Classifications

• • C—CHEMISTRY; METALLURGY
  • C30—CRYSTAL GROWTH
  • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
  • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
  • C30B29/02—Elements
  • C30B29/06—Silicon
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
  • B01J8/1809—Controlling processes
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
  • B01J8/1818—Feeding of the fluidising gas
  • B01J8/1827—Feeding of the fluidising gas the fluidising gas being a reactant
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
  • B01J8/1836—Heating and cooling the reactor
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
  • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
  • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
  • B01J8/34—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with stationary packing material in the fluidised bed, e.g. bricks, wire rings, baffles
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B33/00—Silicon; Compounds thereof
  • C01B33/02—Silicon
  • C01B33/021—Preparation
  • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
• • C—CHEMISTRY; METALLURGY
  • C30—CRYSTAL GROWTH
  • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
  • C30B28/00—Production of homogeneous polycrystalline material with defined structure
  • C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
  • C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
• • C—CHEMISTRY; METALLURGY
  • C30—CRYSTAL GROWTH
  • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
  • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
• • 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
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00008—Controlling the process
  • B01J2208/00017—Controlling the temperature
  • B01J2208/00389—Controlling the temperature using electric heating or cooling elements
  • B01J2208/00398—Controlling the temperature using electric heating or cooling elements inside the reactor bed
• • 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
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00008—Controlling the process
  • B01J2208/00017—Controlling the temperature
  • B01J2208/00389—Controlling the temperature using electric heating or cooling elements
  • B01J2208/00407—Controlling the temperature using electric heating or cooling elements outside the reactor bed
• • 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
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00008—Controlling the process
  • B01J2208/00017—Controlling the temperature
  • B01J2208/00389—Controlling the temperature using electric heating or cooling elements
  • B01J2208/00415—Controlling the temperature using electric heating or cooling elements electric resistance heaters
• • 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
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00008—Controlling the process
  • B01J2208/00017—Controlling the temperature
  • B01J2208/00477—Controlling the temperature by thermal insulation means
  • B01J2208/00495—Controlling the temperature by thermal insulation means using insulating materials or refractories
• • 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
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00008—Controlling the process
  • B01J2208/00539—Pressure
• • 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
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00796—Details of the reactor or of the particulate material
  • B01J2208/00823—Mixing elements
  • B01J2208/00831—Stationary elements
  • B01J2208/0084—Stationary elements inside the bed, e.g. baffles
• • 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
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00796—Details of the reactor or of the particulate material
  • B01J2208/00991—Disengagement zone in fluidised-bed reactors
• • 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
  • B01J2219/0209—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components of glass
• • 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
  • B01J2219/0218—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components of ceramic
• • 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
• • 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
  • B01J2219/025—Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
  • B01J2219/0254—Glass
• • 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
  • B01J2219/025—Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
  • B01J2219/0272—Graphite
• • 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
  • B01J2219/025—Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
  • B01J2219/0277—Metal based
  • B01J2219/029—Non-ferrous metals

Definitions

• the present invention relates to a method for preparation of polycrystalline
• High purity polycrystalline silicon is widely used as a chemical or an
• the polycrystalline silicon is prepared by thermal decomposition
• bell-jar type reactor is rod-shaped and has a diameter of about 50-300 mm.
• the bell-jar type reactor which consists fundamentally of the electric resistance
• SiH 4 monosilane
• SiHaCb dichlorosilane
• SiHCb trichlorosilane
• silicon-containing reaction gas which can further comprise at least one gas
• component selected from hydrogen, nitrogen, argon, helium, etc.
• reactor yields polycrystalline silicon product in the form of particles, that is, granules.
• the seed crystals may be any material that lose fluidity and ultimately being moved downwards.
• the seed crystals may be any material that lose fluidity and ultimately being moved downwards.
• the seed crystals may be any material that lose fluidity and ultimately being moved downwards.
• the seed crystals may be any material that lose fluidity and ultimately being moved downwards.
• polycrystalline silicon product may be discharged from the lower part of the reactor
• processing for the follow-up processes such as single crystal growth, crystal block
• Silicon deposition occurs and is accumulated on the hot solid surfaces inside
• the fluidized bed reactor including the silicon particles, the inner wall of the reactor
• the thickness of the accumulated deposition layer increases with time.
• thickness of the silicon deposition layer gradually increases on the surfaces of the
• reaction gas supplying means exposed to or in contact with the high-temperature
• This method using an etching gas may also be applied to the removal of
• an inert gas as hydrogen, nitrogen, argon, helium or a mixture thereof
• the reactor tube tends to break when the reactor is cooled because of the
• Fig. 1 schematically illustrates the method for preparing granular polycrystalline silicon in accordance with the present invention.
• Fig. 2 schematically illustrates the silicon particle preparation step of the
• Fig. 3 schematically illustrates the silicon deposit removal step of the present
• Fig. 4 schematically illustrates another example of the silicon particle
• Fig. 5 schematically illustrates another example of the silicon deposit
• Fig. 6 schematically illustrates the various constructions of the fluidized bed
• Fig. 7 schematically illustrates another various constructions of the fluidized
• An object of the present invention is to provide a method for continual
• the present invention provides a
• reaction gas supplying means that supplies a silicon-containing reaction gas so that
• silicon deposition may occur while the bed of silicon particles formed inside a
• reactor tube remains fluidized, is located inside of the bed of silicon particles and,
• reaction zone provided for silicon deposition
• reaction gas and a heating zone provided for heating the silicon particles
• reaction gas supplying means so that silicon deposition occurs on the surface of
• the present invention also relates to a method for preparation of
• polycrystalline silicon which further comprises (iv) a silicon particle replenishing
• silicon particles are replenished into the reactor tube to form a bed of
• the present invention also relates to a method for preparation of
• the present invention also relates to a method for preparation of
• polycrystalline silicon in which the fluidized bed reactor comprises a reactor shell
• reactor shell is defined as an outer zone where the bed of silicon particles is
• the present invention also relates to a method for preparation of polycrystalline silicon in which (i) the silicon particle preparation step comprises the
• reaction zone becomes fluidized
• the present invention also relates to a method for preparation of
• nitrogen, argon and helium is supplied to the outer zone in order to maintain the
• the present invention also relates to a method for preparation of
• the present invention also relates to a method for preparation of
• the present invention also relates to a method for preparation of
• etching gas further comprises at least one
• the present invention also relates to a method for preparation of
• polycrystalline silicon in which, in (i) the silicon particle preparation step and/ or (iii)
• the absolute pressure at the reaction zone is
• the present invention also relates to a method for preparation of
• reaction gas supplying means using the etching gas is a reaction gas supplying means using the etching gas.
• the present invention also relates to a method for preparation of
• the present invention also relates to a method for preparation of polycrystalline silicon in which, in (iii) the silicon deposit removal step, a fluidizing
• the present invention also relates to a method for preparation of
• the present invention also relates to a method for preparation of
• fluidized by the fluidizing gas is formed in addition to the bed of silicon particles at
• the present invention also relates to a method for preparation of
• step off-gas including the fluidizing gas being passed through the bed of silicon
• the present invention also relates to a method for preparation of
• reaction gas comprises at least one silicon- containing substance selected from monosilane (SiHU), dichlorosilane (SiHaCb),
• SiHCb trichlorosilane
• SiCl 4 silicon tetrachloride
• the present invention also relates to a method for preparation of
• the present invention also relates to a method for preparation of
• reaction gas (llr) so that silicon deposition may occur while the bed of
• reaction zone (Z r ) provided for the silicon deposition reaction (Rd) by the reaction
• reaction gas (llr) silicon deposition also occurs at the reactor components
• step can be sustained for from a few days to several weeks.
• present invention makes it possible to resume silicon deposition after removing the
• step is followed by a silicon particle partial discharging step, wherein, without
• reaction gas supplying means (15r) may also be removed by its natural contact with
• reaction gas outlet of the reaction gas As described hereinbefore, the reaction gas outlet of the reaction gas
• reaction zone (Z r ) provided for silicon deposition reaction (Rd) by the reaction gas
• product particles are prepared by silicon deposition on the surface of the silicon
• the present invention comprises a
• reaction gas. (llr) a part of the silicon particles (3) is discharged out of the fluidized
• reactor tube (2) does not exceed the height of the outlet, and a silicon deposit
• tube (2) is substantially removed with the etching gas via the silicon deposit removal
• reactor tube (2) to form a bed of silicon particles (3) in the reaction zone (Z r ).
• the present invention may ultimately provide a method for
• the silicon deposit removal step may be
• the silicon particle partial discharging step is smaller than the total amount of the
• silicon particle replenishing step is very short as compared with that required for the
• the reactor needs not be disassembled and the reactor tube (2) can be
• the present invention can be applied to any type of
• a reactor tube for example, as schematically illustrated in Fig. 4 and Fig. 5, a reactor tube
• reactor tube (2) is defined as an inner zone (4) where the bed of silicon particles (3) is
• the inner zone (4) includes a heating zone (Zh) and a reaction zone (Z r ).
• the silicon particle preparation step executed using the fluidized bed reactor
• the etching gas (lie) may
• reaction gas supplying means as an etching gas supplying means (15e), as
• reaction gas (llr) may be constructed such that the reaction gas (llr) and the
• etching gas (lie) can pass through the same route or nozzles, or such that the
• reaction gas (llr) and the etching gas (He) can pass through different routes or
• the etching gas (He) may be supplied using an etching gas supplying means (15e) which is equipped
• the silicon deposit removal step may be carried out by supplying the
• the present invention is characterized in that the bed of silicon particles (3) is
• silicon particles (3) be formed not only in the heating zone (Zh) but also in the
• reaction zone (Z r ) and that the silicon particles (3) in the two zones can be mixed
• the bed of the silicon particles (3) present in the heating zone (Zh) may be a
• a fluidizing gas (10) be supplied by a fluidizing gas
• heating zone (Zh) remain fluidized for effective exchange of the silicon particles between the two zones (Z r , Zh).
• silicon particles (3) within the reactor tube (2) becomes lowered with time to or
• silicon particles present in the heating zone (Zh) may remain as fixed or partly
• bed of silicon particles present in the heating zone (Zh) may remain as fixed or partly
• etching-step off-gas (13e) comprising the fluidizing gas being passed through the bed of silicon particles (3) be remained, and a non-reacted etching gas and/ or an
• etching reaction product gas be discharged out of the fluidized bed reactor using a
• the silicon particles should be purified to avoid contamination of the silicon particles.
• the silicon particles should be purified to avoid contamination of the silicon particles.
• fluidizing gas (10) is one not reacting with the silicon particles and is selected from
• the fluidizing gas (10) may further comprise
• reaction byproduct gas such as silicon tetrachloride (SiCl 4 ),
• SiHCb trichlorosilane
• SiH 2 Cl 2 dichlorosilane
• HCl hydrogen chloride
• the fluidizing gas (10) used in the present invention may comprise at least
• H 2 hydrogen
• N 2 nitrogen
• Ar argon
• He helium
• SiCU silicon tetrachloride
• SiHCb trichlorosilane
• SiH 2 Cb dichlorosilane
• the fluidizing gas (10) mentioned in the present description represents a gas
• the fluidizing gas (10) can be adjusted differently at each step of a silicon deposition
• a fixed bed i.e., a fixed bed
• the fluidizing gas (10) per unit time may not become excessive.
• the packing materials be at least 5-10 times higher than that of the silicon particles
• the fixed bed be not physically deformed by the movement or fluidization of the
• silicon particles (3) and the material be selected so that impurity contamination of the silicon particles (3) can be minimized. While the silicon deposition cycles are not
• particle preparation step should comprise a silicon-containing substance, so that
• gas (llr) may comprise at least one substance selected from monosilane (SiH 4 ),
• reaction gas (llr) may comprise only the afore-mentioned silicon deposition source
• material may further comprise at least one gas component selected from
• reaction gas (Hr) to supplying the source material for silicon deposition, the reaction gas (Hr)
• the silicon deposit (D) by forming gaseous silicon compounds through its reaction with the silicon deposit (D) during the silicon deposit removal step may comprise at
• At least one chlorine-containing substance selected from silicon tetrachloride (SiCl 4 ),
• the etching reaction (Re) triggered by the etching gas (lie) may comprise: (1)
• chlorosilane formation from a mixture of silicon metal/chlorine.
• present invention may comprise only the chlorine-containing substance. But, it is not limited to
• the molar concentration of the diluent gas do not exceed about 2-3 times that of hydrogen chloride.
• reaction temperature for monosilane is about 600-850 0 C
• the temperature of the silicon deposit removal step it is preferred that the temperature
• the heating means (8a, 8b) may be carried out not only directly by radiation heating,
• Fig. 7 illustrate respectively in a comprehensive way the schematics of the
• the fluidized bed reactor that can be used for the present invention
• the inner space of the reactor is
• the reactor shell (1) is isolated from the outside of the reactor by the reactor shell (1).
• the reactor tube (2) is installed vertically inside the reactor shell
• the reactor tube (2) is defined as an inner zone (4) in which the bed of silicon
• the reactor tube (2) and the reactor shell (1) is defined as an outer zone (5) in which
• the bed of silicon particles (3) is not present and silicon deposition does not occur.
• the reactor shell (1) may be made of a metallic material with reliable
• the reactor shell (1) may be composed of several components (Ia, Ib, Ic, Id) for convenience in fabrication,
• gaskets or sealing materials made of a variety of materials in order to completely
• (1) may be in the form of a cylindrical pipe, a flange, a tube with fittings, a plate, a
• each component may be coated with a protective
• a protective wall in the form of tube or shaped
• liner which may be made of a metallic material or a non-metallic material such as
• a cooling medium such as water, oil, gas and air for protecting the equipment
• cooled are preferably designed to comprise a coolant-circulating means at their inner
• an insulation material may be equipped on the outer
• the reactor tube (2) may be of any shape only if it can be hold by the reactor
• the reactor tube (2) may have the
• the reactor tube (2) may comprise a plurality of
• the reactor tube (2) is preferably made of an inorganic material, which is
• a carbon-containing material such as silicon carbide, graphite, glassy
• the reactor tube (2) is made of a carbon-containing organic compound
• the inner wall of the reactor tube (2) is preferred to be coated or lined with
• the reactor tube (2) is of one-
• the sealing means are preferred to be
• organic polymers graphites, silicas, ceramics, metals or composite materials thereof.
• the sealing means (41a, 41b) may be installed not too firmly so that the possibility of
• cracking of the reactor tube (2) can be lowered during assembly, operation and
• the inner zone (4) should be heated to a temperature required for silicon deposition
• One or a plurality of heating means (8a, 8b) may be installed in the inner zone (4)
• a heating means may be any suitable heating means.
• a heating means may be any suitable heating means.
• a plurality of heating means may be
• a plurality of heating means (8a, 8b) may be
• the reactor with an electric source (E) located outside the reactor may comprise
• metallic material in the form of a cable, a bar, a rod, a shaped body, a socket, a
• heating means can be prepared by extending a part of the heating means (8a, 8b).
• electrical insulation is also important besides the mechanical sealing for preventing
• the fluidized bed of the silicon particles (3) which are moved by gas flow, is formed
• silicon particles i.e., granular silicon product.
• silicon particles i.e., granular silicon product.
• fluidizing gas supplying means (14, 14') which supplies the fluidizing gas (10) to the
• silicon-containing reaction gas (llr) are installed as coupled with the reactor shell
• An etching gas supplying means (15e) may be installed at the fluidized bed
• means (15r) may be used to supply the etching gas (He) during the silicon deposit
• the reaction gas supplying means (15r) may have a simple structure, as
• etching gas He
• He etching gas
• reaction gas supplying means (15r) may have a plurality of gas paths or nozzles, so that the reaction gas (llr) and the
• etching gas He can pass through different paths or nozzles.
• supplying means (15r) may be composed of such components as a tube or nozzle, a
• part of the inner zone (4) are preferably composed of a tube, a liner or a shaped
• fluidizing gas (10) is preferably equipped along with the fluidizing gas supplying
• the gas distributing means (14, 14') and the reaction gas supplying means (15r).
• the gas distributing means (14, 14') and the reaction gas supplying means (15r).
• means (19) may be in the form of a multi-hole or porous distribution plate, a packing
• the fluidizing gas (10) may be any fluidizing gas supplied means (14, 14').
• the fluidizing gas (10) may be any fluidizing gas supplied means (14, 14').
• the fluidizing gas (10) may be any fluidizing gas supplied means (14, 14').
• the fluidizing gas (10) may be any fluidizing gas supplied means (14, 14').
• the fluidizing gas (10) may be any fluidizing gas supplied means (14, 14').
• the fluidizing gas (10) may be
• a fluidizing gas supplying means (14, 14') comprising a gas chamber
• the fluidizing gas (10) may be utilized as a part of the gas distributing means.
• a fluidizing gas (10) may be supplied by
• a fluidizing gas supplying means (14) coupled with the reactor shell (1) so that one
• a plurality of fluidizing gas nozzle outlet may be positioned in between the gas
• distributing means (19) may comprise at least two components selected from a
• the gas distributing means (19) may comprise the fixed bed of the packing
• the packing materials (22) have such a large size or sufficient unit mass as
• the packing is a sphere, an oval, a pellet, a nugget, a tube, a rod or a ring.
• the packing is preferably, the packing
• the material (22) is a high purity silicon material, having an average diameter in the
• bed is preferably formed at a height lower than the reaction gas outlet of the reaction
• the fixed bed is formed in the heating zone (Zh), movement of the silicon particles
• part of the reactor may be utilized for pre-heating the fluidizing gas (10).
• heating means (8a, 8b) can contact and be
• reaction gas (llr) supplied by the reaction gas supplying means (15r) while residing temporarily or over a substantial period of time or with a regular or
• silicon particle partial discharging step silicon deposit removal step and/ or silicon
• supplying means (14) enable supply of the fluidizing gas (10) to the inner zone (4),
• silicon seed crystals (3a) to the inner zone (4) in order to maintain the number and average particle diameter of the silicon particles (3) as constant as possible in the
• polycrystalline silicon particles needs to be installed as coupled with the reactor shell
• the discharge pipe of the particle discharging means (16) may be assembled
• reaction gas supplying means (15r) as in Fig. 6 or may be installed
• the silicon particles (3b) can be discharged from the inner zone (4) at the right time
• the silicon particles (3b) may be coupled with the reactor shell (1), so that the silicon particles (3b) can be
• the small sized ones can be readily utilized as seed crystals (3a).
• the silicon particles (3b) are preferably cooled while being
• nitrogen, argon, helium or other gas may be flown through the particle discharging
• a cooling medium such as water, oil, gas, etc., may be circulated along
• the particle discharging means (16) may be equipped as coupled with the
• particles (3b) are discharged out of the fluidized bed reactor after being sufficiently
• silicon product particles (3b) in the form of a tube, a liner or a shaped body made of
• wall of which can be cooled by a cooling medium may consists of a tube, a liner or a
• shaped body made of a metallic material coated or lined with a fluorine-containing
• the silicon product particles (3b) may be discharged
• product storage means to classify the silicon product particles (3b) depending on
• a variety of industrially available particle separation devices may be used.
• the silicon product particles (3b) is preferably made of a material used in the particle
• the particle discharging means (16) may be also utilized in the silicon particle partial discharging step as a
• the partial discharging step can also be performed
• silicon particles (3) may be equipped at the bottom of the reaction gas supplying
• Fine silicon powders or high-molecular-weight reaction byproducts Fine silicon powders or high-molecular-weight reaction byproducts
• gas treating means (34) selected among a cyclone, a filter, a packing tower, a
• seed crystals (3a) may be utilized for other purposes.
• the gas discharging means (17) enables discharging of the fluidizing gas (10),
• the inner zone (4) not only during the silicon particle preparation step, but also
• silicon particles (3b) discharged as product As described above, although the silicon
• a classifying means may be
• silicon seed crystals are prepared by pulverizing some of the
• the seed crystals (3a) may be supplied continuously, periodically or intermittently at the right time into the reactor inner zone (4) through
• a seed crystal supplying means (18) installed as coupled with the reactor shell (Id),
• the silicon particles may be pulverized into seed crystals inside the
• step may be contained in product particles (3b) or put aside and supplied to the
• silicon seed crystals (3a) may be supplied to the inner zone (4) through the seed
• the inner zone (4) comprises all spaces required for forming the bed of silicon particles (3)
• the inner zone (4) plays an important role in producing polycrystalline
• silicon particles by silicon deposition in the fluidized bed of silicon particles (3).
• the outer zone (5) is an independently formed space in between
• silicon particles (3) is not present and silicon deposition does not occur.
• outer zone (5) as mentioned in this description is the space of the inner space of the
• reactor shell (1) excluding the inner zone (4) or is formed in between the reactor tube
• An inert gas is supplied to the outer zone (5) to maintain the outer zone under
• the outer zone (5) provides a space for protecting the reactor tube (2), which is
• the outer zone (5) within a certain range. Second, the outer zone (5) provides a space
• the outer zone (5) provides a space for installing a heating means, if required, around the reactor tube (2) for heating the reactor. Fourth, the outer zone
• reactor tube (2) to prevent dangerous gas containing oxygen and impurities from
• the outer zone (5) allows a real ⁇
• (28, 28a, 28b) may reveal the presence or concentration of a gas component that may
• the outer zone (5) may provide a space
• zone may be partitioned into several sections in an up-and-down and/ or a radial or
• the divided sections are preferred to spatially communicate with each other while having substantially the same atmospheric
• An insulation material (6) which may be installed in the outer zone (5) for
• the heating means (8) which is connected to an electric energy supplying
• in the fluidized bed reactor may be installed either in the outer zone (5) or in the
• the heating means may be installed inside the bed of
• the heating means (8a, 8b) may be installed both
• heating means (8b) may be installed in the outer zone (5) only, as illustrated in Fig. 7.
• the whole or part of the heating means (8a, 8b) may be also utilized to heat the
• silicon deposit (D) directly or indirectly during the silicon deposit removal step.
• the silicon particles (3) can be directly heated in the inner zone (4).
• the heating means (8a) be positioned lower than the
• an inert gas (12) comprising at least one substance selected from nitrogen,
• this manipulation is performed in all steps of the
• inert gas (12) may be in the form of a tube, a nozzle, a flange,
• valve a valve, a fitting, etc., or a combination thereof.
• an outer zone connection means (28, 28a, 28b) may also be installed at the part of the reactor shell
• the outer zone (5) can be maintained under an inert gas atmosphere with a
• means (26a, 26b) may be used to perform the supply and discharge of the inert gas
• the inert gas connection means (26a, 26b) may be utilized for
• composition which may also be performed using the outer zone connection means
• outer zone connection means (28, 28a, 28b), which may be installed independently of
• the inert gas connection means (26a, 26b), is installed for measurement and/ or
• 28a, 28b may also be in the form of a tube, a nozzle, a flange, a valve, a fitting, etc.
• the outer zone connection means (28, 28a, 28b) may be utilized for the supply or
• connection means (28, 28a, 28b) in respect of shape and function.
• the inner zone (4) has a different
• the pressure (Pi) of the inner zone (4) is different depending on the location.
• pressure may be applied to the nature of the fluidization of solid particles.

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• 2006
  • 2006-06-15 KR KR1020060053826A patent/KR100813131B1/ko not_active Expired - Fee Related
• 2007
  • 2007-06-14 EP EP07746914.6A patent/EP2032746B1/en not_active Not-in-force
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