EP2736845A1 - Utilisation de sous-produits de type tétrachlorure de silicium pour produire du silicium au moyen d'une réaction faisant intervenir des agents réducteurs métalliques - Google Patents

Utilisation de sous-produits de type tétrachlorure de silicium pour produire du silicium au moyen d'une réaction faisant intervenir des agents réducteurs métalliques

Info

Publication number
EP2736845A1
EP2736845A1 EP12722738.7A EP12722738A EP2736845A1 EP 2736845 A1 EP2736845 A1 EP 2736845A1 EP 12722738 A EP12722738 A EP 12722738A EP 2736845 A1 EP2736845 A1 EP 2736845A1
Authority
EP
European Patent Office
Prior art keywords
silicon
ppm
production
ppt
use according
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.)
Withdrawn
Application number
EP12722738.7A
Other languages
German (de)
English (en)
Inventor
Ekkehard MÜH
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 EP2736845A1 publication Critical patent/EP2736845A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • C01B33/021Preparation
    • C01B33/027Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/033Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by reduction of silicon halides or halosilanes with a metal or a metallic alloy as the only reducing agents

Definitions

  • the invention relates to the use of the by-product silicon tetrachloride, in particular obtained as a byproduct in the production of silicon or halosilanes, for the production of silicon, by reacting the by-product silicon tetrachloride with an elemental, metallic reducing agent to silicon and metal chlorides.
  • silicon tetrachloride is obtained as a by-product both in the production of silicon in the context of the Siemens process and in the production of halosilanes, such as trichlorosilane.
  • Trichlorosilane is obtained by reacting crude silicon with hydrogen chloride in the fluidized bed.
  • silicon tetrachloride is usually formed to be 10 to 15%.
  • silicon in particular high-purity silicon from chlorosilanes in the presence of hydrogen.
  • silicon tetrachloride silicon tetrachloride
  • silicon tetrachloride is formed. It is known to convert the silicon tetrachloride by reaction with hydrogen back into Tnchlorsilan and feed the Siemens process again. Also in the recycling silicon tetrachloride is again formed from Tnchlorsilan in the synthesis of silicon.
  • the conversion of monosilane SiH into silicon also proceeds via the production of tochlorosilane, in which silicon tetrachloride is formed as a by-product.
  • fumed silica silicon dioxide
  • silicon tetrachloride silicon dioxide
  • Silicon tetrachloride in Tnchlorsilan is energetically and economically expensive.
  • a particular disadvantage is that not only silicon but also silicon tetrachloride is formed from the Tnchlorsilan, so that this cycle the
  • the object of the present invention was to provide a further economical use of silicon tetrachloride by-products, which are the abovementioned
  • Disadvantages does not have and preferably directly apply, without that cycle again and again, such as the above, must be traversed. Another task was to avoid the use of environmentally harmful compounds, or compounds that are expensive to dispose of. Preferably, a use should be provided which essentially allows the
  • the object of the invention was also the reduction or avoidance of waste and unusable by-products per kilogram of hyperpure silicon in the implementation of the Siemens process.
  • the problem is solved by the use according to the invention
  • the invention relates to the use of silicon tetrachloride, as
  • By-product is obtained in the production of silicon, monosilane or halosilanes, or generally by silicon tetrachloride by-products for the production of silicon, by the silicon tetrachloride is reacted with an elemental, metallic reducing agent, in particular sodium or zinc, to silicon and metal chlorides.
  • an elemental, metallic reducing agent in particular sodium or zinc
  • sodium chloride and / or zinc chloride are obtained as metal chlorides.
  • SiCl 4 + 2 Zn -> Si + 2 ZnCl 2 object of the invention is thus the use of silicon tetrachloride, which is obtained in particular as a by-product in the Siemens process, for the production of silicon by this silicon tetrachloride with an elementary, metallic reducing agent to silicon and the corresponding metal chloride is reacted.
  • Another object of the invention is also the use of
  • Silicon tetrachloride which is obtained in particular as a byproduct in the production of halosilanes or monosilane, for the production of silicon by this silicon tetrachloride is reacted with an elemental, metallic reducing agent to silicon and the corresponding metal chloride.
  • halosilane are SiHal x H -x , with shark equal to chlorine and x is 1, 2, 3 or 4, but also
  • Polyhalosilanes such as a Halogendisilan, Halogentrisilan and higher halosilanes, but especially hexachlorodisilane.
  • the silicon tetrachloride used is an i) by-product of the Siemens process in which silicon is formed from suitable toluene silane by reduction with hydrogen; and / or ii) a by-product of the preparation of silicon-based thiol with hydrogen chloride; and / or a) is a by-product of dismutation reactions in the preparation of monosilane, monochlorosilane, dichlorosilane, tochlorosilane and / or polyhalosilanes.
  • a polyhalosilane is also a Halogendisilan, Halogentrisilan and higher
  • Halogensilanes but especially hexachlorodisilane. If a high-purity silicon tetrachloride is used according to the invention, for example, from one or more of the abovementioned processes, it is preferable to use an equally pure elemental, metallic reducing agent.
  • Reducing agent does not need to be cleaned again, but directly with the
  • Reductant, in particular with sodium or zinc, to silicon and metal chloride can be implemented.
  • the silicon thus obtained may, if necessary or desired, be purified by directional solidification or as described below.
  • the metal chlorides are sodium chloride when sodium is used, and zinc chloride when zinc is used.
  • Silicon tetrachloride which is obtained as a by-product in the production of silicon, monosilane or halosilanes without further purification, in particular without
  • Elementary, metallic reducing agents according to the invention comprise an alkali metal, an element of the 2nd subgroup of the Periodic Table or a mixture containing at least one of the elements, in particular sodium being used as the reducing agent or zinc used. These are lithium, potassium, sodium, zinc, cadmium or
  • Particularly preferred reducing agents are sodium and zinc.
  • the use according to the invention is characterized in that the before a reduction of silicon tetrachloride, if necessary, if necessary, metallic impurities, in particular impurities with metallic solids in the silicon tetrachloride by means of filtration, liquid impurities by means of a
  • Adsorbent dissolved impurities by means of an adsorbent or impurities by means of a combination of the aforementioned measures before the reaction with the reducing agent are separated. Not reduced
  • Silicon tetrachloride may also be contacted by means of said measures prior to re-contacting with the elemental metallic reducing agent
  • a filter preferably has a pore size of less than 100 ⁇ on, preferably less than 50 ⁇ to 5 ⁇ on, more preferably, the filter has a mean pore size between 5 to 30 ⁇ , more preferably from 5 to 10 ⁇ , optionally can be filtered at least once in a further step, the thus treated silicon tetrachloride, wherein the at least one filter has a pore size of less than 5 ⁇ , in particular a pore size less than or equal to 1 ⁇ , more preferably a pore size less than or equal 0.1 ⁇ , or less than or equal 0,05 ⁇ , the content of the filtrate of impurities, such as foreign metals and / or the foreign metal-containing compound is then reduced.
  • the pore size of the filter can also result from the interparticle packing of an adsorbent.
  • the adsorbent used is preferably an organic, amino-functionalized, polymeric adsorbent to which the silicon tetrachloride is contacted to reduce the level of impurities, which generally include foreign or foreign metal-containing compounds.
  • the adsorbent used is essentially anhydrous and free of organic solvents.
  • an adsorbent comprises a divinylbenzene crosslinked one Polystyrene resin having tertiary amino groups and / or quaternary amino groups, wherein the amino groups are substituted by ethyl or methyl groups.
  • Amberlyst A 21 and Amberlyst A 26 OH are both ion exchange resin based on divinylbenzene cross-linked polystyrene resin with trimethylamino- or dimethylamino-functionalized polymeric backbone of the resin.
  • the silicon tetrachloride is sodium or zinc
  • reaction of silicon tetrachloride with zinc is preferably carried out in one
  • silicon tetrachloride and the reducing agent, in this case zinc are used in a stoichiometric ratio to each other or preferably silicon tetrachloride is light
  • the temperature in the reaction zone may be between 880 to 2000 ° C.
  • Unreacted silicon tetrachloride may be re-reacted with the reducing agent and optionally purified from dissolved or solid impurities as described above.
  • the silicon obtained by reduction of metals and / or metal salts, the boiling point of which is below the melting point of silicon can be purified by melting, in particular complete melting, preferably one or more directional solidification processes are subsequently carried out.
  • the silicon is purified of sodium chloride, sodium, zinc and / or zinc chloride and other foreign metals by directional solidification.
  • the person skilled in the art is familiar with the various solidification processes, which include zone melting with a constant melt volume, or also the Vertical Bridgman method, Vertical Gradient Freeze method (VGF), Czochralski method or the neck Kyropoulos method.
  • the silicon produced by directional solidification vorzugseise has a resistivity of between 10 -2 and 10 4 Ohm x cm.
  • the silicon produced has to meet particularly stringent purity requirements. Impurities in the starting compounds in the stated field of application are already disturbing in the mg / kg (ppm range), g / kg) ppb to ppt range. Due to their electronic properties, elements of the III and V group of the periodic table interfere particularly, so that for these elements, the limits of contamination in the silicon are particularly low. For example, on the pentavalent phosphorus and arsenic, the doping of the produced silicon caused by them is n-type semiconductor
  • Si sg solar grade silicon having a purity of 99.999% (5.9's) or 99.9999% (6.9's).
  • semiconductors silicon electronic grade silicon, Si eg
  • Si eg semiconductor grade silicon
  • the invention also relates to the use of the by-product
  • Silicon tetrachloride for producing high-purity silicon comprising reduction with elemental, metallic reducing agents, preferably with subsequent melting, for example directional solidification processes and / or phase separation, the pure silicon being a silicon having the following impurity profile: Aluminum less than or equal to 5 ppm, or between 5 ppm and 0.0001 ppt, in particular between 3 ppm to 0.0001 ppt, preferably between 0.8 ppm to 0.0001, ppt, more preferably between 0.6 ppm to 0.0001 ppt more preferably between 0.1 ppm to 0.0001 ppt, most preferably between 0.01 ppm and 0.0001 ppt, more preferably 1 ppb to 0.0001 ppt,
  • Iron less than or equal to 20 ppm, preferably between 10 ppm and 0.0001 ppt,
  • Nickel less than or equal to 10 ppm, preferably between 5 ppm and 0.0001 ppt,
  • Phosphorus less than 10 ppm to 0.0001 ppt, preferably between 5 ppm to 0.0001 ppt, in particular less than 3 ppm to 0.0001 ppt, preferably between 10 ppb to 0.0001 ppt and most preferably between 1 ppb to 0.0001 ppt
  • Titanium less than or equal to 2 ppm, preferably less than or equal to 1 ppm to 0.0001 ppt,
  • Zinc less than or equal to 3 ppm, preferably less than or equal to 1 ppm to 0.0001 ppt,
  • metallic reducing agent As a pure elemental, metallic reducing agent are reducing agent having a content of 99% reducing agent and a maximum of 1% contamination with other metallic compounds and / or other metals.
  • Metallic impurities are iron, manganese, nickel, copper, aluminum, boron, calcium, phosphorus, titanium, zinc. More preferably, the reducing agent has a content of 99.9% reducing agent, particularly preferably 99.99% reducing agent.
  • Solar grade silicon or semiconductor grade silicon preferably has a content of 99.99% of the reducing agent, more preferably of 99.9999%.
  • the elemental, metallic reducing agent has at most a total impurity content of foreign metals of ⁇ 1 ppm.
  • a particular advantage of the use according to the invention of silicon tetrachloride, which is obtained as a by-product, in particular in the abovementioned processes, is that the silicon produced in this way directly comprises a technical silicon with a content of at least 96% by weight.
  • Silicon is, in particular, it is pure silicon with a content of 99 wt .-% silicon, preferably high-purity silicon having a content of 99.99 wt .-% silicon, more preferably it is solar grade silicon with a
  • the foreign metal content and / or the content of the foreign metal-containing compound in the silicon tetrachloride is preferably in relation to the metallic compound, in particular independently, in each case to a content in the range of less than 100 ⁇ g kg to the detection limit, in particular of less than 25 ⁇ g kg, preferably below 15 ⁇ g kg, particularly preferably 0.1 to 10 ⁇ g kg are reduced to the respective detection limit.
  • the contents of boron, aluminum, potassium, lithium, sodium, magnesium, calcium, zinc and / or iron are preferably below the stated values.
  • the content of boron and iron in the silicon tetrachloride is particularly preferably below the stated contents.
  • the compounds are present dissolved in silicon tetrachloride and can be well separated by means of an adsorbent, such as BCI 3 .
  • the foreign metals or foreign metal-containing compounds are generally metal halides, metal hydrogen halides and / or metal hydrides and mixtures of these compounds. But even with organic radicals such as alkyl or aryl groups, functionalized metal halides, metal hydrogen halides or metal hydrides can be removed with very good results from silicon tetrachloride. Examples thereof may be aluminum trichloride or else iron (III) chloride as well as entrained particulate metals, which may originate from continuous processes. In the context of the use according to the invention, it is particularly preferred if the i) the silicon obtained by reduction of metals, in particular
  • the silicon produced by directional solidification preferably has a resistivity between 10 "2 and 10 4 ohm.cm.Optically or additionally, ii) the silicon obtained from reduction of metals, in particular foreign metals, and / or metal salts, in particular foreign metal salts, their boiling point above the
  • Phase separation can be used to remove contaminants, foreign metals and foreign metals Compounds are reliably separated from the silicon.
  • one or more systems for directional solidification subsequently join.
  • the silicon produced by directional solidification preferably has a specific one
  • the silicon produced according to the invention has a resistivity between 10 "6 and 10 10 ohm.cm, in particular, the silicon produced by reduction with the elemental metallic reducing agent has a resistivity between 10 " 5 and 2 x 10 "2 ohms x It is preferred if it did not have to be further purified for this resistance value after the reduction, in particular if it originated from one of the abovementioned processes and no significant impurities were introduced by the reducing agent.
  • the content of silicon or, better, the purity of the silicon with respect to metallic impurities is 99.99 to 99.9999% d. 4n to 6n, preferably from 99.999 to 99.9999999%, d. H. 5n to 9n as high purity silicon.
  • the content of silicon, or better, the purity of silicon with respect to metallic impurities can be determined by the resistivity of a prepared Si layer or Si-rod. The measurement of the resistivity of silicon can serve to determine the purity of the silicon as well as to indirectly determine the purity of the silicon tetrachloride used.
  • the content of impurities by elements of the 3rd main group of the elements of the Periodic Table is critical for z.
  • the method of determining the resistivity is suitable for detecting and increasing extremely low concentrations of impurities by elements of the 3rd and 5th main groups of the Periodic Table of the Elements quantify, because it is these impurities that influence the resistivity of a silicon layer.
  • the specific resistance (in short: for specific electrical resistance or resistivity) is a temperature-dependent material constant with the symbol p.
  • the measurement of the resistance and the layer thickness can take place via the so-called SRP method (spreading resistance probe).
  • SRP method spreading resistance probe
  • Beveling angle and the path length can also calculate the layer thickness.
  • the determination of the layer thickness is unnecessary for continuous homogeneous substrates.
  • the method is described in detail in several standards and specifies the procedure described above. The methods used here follow the SEMI standards MF672 and MF674, which are referred to in the MF672.
  • the SEMI standard MF672 is an extension of the SEMI standard MF525.
  • the SEMI standards are also published as ASTM standards (eg ASTM F 672-80).
  • the method for determining the resistivity of silicon can also be found in DE 2010002342.6, the content of which is fully incorporated by reference.
  • the method of determining the resistivity provides that the impurities are not directly determined by silicon applied
  • the specific resistance (short for specific electrical resistance or resistivity) is a temperature-dependent material constant with the symbol p.
  • the silicon obtained according to the invention if it is not already present as a shaped or specimen, a specimen having defined dimensions, for example by melting, shaping and subsequent solidification.
  • the resistance and the layer thickness are measured by the so-called SRP method (spreading resistance probe).
  • SRP method spreading resistance probe
  • a piece of the specimen is ground at a defined angle.
  • the resistance measurement is then carried out by means of two probe tips, which scan the entire profile at certain intervals and each result in a resistance value to a specific layer thickness.
  • About the bevel angle and the path length can also calculate the layer thickness. The method is described in detail in the standards already mentioned above and specifies the procedure described above.
  • the use of the silicon tetrachloride by-products in a large-scale process d. h. the silicon tetrachloride is reacted with an elemental, metallic reducing agent to silicon and metal chlorides in a large-scale process.
  • Silicon carbide in silicon As a large-scale process is a conversion of Silium tetrachloride ⁇ 50 kg / hour with a metallic reducing agent,
  • the invention also relates to the use of the resulting metal chlorides, which can be supplied for commercial use and so to
  • the i) sodium chloride obtained by the use according to the invention can be used: as table salt (according to the definition of the regulations for food, for example table salt may contain only 1% colloidal silica, max 20 ppm
  • Hexacyanoferrate pickling salt
  • iron oxide in animal husbandry
  • road salt as road salt
  • Industrial salt in particular with colored marking as road salt, for the preparation of cold mixes, for salting out soaps, for use as pit salt; for water treatment, for the preservation of hides, for the preparation of inhalation solutions, for
  • Caustic soda, and / or ii) the zinc chloride can be used: for the preparation of salt baths in the production of polyacrylic fibers, as an electrolyte in
  • Lewis elements High power cells (Leclanche elements); soldering fluid; Lewis acid, in particular as Lewis acid for dehydration and / or condensation in organic
  • diazonium in the production of dyes; for the manufacture of paper mache and vulcanized fiber, for the production of medical wash waters, caustics or pastes, in particular for the treatment of infected wounds and ulcers; as a disinfectant; for the preparation of emulsions for use in photography, for the production of copy paper; as a staining reagent in the
  • both the sodium chloride and the zinc chloride can be converted by means of electrolysis in sodium or zinc and chlorine and the inventive
  • Treatment has a purity of 99.1% and is therefore suitable for technical applications.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

L'invention concerne l'utilisation du sous-produit tétrachlorure de silicium, généré comme sous-produit lors de la production de silicium ou d'halogénosilanes, pour produire du silicium selon un procédé consistant à faire réagir ledit sous-produit tétrachlorure de silicium avec un agent réducteur métallique élémentaire pour obtenir du silicium et des chlorures métalliques.
EP12722738.7A 2011-07-25 2012-05-23 Utilisation de sous-produits de type tétrachlorure de silicium pour produire du silicium au moyen d'une réaction faisant intervenir des agents réducteurs métalliques Withdrawn EP2736845A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102011079755 2011-07-25
DE201110109543 DE102011109543A1 (de) 2011-07-25 2011-08-03 Verwendung von Siliciumtetrachlorid-Nebenprodukten zur Herstellung von Silizium durch Umsetzung mit metallischen Reduktionsmitteln
PCT/EP2012/059549 WO2013013857A1 (fr) 2011-07-25 2012-05-23 Utilisation de sous-produits de type tétrachlorure de silicium pour produire du silicium au moyen d'une réaction faisant intervenir des agents réducteurs métalliques

Publications (1)

Publication Number Publication Date
EP2736845A1 true EP2736845A1 (fr) 2014-06-04

Family

ID=47503145

Family Applications (1)

Application Number Title Priority Date Filing Date
EP12722738.7A Withdrawn EP2736845A1 (fr) 2011-07-25 2012-05-23 Utilisation de sous-produits de type tétrachlorure de silicium pour produire du silicium au moyen d'une réaction faisant intervenir des agents réducteurs métalliques

Country Status (4)

Country Link
EP (1) EP2736845A1 (fr)
DE (1) DE102011109543A1 (fr)
TW (1) TW201317180A (fr)
WO (1) WO2013013857A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115215340A (zh) * 2021-04-19 2022-10-21 四川物科金硅新材料科技有限责任公司 一种纳米硅线及其制备方法

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10217126A1 (de) * 2002-04-17 2003-10-30 Wacker Chemie Gmbh Verfahren zur Herstellung von amorphem Silicium über Siliciumtetrachlorid
JP2007284259A (ja) * 2006-04-12 2007-11-01 Shin Etsu Chem Co Ltd シリコンの製造方法及び製造装置
EP2021279A2 (fr) * 2006-04-13 2009-02-11 Cabot Corporation Production de silicium selon un procédé en boucle fermée
JP2009208994A (ja) * 2008-03-04 2009-09-17 Sumitomo Chemical Co Ltd シリコン製造方法及びシリコン製造装置
JPWO2010029894A1 (ja) * 2008-09-09 2012-05-17 Jnc株式会社 高純度結晶シリコン、高純度四塩化珪素およびそれらの製造方法
DE102010002342A1 (de) 2010-02-25 2011-08-25 Evonik Degussa GmbH, 45128 Verwendung der spezifischen Widerstandsmessung zur indirekten Bestimmung der Reinheit von Silanen und Germanen und ein entsprechendes Verfahren
CN102161488A (zh) * 2011-02-28 2011-08-24 中南大学 一种制备太阳能级多晶硅的方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2013013857A1 *

Also Published As

Publication number Publication date
TW201317180A (zh) 2013-05-01
WO2013013857A1 (fr) 2013-01-31
DE102011109543A1 (de) 2013-01-31

Similar Documents

Publication Publication Date Title
EP2229342B1 (fr) Procédé pour réduire la teneur en éléments, tels que du bore, d'halosilanes et installation pour la mise en oeuvre dudit procédé
EP2426085B1 (fr) Procédé de fabrication de silicium polycristallin
EP2274238B1 (fr) Procédé d'hydrolyse de sels métalliques solides à l'aide de solutions salines acqueuses
EP2078695A2 (fr) Procédé et appareil pour séparer un produit gazeux d'un flux d'alimentation comprenant des contaminants
EP2294006A1 (fr) Procédé pour éliminer des impuretés contenant du bore d halogénosilanes et installation pour mettre en uvre le procédé
EP2637968B1 (fr) Procédé de fission sélective de silanes supérieurs
DE102008004396A1 (de) Anlage und Verfahren zur Verminderung des Gehaltes von Elementen, wie Bor, in Halogensilanen
EP4065512B1 (fr) Procédé permettant d'éliminer une impureté d'un mélange de chlorosilane
DE112008002370T5 (de) Verfahren zur Herstellung von Silicium
DE1906197A1 (de) Verfahren zur Entfernung von borhaltigen Verunreinigungen aus Chlorsilanverbindungen
WO2012062562A2 (fr) Procédé de fission de silanes supérieurs
DE112014005811B4 (de) Neutraler Komplex eines cyclischen Silans, Herstellungsverfahren dafür und Verfahren zur Herstellung eines cyclischen hydrierten Silans oder eines cyclischen organischen Silans
EP0094139B1 (fr) Procédé de préparation de dioxyde de silicium pur
WO2013013857A1 (fr) Utilisation de sous-produits de type tétrachlorure de silicium pour produire du silicium au moyen d'une réaction faisant intervenir des agents réducteurs métalliques
US3506394A (en) Method for producing sodium silicofluoride from wet process phosphoric acid
DE112006001649T5 (de) Verfahren zur Herstellung von Silicium hoher Reinheit
DE1291324B (de) Verfahren zur Reinigung von Halogensilanen
EP3013745B1 (fr) Procédé de production de trichlorosilane
JP4036426B2 (ja) ろ過性の優れた石膏の製造方法
EP3233729A2 (fr) Procédé de production d'un anion perhalogéné d'hexasilane et procédé de production d'une liaison silane cyclique
EP3966164B1 (fr) Procédé de production d'hexachlordisilane par réaction d'au moins un chlorordisilane partiellement hydrogéné sur un adsorbeur solide non fonctionnalisé
WO2020114609A1 (fr) Procédé pour diminuer la teneur en composés de bore dans une composition contenant de l'halogénosilane
DE102012015417B4 (de) Verfahren zur Aufarbeitung von Sägerückständen aus der Produktion von Siliciumwafern
KR20160069574A (ko) 염화실란 또는 메틸염화실란으로부터 불순물인 금속염화물을 제거하는 방법
Bounou et al. Pretreatment of industrial phosphoric acid by dolomitic sediment: Optimization using design of experiments

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20140121

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

DAX Request for extension of the european patent (deleted)
STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 20140916