WO2012113672A2 - Dispositif et procédé pour façonner un matériau à base de sio2 - Google Patents

Dispositif et procédé pour façonner un matériau à base de sio2 Download PDF

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Publication number
WO2012113672A2
WO2012113672A2 PCT/EP2012/052448 EP2012052448W WO2012113672A2 WO 2012113672 A2 WO2012113672 A2 WO 2012113672A2 EP 2012052448 W EP2012052448 W EP 2012052448W WO 2012113672 A2 WO2012113672 A2 WO 2012113672A2
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WO
WIPO (PCT)
Prior art keywords
materials
silicon
roller
water mixture
containing material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2012/052448
Other languages
German (de)
English (en)
Other versions
WO2012113672A3 (fr
Inventor
Jürgen Erwin LANG
Hartwig Rauleder
Bodo Frings
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Evonik Operations GmbH
Original Assignee
Evonik Degussa GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Evonik Degussa GmbH filed Critical Evonik Degussa GmbH
Publication of WO2012113672A2 publication Critical patent/WO2012113672A2/fr
Publication of WO2012113672A3 publication Critical patent/WO2012113672A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C01B33/023—Preparation by reduction of silica or free silica-containing material
    • C01B33/025—Preparation by reduction of silica or free silica-containing material with carbon or a solid carbonaceous material, i.e. carbo-thermal process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/50—Mixing liquids with solids
    • B01F23/53—Mixing liquids with solids using driven stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
    • B01F27/051—Stirrers characterised by their elements, materials or mechanical properties
    • B01F27/053—Stirrers characterised by their elements, materials or mechanical properties characterised by their materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
    • B01F27/272—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces
    • B01F27/2722—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces provided with ribs, ridges or grooves on one surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
    • B01F27/272—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces
    • B01F27/2723—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces the surfaces having a conical shape

Definitions

  • the present invention relates to an apparatus for processing Si0 2 -containing materials and a process for the preparation of starting materials for the
  • Silicon for example, solar silicon, which is processed into solar cells, is usually made of silicon dioxide or silica. This is
  • Starting material is introduced into the manufacturing process of silicon, and must be prepared for this purpose.
  • One way of introducing is the precipitation of silica from an alkali silicate solution. In some processes, the
  • the liquefied Si0 2 -water mixture can be further processed into moldings, which are then dried and optionally sintered or otherwise thermally or mechanically compressed.
  • Si0 2 -water mixture usually further processed by it is reduced to produce a high-purity silicon melt from which the silicon solar then is crystallized.
  • Purity specifications for silicon on all metals of the Periodic Table of the Elements in particular on the chemical elements aluminum, boron, calcium, phosphorus, iron, nickel, titanium, zinc, tin, sodium and potassium.
  • Process steps include the addition of the halosilanes with complexing agents and precipitation and precipitation of the complexes.
  • Impurities can be oxidized by suitable reactants.
  • Device and a method are provided, which allow cost-effective, stable and efficient processing of SiO 2 -containing materials.
  • At least one device part which comes into contact with the SiO 2 -containing materials, at least partially coated with one or more materials and / or consists of one or more materials, the material or materials essentially of silicon and / or of oxygen, hydrogen, nitrogen, carbon, sulfur and / or other elements of the
  • Periodic Table of Elements is or are constructed in the context of Processing of Si0 2 -containing material are part of the Si0 2 -containing material to be added substances.
  • At least part of a surface with which the starting materials come into contact during their preparation or preparation is obtained from a material whose abrasion has no or only a slight negative influence on the purity of the silicon produced.
  • the harmlessness of the abrasion can result from the fact that the material, from which the abrasion consists, in the further course of the process like a
  • Starting material or an added substance is a starting material or an already added substance.
  • the harmlessness of the abrasion can also result from the fact that the material from which the abrasion consists is deposited with an already provided deposition process.
  • an already added substance may for example be an activator for reactions, a precipitating agent or a complexing agent.
  • Device parts according to the invention which are components of the device that come into contact with the starting materials, can be, for example, channels and
  • a basic body to be coated with one of the aforementioned surface materials can be made of metal, for example steel or
  • the coating can, for example, by flame spraying, sintering, grafting of
  • polymerizable starting material such as resins, laminating with foil or other known suitable coating methods.
  • the coating can also be done by gluing or plating with a ceramic film of one of the aforementioned ceramic materials. Flame spraying can be used for example when using polyetheretherketone as a coating.
  • Particularly advantageous embodiments of the invention can provide that the material or materials to at least 90%, preferably at least 99%, particularly preferably 99.9% of silicon, oxygen, hydrogen and / or from are constructed of the elements of the PSE, which are in the context of the processing of the shady material part of the Si0 2 -containing material to be added substances.
  • Substances that are part of the Si0 2 -containing material to be incorporated in the processing of Si0 2 -containing materials include carbon, which is added to reduce the S1O 2 to silicon, and / or chlorine, which is hydrochloric acid (HCl (aq)) for purifying the aqueous silica-water mixture (Si0 2 -Wasser mixture) is added.
  • the material or the materials consist of or consist of silicon, oxygen, hydrogen, carbon, nitrogen and / or chlorine. These are typically just the substances that are during a
  • Carbon is used in many silica manufacturing processes to reduce silica and is also added to the starting materials for reduction for this purpose.
  • pure carbon but alternatively or additionally also carbon compounds such as silicon carbide or organic compounds can be added.
  • Hydrogen combines with water released from the reduction to form water and can be easily removed from the process, for example, by removing water vapor from a reactor in which the reduction takes place. Nitrogen is also removable from the Si0 2 -containing material by reacting the nitrogen with released oxygen at high temperatures
  • Temperatures connects to nitrogen oxides, which can be withdrawn from the reactor. If the reduction is carried out in a wet-chemical low-temperature process, nitrogen compounds can be formed which are to be separated from the resulting silicon.
  • Silicon carbide (SiC) is available as a sintered block material and can be made as a green compact before sintering in the required form. The same applies to sintered silicon dioxide and sintered silicon nitride, which also
  • Quartz glass can be made into a suitable shape by known glass processing techniques. Polysiloxanes do not have high strength, but have good chemical and temperature resistance. Sufficient strength can be achieved, for example, by depositing components of polysiloxane which are in contact with the starting materials, for example with metal.
  • the material is a
  • Composite material is whose constituents are selected from the materials according to the invention, for example, a composite material of SiC and polysiloxane.
  • the material or the materials are selected from S1O 2 , silicon carbide, silicon nitride, polymers and / or graphite, preferably isostatically pressed graphite.
  • the material or the materials consists or consist at least predominantly of carbon and / or hydrocarbon, preferably of at least one organic compound, more preferably of polyaryletherketone (PAEK), polyetherketone (PEK), polyetheretherketone (PEEK), polyetherketone ketone ( PEKK), polyvinyl chloride (PVC) and / or polyimide (PI).
  • PAEK polyaryletherketone
  • PEK polyetherketone
  • PEEK polyetherketone
  • PEKK polyetherketone ketone
  • PVC polyvinyl chloride
  • PI polyimide
  • the plastics mentioned consist to a large extent of carbon and hydrogen, and partly of low nitrogen contents.
  • PVC contains chlorine in addition to carbon and hydrogen.
  • Polyetheretherketone has by its chemical resistance, especially by its acid resistance to silica, and chemical composition very well suited chemical properties, and also good mechanical properties, which
  • PI has a high mechanical strength and a very high Temperature resistance and good chemical resistance. It consists of carbon and hydrogen as well as a small amount of nitrogen. It is therefore well suited for the present task.
  • the plastics mentioned are available as block and rod material, whereby components for a device according to the invention can be easily produced by machining.
  • Graphite can be produced by hot isostatic pressing as a block material and can be machined. It is available as a high-purity material, for example, from SGL Carbon, and has mechanical and chemical properties that are particularly well suited to the task at hand, that is, good abrasion resistance and above all, no detrimental effect on final purity silicon.
  • the material or the materials is or are made up of a polymer or of polymers, preferably of PAEK, PEK, PEKK and / or PEEK.
  • the material or the materials have a Shore hardness in the range of 90 to 100, preferably in the range of 95 to 100, particularly preferably 99, have.
  • the Shore hardness is determined according to ISO 868. It can therefore be provided that the material or the materials has a Shore hardness of 99.
  • the polymers have a glass transition temperature of at least 140 ° C.
  • At least one device part which is in contact with the SiO 2 -containing materials is at least partially coated with one or more materials, wherein the coating has a thickness of at least 10 pm,
  • the Si02-containing material to be processed has a purity of at least 99%.
  • a further embodiment of the invention provides that at least one material is a high-purity material. This prevents unwanted substances from being present in the abrasion, which are difficult to remove from the process or which would require additional purification steps.
  • graphite and PEEK are available as high purity materials. Since the amount of abrasion is small compared to the amount of processed raw material, the
  • Surface materials are not necessarily designed as purified or high purity materials.
  • the pollution with pollutants can still be small enough to achieve a high quality, so purity of the silicon.
  • a high-purity material is considered a material whose metallic
  • the aluminum and boron contaminants are less than 20 ppm, less than or equal to 5 ppm calcium, less than or equal to 150 ppm iron, less than or equal to 25 ppm magnesium, manganese, and less chromium and less than 10 ppm phosphorus , with titanium less than 5 ppm, with zinc less than or equal to 3 ppm and the sum of impurities with sodium silicate less than 5 ppm.
  • the SiO 2 -containing material is a SiO 2 -water mixture, preferably with 30 to 70 percent by weight H 2 O, particularly preferably with 40 to 60 percent by weight H 2 O, very particularly preferably with about 53
  • Devices according to the invention may also be characterized in that the device comprises at least one extruder. According to a further particularly advantageous embodiment of the invention can be provided that the device comprises at least one liquefying device for liquefying Si0 2 water mixture, wherein with the
  • Condensing device preferably shear forces in the Si0 2 -Wasser mixture are transferable.
  • the liquefaction device comprises a mixer.
  • the mixer can be designed, for example, as a mixer with a rotating drum or as a ring-layer mixer.
  • the shearing forces prevailing in the mixer liquefy the silica-water mixture (Si0 2 -water mixture).
  • a mixture with other substances may, but does not have to take place.
  • the liquefying device comprises a nozzle through which a Si0 2 -water mixture can flow. This applies at least for liquefied Si0 2 -water mixture.
  • a rotationally symmetrical roller is rotatably mounted in a rotationally symmetrical recess in the interior of the nozzle, so that an annular gap is formed between the roller and the inner surface of the recess, preferably a conical recess in which a conical roller is rotatably mounted that results in a conically converging annular gap.
  • a roller is to be understood as an arbitrary rotationally-shaped body according to the invention, the term here is by no means restricted to cylindrical rollers.
  • roller is connected to a drive with which the roller is rotatable in the nozzle.
  • the nozzle Adhesion effect on the surface of the nozzle and the acceleration of the Volumetric shear forces exerted so that the silica-water mixture at least partially liquefied.
  • the nozzle is advantageously designed with a conical profile. By providing a nozzle with a smaller surface area compared to a mixer, the abrasion is minimized.
  • the rotational movement of the roller produces a relative speed of the surface of the roller to the inner surface of the nozzle.
  • the shear forces and the liquefaction effect are thereby increased.
  • the applied nubs again increase the shear forces in the layer of silicon dioxide-water mixture, so that a further improvement in the liquefaction effect occurs without the surface of the components having to be substantially increased for this purpose. Due to the design of the protruding elements as nubs less abrasion is generated in comparison to the mixing blades in a ring layer mixer or in a mixer with rotating mixing drum by their smaller surface-to-volume ratio and also by their low height.
  • At least a part of the surface with which the starting materials come into contact during the treatment consists predominantly of silicon or of one or more silicon compounds.
  • silicon-containing abrasion is harmless to the process, as far as it is concerned with the following
  • components of the device that come into contact with the starting materials in the preparation consist of solid material of one or more of the aforementioned materials or of a base material with a coating of one or more of the aforementioned materials. It can also be provided according to the invention that the surface of a
  • Silicon is selected so that minimal abrasion results from the size of the surface in contact with the starting materials and the flow rate and pressure resulting from the size of the surface in the channel for a given volume flow ,
  • a geometry in the area of the optimum can do this with the help of a
  • Flow simulation program and corresponding wear parameters that depend on the subsidized starting materials and the surface material of the device can be determined.
  • the object of the invention is also achieved by a process for the preparation of starting materials for the production of silicon, preferably with such a device, wherein SiO2-containing materials are processed, which are conveyed in the process, liquefied and / or compressed.
  • the surface which comes into contact with the shady material, at least partially comprises at least one material consisting essentially of silicon, oxygen, hydrogen and / or consists of the elements of the PSE, which are added to the SC-containing material during the processing of the shady material.
  • an SC-water mixture is liquefied, preferably in a nozzle, particularly preferably with a rotating roller comprising a multiplicity of nubs on its surface.
  • shear forces are introduced into the Si0 2 -containing material, wherein the Si0 2 -containing material is liquefied thereby and preferably a part of the device is rotated, in particular the roller. While not wishing to be bound by any particular theory, the inventors believe that the shear forces thereby disrupt weak bonds between silica particles in the SiO 2 -water mixture, mobilizing the particles and turning them into a gel-like liquid.
  • a smaller layer thickness of the silica-water mixture increases the flow speed and consequently the shear forces, and thus also improves the liquefaction effect.
  • the invention is based on the surprising finding that through the
  • Process step is removed anyway from the material or even the raw material itself. These introduced impurities then do not lead to a significant deterioration of the purity of the final product. There are also no additional process steps necessary to remove the introduced into the material foreign matter. Such process steps are in fact already included in the production in order to remove the impurities introduced anyway.
  • Preparation process already in the starting materials Precipitated silicic acid, especially high-purity silica, causes heavy abrasion on parts of the equipment with which it comes in contact with the raw material for the silicon production process during industrial processing.
  • the abrasion caused by abrasion in particular in the promotion, compression and liquefaction of silica-water mixture, contaminates the silica, which can degrade the purity of the silicon produced.
  • Reduced impurities in the produced silicon can be achieved by reducing the amount of abrasion and generating a type of abrasion that is as harmless as possible for the further process. This applies to all
  • Polyvinyl chloride can be used, for example, if the S1O 2 is reduced with carbon in a later process step and hydrochloric acid (HCl) is used in a second, later process step for the purification.
  • Water (H 2 0), or the elements hydrogen and oxygen are always critical especially when using a silica-water mixture (S1O 2 - water mixture), since it is always contained in the starting materials or intermediates and also the semiconductor properties of silicon is not adversely affected.
  • the invention is therefore also based on the particularly surprising finding that, to avoid contamination, it is not always the case that harder materials are used to reduce the amount of abrasion, as is the prevailing view, but materials with a high degree of abrasion can also be used contribute to an already existing pollution.
  • the following figures and embodiments serve only the following figures and embodiments.
  • Figure 1 a schematic representation of a portion of an inventive
  • FIG. 1 shows a schematic side view of a liquefaction device or condenser according to the invention.
  • the condenser comprises an inlet 1 for incoming gelled SiO 2 -water mixture 7, a rotationally symmetrical, tapered nozzle 2 and an outlet 3 for effluent liquefied S1O2- water mixture 8.
  • a roller 5 is provided, the one
  • Gap thickness decreases in the flow direction of the SiO2-water mixture. As a result, the shearing action of the gap on the flowing SiO 2 -water mixture is increased.
  • the circumference of the roller 5 is provided with nubs 6, which are shown schematically in Figure 1.
  • the nubs 6 may be distributed approximately evenly on the surface of the roller 5.
  • the roller 5 is supported by a shaft 4.
  • the inner surfaces on and in the condenser 1, 2 and 3 as well as the outer surfaces of the shank 4 and the roller 5 can be advantageously made of S1O2, silicon carbide,
  • the nubs 6 are coated on the surface with a material 9, which contains only (except for some impurities) chemical elements in the following process steps of the silicon-containing material or the
  • silicon or silicon dioxide can be a component of the material 9, and / or which are already present in the SiO 2 -water mixture but can be removed at a later time.
  • PEEK Polyetheretherketone
  • gelled SiO 2 -water mixture 7 is conveyed to the condenser with a conveyor, such as a screw conveyor (not shown).
  • a conveyor such as a screw conveyor (not shown).
  • Feed screw is advantageously at least on the surface of a second material such as the material 9 of the coating 9 of the studs 6.
  • the shaft 4 can rotate in use with the roller 5 about an axis AA, wherein the axis of rotation A- A of the roller 5 is selected in that it coincides with the axis of rotational symmetry of the roller 5.
  • a roller may also rotate eccentrically in a nozzle. The resulting wedge gap causes in the circumferential direction increased shear forces on the SiO 2 -water mixture, which is drawn by the rotation in a circumferentially tapered part of the gap.
  • the liquefaction effect of the condenser is further improved by the additional shearing forces introduced by the knobs 6 on the SiO 2 -water mixture 7.
  • the nubs 6 are arranged helically on the surface of the roller 5, they cause an additional conveying effect on the SiO 2 -water mixture 7, 8.
  • the nubs 6 are advantageously arranged taking into account the direction of rotation of the roller 5, that the conveying effect in the direction the outlet 3 of the condenser acts.
  • nubs 6 Longitudinal axis lies in the screw direction.
  • An advantageous embodiment of the nubs 6 is a round shape, since this is easy and inexpensive to manufacture.
  • the ratio of the diameter to the height of such nubs 6 is preferably in the range of 1: 3 to 3: 1, more preferably the ratio is about 1: 1.
  • the gelled Si0 2 -water mixture 7 can be supplied tangentially to the liquefier, for example through a tangential opening in the nozzle 2 (not shown).

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne un dispositif pour façonner des matériaux à base de SiO2. Au moins une partie dudit dispositif qui vient en contact avec les matériaux à base de SiO2 est recouverte au moins par endroits d'un ou de plusieurs matériaux et/ou se compose d'un ou de plusieurs matériaux, ledit ou lesdits matériaux étant ou se composant essentiellement de silicium et/ou d'oxygène, d'hydrogène et/ou des éléments de la classification périodique des éléments qui font partie des substances à ajouter au matériau à base de SiO2 dans le cadre du façonnage du matériau à base de SiO2. L'invention concerne en outre un procédé de façonnage de substances de base pour produire du silicium, de préférence au moyen d'un dispositif de ce type, procédé selon lequel des matériaux à base de SiO2 acheminés, fluidifiés et/ou compactés pendant le déroulement dudit procédé sont façonnés.
PCT/EP2012/052448 2011-02-25 2012-02-14 Dispositif et procédé pour façonner un matériau à base de sio2 Ceased WO2012113672A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102011004750A DE102011004750A1 (de) 2011-02-25 2011-02-25 Vorrichtung und Verfahren zum Verarbeiten eines SiO2-haltigen Materials
DE102011004750.6 2011-02-25

Publications (2)

Publication Number Publication Date
WO2012113672A2 true WO2012113672A2 (fr) 2012-08-30
WO2012113672A3 WO2012113672A3 (fr) 2013-04-18

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DE (1) DE102011004750A1 (fr)
TW (1) TW201247538A (fr)
WO (1) WO2012113672A2 (fr)

Cited By (1)

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CN107583594A (zh) * 2017-09-29 2018-01-16 宜昌南玻硅材料有限公司 一种带环隙空气强制冷却嘴套的精密反应器及纳米级气相法白炭黑的制备方法

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CN105195036A (zh) * 2015-09-18 2015-12-30 宁波天工机械密封有限公司 混合搅拌机

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Publication number Priority date Publication date Assignee Title
WO2007106860A2 (fr) 2006-03-15 2007-09-20 Reaction Sciences, Inc. Procédé de fabrication de silicium pour cellules solaires et pour d'autres applications
DE102008004396A1 (de) 2008-01-14 2009-07-16 Evonik Degussa Gmbh Anlage und Verfahren zur Verminderung des Gehaltes von Elementen, wie Bor, in Halogensilanen
DE102008004397A1 (de) 2008-01-14 2009-07-16 Evonik Degussa Gmbh Verfahren zur Verminderung des Gehaltes von Elementen, wie Bor, in Halogensilanen sowie Anlage zur Durchführung des Verfahrens
WO2010037705A1 (fr) 2008-09-30 2010-04-08 Evonik Degussa Gmbh Procédé de préparation de sio2 de grande pureté à partir de solutions silicate

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107583594A (zh) * 2017-09-29 2018-01-16 宜昌南玻硅材料有限公司 一种带环隙空气强制冷却嘴套的精密反应器及纳米级气相法白炭黑的制备方法

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DE102011004750A1 (de) 2012-08-30
WO2012113672A3 (fr) 2013-04-18
TW201247538A (en) 2012-12-01

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