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EP2337765A1 - Method for removing titanium from hexachlorodisilane - Google Patents

Method for removing titanium from hexachlorodisilane

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Publication number
EP2337765A1
EP2337765A1 EP09783845A EP09783845A EP2337765A1 EP 2337765 A1 EP2337765 A1 EP 2337765A1 EP 09783845 A EP09783845 A EP 09783845A EP 09783845 A EP09783845 A EP 09783845A EP 2337765 A1 EP2337765 A1 EP 2337765A1
Authority
EP
European Patent Office
Prior art keywords
hexachlorodisilane
compounds
titanium
distillation
structural units
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Withdrawn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
EP09783845A
Other languages
German (de)
French (fr)
Inventor
Wolfgang Knies
Hans Eiblmeier
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.)
Wacker Chemie AG
Original Assignee
Wacker Chemie AG
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Filing date
Publication date
Application filed by Wacker Chemie AG filed Critical Wacker Chemie AG
Publication of EP2337765A1 publication Critical patent/EP2337765A1/en
Withdrawn legal-status Critical Current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
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • 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
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/10778—Purification
    • C01B33/10794—Purification by forming addition compounds or complexes, the reactant being possibly contained in an adsorbent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D37/00—Processes of filtration

Definitions

  • the invention relates to a process for removing titanium from hexachlorodisilane by treatment with organic compounds.
  • Hexachlorodisilane which is made from silicides, always contains traces of titanium and other metallic impurities. Titanium is critical in that the titanium (IV) chloride is only slightly different in boiling point from hexachlorodisilane. To separate it, a complex fractional distillation is necessary.
  • Chlorosilanes distillation can be relatively easily removed from titanium. During the silicon deposition% arise from the chlorosilanes turn disilanes, but present in concent ⁇ rations at first. When storing these silanes in stainless steel containers Titan Pro ⁇ domestic product may occur due to corrosion in turn, which in turn could previously only separated by fractional distillation.
  • the process according to the invention has the further advantage that hexachlorodisilane is obtained in high purity. Purity of at most 100, in particular at most 50 ppb of Ti (by weight) are achievable.
  • the bound titanium compounds can be separated from the hexachlorodisilane in different ways.
  • the bound titanium compounds are separated from the hexachlorodisilane by distillation, decantation or filtration.
  • the distillation is greatly simplified compared to the untreated hexachlorodisilane, because the complicated boiling fraction of the bound titanium compounds eliminates the complicated fractional distillation.
  • the bound titanium compounds remain in the bottom of the distillation.
  • a solvent When removing titanium compounds from hexachlorodisilane, a solvent can also be used.
  • Preferred compounds (V) are cyclic ether compounds which preferably have at least 5 ring atoms and preferably at most 30 ring atoms, such as 1, 3-dioxolane, tetrahydrofuran, tetrahydropyran, tetrahydropyran, 1,4-dioxane, [12] crown-4,
  • the cyclic ether compounds may have hydrocarbon substituents, in particular alkyl radicals having 1 to 6 carbon atoms, preferably methyl and ethyl.
  • Examples of substituted cyclic ether compounds are 4-methyl 1, 3-dioxolane, 3-methyl-tetrahydrofuran, 2, 2-dimethyl-1, 4-dioxane.
  • monoethers ethers are preferred with a boiling point of at least 6O 0 C at 1 bar, for example, di-n-propyl ether.
  • Polyethers which can also be used are polyalkylene glycols, such as polyethylene glycol and polypropylene glycol.
  • the average molecular weights Mn of the polyalkylene glycols are preferably at least 150, in particular at least 500 and preferably at most 10000, in particular at most 5000.
  • Preferred compounds (V) are also cyclic and linear thioether compounds, such as dialkyl sulfides.
  • thiols ( ⁇ C-SH) compounds having a molecular weight of at least 1000 are preferred.
  • vinyl polymers with SH groups such as ion exchanger, for example Amberlite ® G 73rd
  • At least 100 parts by weight of hexachlorodisilane are preferably used for at least 0.001 parts, more preferably at least 0.05 parts by weight of compound (V), and preferably not more than 10, particularly preferably not more than 5 parts by weight of compound (V).
  • Mixtures containing hexachlorodisilane can also be treated with organic compound (V).
  • the hexachlorodisilane used contains at most 100 ppm, particularly preferably 10 ppm, in particular 1 ppm of titanium, each by weight.
  • These chlorosilane mixtures used may have been treated with chlorine before or during the purification in order to convert hydrogenchlorosilanes to chlorosilanes, since in particular hydrogenchlorosilanes with a higher hydrogen content may be self-igniting.
  • chlorosilane mixtures used can also be combined with other substances, such as e.g. Activated charcoal or, if at all, preferably pyrolytic or silica produced by the precipitation process.
  • substances such as e.g. Activated charcoal or, if at all, preferably pyrolytic or silica produced by the precipitation process.
  • the treatment with organic compound (V) is preferably carried out at at least -5 0 C, preferably at least 15 ° C.
  • the distillation can be carried out either under normal pressure, overpressure or reduced pressure.
  • the distillation according to the invention can be carried out in the presence or absence of inert gas, such as nitrogen, helium or argon, but it can also be carried out in air as long as the moisture content is at most 10 ppbw. For reasons of cost, the distillation is preferably carried out in the presence of nitrogen.
  • inert gas such as nitrogen, helium or argon
  • Example 3 ca 100g hexachlorodisilane added with 4 g of Amberlite ® GT 73 stirred at room temperature for 6 hours. A sample was filtered off and examined.

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

Abstract

The invention relates to a method for removing titanium compounds from hexachlorodisilane, wherein hexachlorodisilane is treated with an organic compound (V) which contains the structural units =C-S- or =C-O-.

Description

Verfahren zur Entfernung von Titan aus Hexachlordisilan Process for removing titanium from hexachlorodisilane
Die Erfindung betrifft ein Verfahren zur Entfernung von Titan aus Hexachlordisilan durch Behandlung mit organischen Verbin- düngen .The invention relates to a process for removing titanium from hexachlorodisilane by treatment with organic compounds.
Hexachlordisilan, das aus Siliciden hergestellt wird, enthält immer Spuren an Titan und anderen metallischen Verunreinigungen. Titan ist insofern kritisch, da das Titan (IV) Chlorid sich im Siedepunkt nur geringfügig von Hexachlordisilan unterscheidet. Um es abzutrennen, ist eine aufwendige fraktionierte Destillation notwendig.Hexachlorodisilane, which is made from silicides, always contains traces of titanium and other metallic impurities. Titanium is critical in that the titanium (IV) chloride is only slightly different in boiling point from hexachlorodisilane. To separate it, a complex fractional distillation is necessary.
Eine Möglichkeit ist, das bei der Siliziumabscheidung anfallen- de Silangemisch aufzuarbeiten, da die hierzu eingesetztenOne possibility is to work up the silane mixture obtained during the silicon deposition, since the components used for this purpose are
Chlorsilane destillativ vergleichsweise einfach von Titan befreit werden können. Während der Siliziumabscheidung entstehen aus den Chlorsilanen wiederum Disilane, allerdings in Konzent¬ rationen unter 1 Gew.%. Bei der Aufbewahrung dieser Silane in Edelstahlgebinden kann durch Korrosion wiederum Titan im Pro¬ dukt auftreten, das dann wiederum bisher nur durch fraktionierte Destillation abgetrennt werden konnte.Chlorosilanes distillation can be relatively easily removed from titanium. During the silicon deposition% arise from the chlorosilanes turn disilanes, but present in concent ¬ rations at first. When storing these silanes in stainless steel containers Titan Pro ¬ domestic product may occur due to corrosion in turn, which in turn could previously only separated by fractional distillation.
US 3878291 (Apr. 15, 1975, Kleber e.a.) beschreibt ein aufwen- diges Verfahren, um Tetrachlorsilan frei von Titan und anderen Metallen zu erhalten.No. 3,878,291 (Apr. 15, 1975, Kleber et al.) Describes a complex process for obtaining tetrachlorosilane free of titanium and other metals.
Gegenstand der Erfindung ist ein Verfahren zur Entfernung von Titanverbindungen aus Hexachlordisilan, bei dem Hexachlordisilan mit organischer Verbindung (V) , die Struktureinheiten sC-S- oder =C~O- enthält, behandelt wird.The invention relates to a process for the removal of titanium compounds from hexachlorodisilane, in which hexachlorodisilane with organic compound (V), the structural units sC-S- or = C ~ O- treated.
Die Titanverunreinigungen, insbesondere Titan (IV) Chlorid, wer- den durch die organischen Verbindungen (V) , die Struktureinhei- ten =C-S~ oder =C-O- enthalten, gebunden und können dadurch leicht abgetrennt werden.The titanium impurities, in particular titanium (IV) chloride, are formed by the organic compounds (V), the structural components th = CS ~ or = CO- bound, and thus can be easily separated.
Das erfindungsgemäße Verfahren hat den weiteren Vorteil, dass Hexachlordisilan in hoher Reinheit erhalten wird. Reinheiten von höchstens 100, insbesondere höchstens 50 ppb Ti (bezogen auf das Gewicht) sind erreichbar.The process according to the invention has the further advantage that hexachlorodisilane is obtained in high purity. Purity of at most 100, in particular at most 50 ppb of Ti (by weight) are achievable.
Nach der Behandlung mit den Verbindungen (V) können die gebundenen Titanverbindungen auf unterschiedliche Weise vom Hexa- chlordisilan abgetrennt werden. Vorzugsweise werden die gebundenen Titanverbindungen durch Destillation, Dekantieren oder Filtration vom Hexachlordisilan abgetrennt.After the treatment with the compounds (V), the bound titanium compounds can be separated from the hexachlorodisilane in different ways. Preferably, the bound titanium compounds are separated from the hexachlorodisilane by distillation, decantation or filtration.
Die Destillation ist stark vereinfacht gegenüber dem unbehan- delten Hexachlordisilan, denn durch den veränderten Siedepunkt der gebundenen Titanverbindungen kann die aufwendige fraktionierte Destillation entfallen. Vorzugsweise verbleiben die gebundenen Titanverbindungen im Sumpf der Destillation.The distillation is greatly simplified compared to the untreated hexachlorodisilane, because the complicated boiling fraction of the bound titanium compounds eliminates the complicated fractional distillation. Preferably, the bound titanium compounds remain in the bottom of the distillation.
Bei der Entfernung von Titanverbindungen aus Hexachlordisilan kann auch ein Lösungsmittel eingesetzt werden.When removing titanium compounds from hexachlorodisilane, a solvent can also be used.
Die Struktureinheiten =≡C-S- oder ≡C-O- werden vorzugsweise ausgewählt aus den Struktureinheiten ==C-S-H, ≡C-S-C≡ und ≡C-O-ö≡. Auch Di- (≡C-SS-C≡) und trisulfide («C-SSS-G≡O sind geeignet.The structural units = ≡C-S- or ≡C-O- are preferably selected from the structural units == C-S-H, ≡C-S-C≡ and ≡C-O-δ. Di- (≡C-SS-C≡) and trisulfide (CC-SSS-G≡O are also suitable.
Bevorzugte Verbindungen (V) sind cyclische Etherverbindungen, die vorzugsweise mindestens 5 Ringatome und vorzugsweise höchstens 30 Ringatome aufweisen, wie 1 , 3-Dioxolan, Tetrahydrofuran, Tetrahydropyran, Tetrahydro-pyran, 1,4-Dioxan, [12]Krone-4,Preferred compounds (V) are cyclic ether compounds which preferably have at least 5 ring atoms and preferably at most 30 ring atoms, such as 1, 3-dioxolane, tetrahydrofuran, tetrahydropyran, tetrahydropyran, 1,4-dioxane, [12] crown-4,
[15]Krone-5. Die cyclischen Etherverbindungen können Kohlenwasserstoffsubtituenten aufweisen, insbesondere Alkylreste mit 1 bis 6 Kohlenstofatomen, bevorzugt Methyl und Ethyl . Beispiele für substituierte cyclische Etherverbindungen sind 4 -Methyl- 1 , 3 -dioxolan, 3 -Methyl -tetrahydrofuran, 2 , 2-Diτnethyl-l, 4- dioxan.[15] crown-fifth The cyclic ether compounds may have hydrocarbon substituents, in particular alkyl radicals having 1 to 6 carbon atoms, preferably methyl and ethyl. Examples of substituted cyclic ether compounds are 4-methyl 1, 3-dioxolane, 3-methyl-tetrahydrofuran, 2, 2-dimethyl-1, 4-dioxane.
Ebenfalls bevorzugte Verbindungen (V) sind lineare oder verzweigte Ξtherverbindungen (≡C-O~C≡=) , wie Mono- und Polyether. Als Monoether sind Ether mit einem Siedepunkt von mindestens 6O0C bei 1 bar bevorzugt, beispielsweise Di-n-propylether . Als Polyether können auch Polyalkylenglycole, wie Polyethy- lenglycol und Polypropylenglycol eingesetzt werden. Die mittleren Molmassen Mn der Polyalkylenglycole betragen vorzugsweise mindestens 150, insbesondere mindestens 500 und vorzugsweise höchstens 10000, insbesondere höchstens 5000.Also preferred compounds (V) are linear or branched verbindungentherverbindungen (≡CO ~ C≡ =), such as mono- and polyether. As monoethers ethers are preferred with a boiling point of at least 6O 0 C at 1 bar, for example, di-n-propyl ether. Polyethers which can also be used are polyalkylene glycols, such as polyethylene glycol and polypropylene glycol. The average molecular weights Mn of the polyalkylene glycols are preferably at least 150, in particular at least 500 and preferably at most 10000, in particular at most 5000.
Bevorzugte Verbindungen (V) sind auch cyclische und lineare Thioetherverbindungen, wie Dialkylsulfide . Bei den Thiolen (≡C- S-H) sind Verbindungen mit einem Molekulargewicht von mindestens 1000 bevorzugt. Beispiele dafür sind Vinylpolymere mit SH- Gruppen, wie Ionentauscher , z.B. Amberlite® G 73.Preferred compounds (V) are also cyclic and linear thioether compounds, such as dialkyl sulfides. In the thiols (≡C-SH), compounds having a molecular weight of at least 1000 are preferred. Examples of these are vinyl polymers with SH groups, such as ion exchanger, for example Amberlite ® G 73rd
Auf 100 Gewichtsteile Hexachlordisilan werden vorzugsweise min- destens 0,001, besonders bevorzugt mindestens 0,05 Gewichtsteile Verbindung (V) , und vorzugsweise höchstens 10, besonders bevorzugt höchstens 5 Gewichtsteile Verbindung (V), eingesetzt.At least 100 parts by weight of hexachlorodisilane are preferably used for at least 0.001 parts, more preferably at least 0.05 parts by weight of compound (V), and preferably not more than 10, particularly preferably not more than 5 parts by weight of compound (V).
Auch Gemische, die Hexachlordisilan enthalten, können mit orga- nischer Verbindung (V) behandelt werden.Mixtures containing hexachlorodisilane can also be treated with organic compound (V).
Vorzugsweise enthält das eingesetzte Hexachlordisilan höchstens 100 ppm, besonders bevorzugt 10 ppm, insbesondere 1 ppm Titan, jeweils auf das Gewicht bezogen.Preferably, the hexachlorodisilane used contains at most 100 ppm, particularly preferably 10 ppm, in particular 1 ppm of titanium, each by weight.
Es können beispielsweise Hexachlordisilan enthaltende Chlorsi- langemische eingesetzt werden, die aus der Reaktion von HCl mit Calciumsilicid, aus der Reaktion von Chlor mit Silizium oder aus den Prozessabgasen der Abscheidung von polykristallinem Si- lizium erhalten werden, besonders bevorzugt Prozessabgase, die bei der Abscheidung von polykristallinem Silizium erhalten werden. Diese eingesetzten Chlorsilangemische können vor oder während der Aufreinigung mit Chlor behandelt worden sein, um Hydrogenchlorsilane zu Chlorsilanen umzuwandeln, da insbesonde- re Hydrogenchlorsilane mit höherem Wasserstoffgehalt selbstentzündlich sein können.Hexachlorodisilane-containing chlorosilane mixtures obtained, for example, from the reaction of HCl with calcium silicide, from the reaction of chlorine with silicon or from the process offgases of the deposition of polycrystalline silicon, particularly preferably process offgases, can be used obtained in the deposition of polycrystalline silicon. These chlorosilane mixtures used may have been treated with chlorine before or during the purification in order to convert hydrogenchlorosilanes to chlorosilanes, since in particular hydrogenchlorosilanes with a higher hydrogen content may be self-igniting.
Die eingesetzten Chlorsilangemische können auch noch mit weiteren Stoffen, wie z.B. Aktivkohle oder ~ wenn überhaupt - bevor- zugt pyrolytisch oder durch Fällungsprozess hergestellte Kieselsäure, versetzt werden.The chlorosilane mixtures used can also be combined with other substances, such as e.g. Activated charcoal or, if at all, preferably pyrolytic or silica produced by the precipitation process.
Die Behandlung mit organischer Verbindung (V) erfolgt vorzugsweise bei mindestens -50C, vorzugsweise mindestens 15°C.The treatment with organic compound (V) is preferably carried out at at least -5 0 C, preferably at least 15 ° C.
Falls die gebundenen Titanverbindungen durch Destillation abgetrennt werden, kann die Destillation entweder unter Normaldruck, Überdruck oder reduziertem Druck erfolgen.If the bound titanium compounds are separated by distillation, the distillation can be carried out either under normal pressure, overpressure or reduced pressure.
Die erfindungsgemäße Destillation kann in Anwesenheit oder Abwesenheit von Schutzgas, wie Stickstoff, Helium oder Argon, durchgeführt werden,- sie kann aber auch an Luft durchgeführt werden, solange der Feuchtigkeitsgehalt maximal 10 ppbw beträgt. Bevorzugt wird aus Kostengründen die Destillation in An- Wesenheit von Stickstoff durchgeführt.The distillation according to the invention can be carried out in the presence or absence of inert gas, such as nitrogen, helium or argon, but it can also be carried out in air as long as the moisture content is at most 10 ppbw. For reasons of cost, the distillation is preferably carried out in the presence of nitrogen.
Sofern nicht anders angegeben, werden die nachstehenden Beispiele bei einem Druck der umgebenden Atmosphäre, also etwa bei 1000 hPa, und bei Raumtemperatur, also bei etwa 23° durchgeführt .Unless stated otherwise, the examples below are carried out at a pressure of the surrounding atmosphere, ie at about 1000 hPa, and at room temperature, ie at about 23 °.
In den folgenden Beispielen wurde der Gehalt an Verunreinigungen nach Hydrolyse mittels ICP-MS (Ion Coupled Plasma Mass Spectrometrie) bestimmt. Beispiel 1In the following examples, the content of impurities after hydrolysis was determined by ICP-MS (Ion Coupled Plasma Mass Spectrometry). example 1
130 g Hexachlordisilan mit einem Gehalt von 120 ppb Titan wurde 3 Tropfen 1,4-Dioxan versetzt. Das Hexachlordisilan wurde am Rückfluss gekocht und anschließend über eine Brücke abdestilliert.130 g of hexachlorodisilane containing 120 ppb of titanium were mixed with 3 drops of 1,4-dioxane. The hexachlorodisilane was refluxed and then distilled off via a bridge.
Ergebnis rohes Wach Behandlung Hexachlordisilan mit DioxanResult of raw awake treatment hexachlorodisilane with dioxane
Ti [ppb] 80 21Ti [ppb] 80 21
Beispiel 2Example 2
In einem weiteren analogen Versuch wurde ebenfalls 130 g Hexachlordisilan mit 3 Tropfen 3 -Methyl -tetrahydropyran versetzt, am Rückfluss gekocht und anschließend über eine Brücke abdestilliert .In a further analogous experiment, 130 g of hexachlorodisilane were likewise mixed with 3 drops of 3-methyltetrahydropyran, boiled under reflux and then distilled off via a bridge.
Ergebnis rohes Nach Behandlung mitResult raw after treatment with
Hexachlordisilan 3 -Methyl -tetrahydro-pyran Ti [ppb] 190 33Hexachlorodisilane 3-methyltetrahydropyran Ti [ppb] 190 33
Beispiel 3 Es wurden ca 100g Hexachlordisilan mit 4g Amberlite® GT 73 versetzt und 6 Stunden bei Raumtemperatur gerührt. Eine Probe wurde abfiltriert und untersucht .Example 3 ca 100g hexachlorodisilane added with 4 g of Amberlite ® GT 73 stirred at room temperature for 6 hours. A sample was filtered off and examined.
Ergebnis rohes Nach Behandlung mit AmberliteResult raw after treatment with Amberlite
Hexachlordisilan Nach 6 Stunden Ti [ppb] 190 7 Hexachlorodisilane After 6 hours Ti [ppb] 190 7

Claims

Patentansprüche claims
1. Verfahren zur Entfernung von Titanverbindungen aus Hexa- chlordisilan, bei dem Hexachlordisilan mit organischer Ver- bindung (V) , die Struktureinheiten ≡C-S- oder ≡≤C-O- enthält, behandelt wird.1. A process for the removal of titanium compounds from hexachlorodisilane in which hexachlorodisilane is treated with organic compound (V) which contains structural units ≡C-S- or ≡≤C-O-.
2. Verfahren nach Anspruch 1, bei dem die Titanverbindungen mit Verbindung (V) gebunden werden und die gebundenen Ti- tanverbindungen, durch Destillation, Dekantieren oder Filtration vom Hexachlordisilan abgetrennt werden.2. Process according to claim 1, in which the titanium compounds are bonded with compound (V) and the bound titanium compounds are separated off from hexachlorodisilane by distillation, decantation or filtration.
3. Verfahren nach Anspruch 1 oder 2, bei dem Titan (IV) Chlorid entfernt wird.3. The method of claim 1 or 2, wherein the titanium (IV) chloride is removed.
4. Verfahren nach Anspruch 1 bis 3, bei dem die Struktureinheiten der Verbindung (V) ausgewählt werden aus ≡C-S-H, =C- S-Cs und =C-O-C≡.4. The method of claim 1 to 3, wherein the structural units of the compound (V) are selected from ≡C-S-H, = C-S-Cs and = C-O-C≡.
5. Verfahren nach Anspruch 1 bis 4, bei dem als Verbindungen (V) eyeIisehe Etherverbindungen eingesetzt werden.5. The method according to claim 1 to 4, wherein as compounds (V) eyeIisehe ether compounds are used.
6. Verfahren nach Anspruch 1 bis 4, bei dem als Verbindungen6. The method according to claim 1 to 4, wherein as compounds
(V) Vinylpolymere mit SH~Gruppen eingesetzt werden. (V) Vinyl polymers with SH ~ groups are used.
EP09783845A 2008-10-17 2009-10-08 Method for removing titanium from hexachlorodisilane Withdrawn EP2337765A1 (en)

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DE102008042936A DE102008042936A1 (en) 2008-10-17 2008-10-17 Process for removing titanium from hexachlorodisilane
PCT/EP2009/063087 WO2010043536A1 (en) 2008-10-17 2009-10-08 Method for removing titanium from hexachlorodisilane

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KR101327625B1 (en) 2013-11-12
DE102008042936A1 (en) 2010-04-22
CN102171143B (en) 2013-10-16
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US20110182794A1 (en) 2011-07-28
US8226919B2 (en) 2012-07-24

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