在密封環280的頂部表面285上,該一或更多個O型環290會接觸並且在該襯墊150與該密封環280之間形成一密封。於沒有下方墊圈296的系統中,密封環280的底部表面286座落在中間環300的頂部上,該一或更多個O型環310會接觸並且在該密封環280與該中間環300之間形成一密封。 In the embodiment shown in the figure, a ring-shaped upper washer 294 is located between the sealing ring 280 and the gasket 150, and is mainly used to protect the O-ring from being caused by the lower surface 154 of the contact gasket 150. Wear and tear. An annular lower washer 296 is positioned between the seal ring 280 and the protruding surface 276. Specifically, the annular upper washer 294 is located between the top surface 285 of the seal ring 280 and the gasket 150; the annular lower washer 296 is located between the bottom surface 286 and the protruding surface 276 of the seal ring 280. Such gaskets are usually unnecessary and can be omitted. However, one or both of the washers 294, 296 may be provided if necessary. The plurality of washer may be made of graphite material, e.g., GRAFOIL ® graphite gasket material is flexible, it has sufficient rigidity such that the plurality of gasket does not slide sideways during operation of the reactor. In a system without an upper washer 294, the lower surface 154 of the gasket 150 is seated on the top surface 285 of the sealing ring 280, and the one or more O-rings 290 are in contact with the gasket 150 and the sealing ring A seal is formed between 280. In a system without a lower gasket 296, the bottom surface 286 of the seal ring 280 sits on top of the intermediate ring 300, and the one or more O-rings 310 will contact and seal the seal ring 280 with the intermediate ring 300. A seal is formed between them.

一入口噴嘴20被提供用以經由一中央路徑22注入一主要氣體以及經由一圍繞中央路徑22的環狀路徑24注入一次要氣體。優點係,噴嘴20被定位為使得矽烷被注入在反應器10的垂直中央軸A1附近的羽狀氣體(plume)180之中。於特殊的配置中,中央入口噴嘴20包括兩個實質上圓柱形的管狀部,其具有實質上圓形的剖面。該主要氣體為矽承載氣體,或者為矽承載氣體、氫氣、及/或惰性氣體(舉例來說,氦氣、氬氣)的混合物。該主要氣體亦可能包含含鹵素的氣體。該次要氣體通常具有和主要氣體混合物中的氫氣及/或惰性氣體實質上相同的組成物。於特殊的配置中,該主要氣體為矽烷與氫氣的混合物,而該次要氣體為氫氣。 An inlet nozzle 20 is provided to inject a primary gas via a central path 22 and a secondary gas via an annular path 24 surrounding the central path 22. The advantage is that the nozzle 20 is positioned so that the silane is injected into a plume 180 near the vertical central axis A 1 of the reactor 10. In a special configuration, the central inlet nozzle 20 includes two substantially cylindrical tubular portions having a substantially circular cross-section. The main gas is a silicon-bearing gas, or a mixture of a silicon-bearing gas, hydrogen, and / or an inert gas (for example, helium, argon). The main gas may also contain a halogen-containing gas. The secondary gas typically has a composition that is substantially the same as the hydrogen and / or inert gas in the primary gas mixture. In a special configuration, the primary gas is a mixture of silane and hydrogen, and the secondary gas is hydrogen.

圖中所示的反應器10進一步包含複數個流化氣體噴嘴40。額外的氫氣及/或惰性氣體能夠經由該些流化噴嘴40被傳送至該反應器之中,用以提供充分的氣流來流化該反應器床裡面的顆粒。 The reactor 10 shown in the figure further includes a plurality of fluidizing gas nozzles 40. Additional hydrogen and / or inert gas can be transferred into the reactor through the fluidizing nozzles 40 to provide a sufficient gas flow to fluidize the particles in the reactor bed.

本發明還提供:一取樣噴嘴50,產物會經由該取樣噴嘴被取樣;以及一或更多個壓力噴嘴60,用以監視該反應器裡面的壓力,該些噴嘴從該中央入口噴嘴20處橫向移開。一或更多個淨化氣體/冷卻氣體噴嘴70、72位在流化噴嘴40下方並且徑向延伸貫穿外殼體80並且進入反應器 10之中。 The present invention also provides: a sampling nozzle 50 through which the product is sampled; and one or more pressure nozzles 60 for monitoring the pressure in the reactor, the nozzles transversely from the central inlet nozzle 20 Move away. One or more purge gas / cooling gas nozzles 70, 72 are located below the fluidization nozzle 40 and extend radially through the outer shell 80 and into the reactor 10 out of 10.

反應器10有一晶種噴嘴110,晶種顆粒會經由該噴嘴被引進至該反應器腔室15之中。該反應器10還具有一或更多個產物出口120,用以從反應器腔室15處移除有矽塗層的顆粒。 The reactor 10 has a seed nozzle 110 through which seed particles are introduced into the reactor chamber 15. The reactor 10 also has one or more product outlets 120 for removing silicon-coated particles from the reactor chamber 15.

在操作中,一晶種顆粒床被提供在反應器腔室內側並且被經由唯一的中央入口噴嘴20以及該些增補的流化噴嘴40所注入的氣體流化。反應器腔室15的內含物會被加熱。該矽承載氣體會分解並且沉積矽在該流化床中的晶種顆粒。冷卻氣體會經由冷卻氣體噴嘴70、72被引進至該腔室15之中。 In operation, a seed particle bed is provided inside the reactor chamber and is fluidized by the gas injected through the sole central inlet nozzle 20 and the supplemental fluidization nozzles 40. The contents of the reactor chamber 15 are heated. The silicon bearing gas decomposes and deposits seed particles of silicon in the fluidized bed. The cooling gas is introduced into the chamber 15 through the cooling gas nozzles 70 and 72.

應該瞭解的係,圖中所示的反應器僅為範例並且不應該被視為限制本發明的範疇。確切地說,本發明的範疇係由下面的申請專利範圍來定義。 It should be understood that the reactors shown in the figures are merely examples and should not be considered as limiting the scope of the invention. Specifically, the scope of the present invention is defined by the following patent application scope.

Claims (17)

一種矽沉積反應器的系統,其包括:一容器,其具有一基底、一頂部頭部、以及一管狀的外殼體,該外殼體垂直延伸在該基底與該頂部頭部之間;一管狀的內殼體,其位在該外殼體內側,該內殼體垂直延伸並且受到該容器的支撐;一管狀的襯墊,其位在該內殼體內側,該襯墊垂直延伸並且受到該內殼體支撐,該襯墊有一內表面,該內表面至少部分定義一腔室,該腔室適合在一流化床中含有複數個矽顆粒,其中該內殼體具有一上方部分與一下方部分,該下方部分包含一凸緣,其相對於該上方部分徑向向內突出,該凸緣有一水平、面朝上的突出表面,以及該襯墊受到該突出表面的支撐;至少一噴嘴,用以注入氣體至該腔室之中;至少一出口,用以從該腔室處移除氣體;以及一密封環,其位在該襯墊與該突出表面之間,使得該密封環受到該突出表面的支撐並且該襯墊受到該密封環的支撐,該密封環具有一環狀內緣表面,其定義一垂直延伸且貫穿該密封環的開口。A system for a silicon deposition reactor, comprising: a container having a base, a top head, and a tubular outer shell, the outer shell extending vertically between the base and the top head; a tubular An inner shell positioned inside the outer shell, the inner shell extending vertically and supported by the container; a tubular gasket positioned inside the inner shell, the gasket extending vertically and receiving the inner shell The cushion has an inner surface which at least partially defines a chamber. The chamber is suitable for containing a plurality of silicon particles in a first-rate bed. The inner shell has an upper portion and a lower portion. The lower portion includes a flange that projects radially inwardly with respect to the upper portion, the flange has a horizontal, upward-facing protruding surface, and the pad is supported by the protruding surface; at least one nozzle for Injecting gas into the chamber; at least one outlet for removing the gas from the chamber; and a sealing ring positioned between the gasket and the protruding surface so that the sealing ring is subjected to the protruding surface Branch And the pad is supported in the seal ring, the seal ring having an annular inner peripheral surface that defines a vertically extending through opening and the seal ring. 根據申請專利範圍第1項的系統,其中:該密封環具有一環狀頂部表面與一環狀底部表面;該密封環的該頂部表面定義至少一環狀向上的開口通道;以及一O型環位在該至少一環狀向上的開口通道之中,用以在該襯墊與該密封環之間提供一密封。The system according to item 1 of the scope of patent application, wherein: the sealing ring has an annular top surface and an annular bottom surface; the top surface of the sealing ring defines at least one annular upward opening channel; and an O-ring It is located in the at least one annular upward opening channel for providing a seal between the gasket and the seal ring. 根據申請專利範圍第1項的系統,其進一步包括一上方墊圈,其位在該密封環與該襯墊之間。According to the system of claim 1, it further includes an upper gasket between the seal ring and the gasket. 根據申請專利範圍第1項的系統,其進一步包括一下方墊圈,其位在該密封環與該突出表面之間。According to the system of claim 1, it further includes a lower gasket between the sealing ring and the protruding surface. 根據申請專利範圍第4項的系統,其中,該下方墊圈位在該密封環的底部表面與該突出表面之間。The system according to item 4 of the patent application, wherein the lower gasket is located between the bottom surface of the seal ring and the protruding surface. 根據申請專利範圍第1項的系統,其進一步包括一中間環,其位在該密封環與該突出表面之間,該中間環受到該突出表面的支撐且該密封環受到該中間環的支撐。According to the system of claim 1, it further includes an intermediate ring located between the sealing ring and the protruding surface, the intermediate ring is supported by the protruding surface and the sealing ring is supported by the intermediate ring. 根據申請專利範圍第6項的系統,其中:該中間環具有一環狀頂部表面,其定義至少一環狀向上的開口通道;以及一O型環位在該至少一環狀向上的開口通道之中。The system according to item 6 of the patent application, wherein: the intermediate ring has a ring-shaped top surface defining at least one ring-shaped open channel; and an O-ring is positioned in the at least one ring-shaped open channel. in. 根據申請專利範圍第7項的系統,其進一步包括一下方墊圈,其位在該密封環與該O型環之間,該O型環位在該中間環的該至少一環狀向上的開口通道之中。The system according to item 7 of the patent application scope, further comprising a lower gasket positioned between the sealing ring and the O-ring, the O-ring positioned in the at least one annular upward open channel of the intermediate ring In. 一種矽沉積反應器的系統,其包括:一容器,其具有一基底、一頂部頭部、以及一管狀的外殼體,該外殼體垂直延伸在該基底與該頂部頭部之間;一管狀的內殼體,其位在該外殼體內側,該內殼體垂直延伸,受到該容器的支撐,並且具有一內表面;一管狀的襯墊,其位在該內殼體內側,該襯墊垂直延伸,該襯墊具有一外表面,該外表面與該內殼體的內表面隔開使得一管狀的空間被定義在該內殼體與該襯墊之間,該襯墊有一內表面,其至少部分定義一腔室,該腔室適合在一流化床中含有複數個矽顆粒,並且該襯墊在其底部附近的一位置處被一O型環密封密封至該內殼體,使得氣體無法從該腔室處進入該空間,其中該內殼體具有一上方部分與一下方部分,該下方部分包含一凸緣,其相對於該上方部分徑向向內突出,該凸緣有一水平、面朝上的突出表面,以及該襯墊受到該突出表面的支撐;至少一噴嘴,用以注入氣體至該腔室之中;至少一出口,用以從該腔室處移除氣體;以及連接至該內殼體的一環狀部件,該環狀部件係位在該襯墊與該內殼體之間的一密封環,該襯墊受到該密封環的支撐,該密封環具有一環狀內緣表面,其定義一垂直延伸且貫穿該密封環的開口。A system for a silicon deposition reactor, comprising: a container having a base, a top head, and a tubular outer shell, the outer shell extending vertically between the base and the top head; a tubular An inner shell located inside the outer shell, the inner shell extending vertically, supported by the container, and having an inner surface; a tubular gasket positioned inside the inner shell, the gasket being vertical Extending, the pad has an outer surface, the outer surface is separated from the inner surface of the inner casing so that a tubular space is defined between the inner casing and the pad, the pad has an inner surface, which A chamber is defined at least in part, the chamber is suitable for containing a plurality of silicon particles in a first-rate bed, and the gasket is hermetically sealed to the inner casing by an O-ring at a position near the bottom thereof, so that the gas The space cannot be accessed from the chamber, wherein the inner casing has an upper portion and a lower portion, the lower portion includes a flange that projects radially inwardly with respect to the upper portion, and the flange has a horizontal, Protruding surface facing up, And the pad is supported by the protruding surface; at least one nozzle for injecting gas into the chamber; at least one outlet for removing gas from the chamber; and a connection to the inner casing A ring-shaped member, which is a sealing ring located between the gasket and the inner casing, the gasket is supported by the sealing ring, and the sealing ring has a ring-shaped inner edge surface, which defines a An opening extending vertically through the seal ring. 根據申請專利範圍第9項的矽沉積反應器的系統,其中:該O型環密封包括至少一O型環,其被定位以在該襯墊與該內殼體之間提供一密封,或是在該襯墊與連接至該內殼體的該環狀部件之間提供一密封。A system for a silicon deposition reactor according to claim 9 in which the O-ring seal includes at least one O-ring positioned to provide a seal between the gasket and the inner housing, or A seal is provided between the gasket and the annular member connected to the inner case. 根據申請專利範圍第9項的矽沉積反應器的系統,其中:該密封環具有一環狀頂部表面與一環狀底部表面;該密封環的該頂部表面定義至少一環狀向上的開口通道;以及一O型環位在該至少一環狀向上的開口通道之中,用以在該襯墊與該密封環之間提供一密封。The system for a silicon deposition reactor according to item 9 of the application, wherein: the seal ring has a ring-shaped top surface and a ring-shaped bottom surface; the top surface of the seal ring defines at least one ring-shaped upward opening channel; And an O-ring is located in the at least one annular upwardly-opening channel to provide a seal between the gasket and the sealing ring. 根據申請專利範圍第9項的矽沉積反應器的系統,其進一步包括一上方墊圈,其位在該密封環與該襯墊之間。The system for a silicon deposition reactor according to item 9 of the application, further comprising an upper gasket positioned between the seal ring and the gasket. 根據申請專利範圍第9項的矽沉積反應器的系統,其進一步包括一下方墊圈,其位在該密封環與該內殼體之間。According to the system of claim 9, the system further includes a lower gasket, which is positioned between the sealing ring and the inner casing. 根據申請專利範圍第9項的矽沉積反應器的系統,其進一步包括一中間環,其位在該密封環與該內殼體之間,該密封環受到該中間環的支撐。According to the system of claim 9 of the patent application scope, the system further includes an intermediate ring located between the sealing ring and the inner casing, and the sealing ring is supported by the intermediate ring. 根據申請專利範圍第14項的矽沉積反應器的系統,其中:該中間環具有一環狀頂部表面,其定義至少一環狀向上的開口通道;以及該系統進一步包括一O型環,其位在該至少一環狀向上的開口通道之中,用以在該密封環與該中間環之間提供一密封。A system for a silicon deposition reactor according to item 14 of the patent application, wherein: the intermediate ring has a ring-shaped top surface defining at least one ring-shaped upward open channel; and the system further includes an O-ring, In the at least one annular upward opening channel, a seal is provided between the seal ring and the intermediate ring. 根據申請專利範圍第15項的矽沉積反應器的系統,其進一步包括一下方墊圈,其位在該密封環與該O型環之間,該O型環位在該中間環的該至少一環狀向上的開口通道之中。According to the system of claim 15 of the patent application scope, the system further includes a lower gasket located between the sealing ring and the O-ring, and the O-ring is located in the at least one ring of the intermediate ring. Shape upward opening channel. 根據申請專利範圍第9項的矽沉積反應器的系統,其中,該O型環密封位在該內殼體與該密封環之間。The system of the silicon deposition reactor according to item 9 of the application, wherein the O-ring seal is located between the inner shell and the seal ring.
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