WO2006054325A2 - Process and plant for the purification of trichlorosilane and silicon tetrachloride - Google Patents
Process and plant for the purification of trichlorosilane and silicon tetrachloride Download PDFInfo
- Publication number
- WO2006054325A2 WO2006054325A2 PCT/IT2005/000662 IT2005000662W WO2006054325A2 WO 2006054325 A2 WO2006054325 A2 WO 2006054325A2 IT 2005000662 W IT2005000662 W IT 2005000662W WO 2006054325 A2 WO2006054325 A2 WO 2006054325A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- purification
- trichlorosilane
- silicon tetrachloride
- compounds
- distillation
- Prior art date
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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
-
- 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
Definitions
- the present invention concerns a process and plant for the purification of trichlorosilane and silicon tetrachloride.
- the invention refers to the purification of technical grade trichlorosilane and silicon tetrachloride in order to obtain electronic grade trichlorosilane and silicon tetrachloride.
- the raw material for the production of silicon polycrystals for electronic use is constituted by technical grade trichlorosilane (also identified by means of the acronym TCS TG, wherein TCS stands for trichlorosilane and TG stands for technical grade) and/or silicon tetrachloride (identified, with the same above methodology, by means of the acronym TET TG).
- the presence of the said impurities prevents technical grade trichlorosilane and silicon tetrachloride from being used in processes for the production of semiconductors, wherein the electrical resistivity control is managed by a rigorous control of doping impurities.
- the hydrochloric acid used in the synthesis of chlorosilanes being a recycle product from the production of organosilanes, is generally contamined by carbon impurities.
- TCS TG and TET TG In order to use TCS TG and TET TG in these processes, i.e. can be classified as having an electronic purity grade, they must be further purified, in order to reduce the concentration of impurities by a factor of at least 10000 or 100000 times.
- the purification of TCS TG or TET TG is generally obtained by means of hyper distillation, based on the difference between the impurities boiling temperature and the TCS and TET boiling temperatures.
- An alternative purification process is constituted by the purification process by means of wet nitrogen bubbles.
- the reaction of TCS and/or TET with moisture carried by nitrogen leads to the formation of SiO2 and high boiling point poly-siloxanes (Si-OH bonds), acting also as complexing agents.
- the purity grade that is obtainable by means of the purification process with "wet N2" does not exceed a P-type value of 100 ohm-cm.
- the complexing effect of the H2O molecules and of the polysiloxanes is in any case lower then the complexing capacity proper of electron rich big molecules.
- the purity level that can be obtained by means of the above said process can be successfully used in cases where a TCS EG having a p-type value of 1000 ohm-cm is considered sufficient. In fact, this kind of process was developed in a period when this level of purity was able to meet the market requirements.
- these additives (about ten are listed in the patent) have a very high electron number and consequently have a great aptitude to the formation of covalent bonds, N (nitrogen) bonds, S (sulfur) bonds, OH groups (examples: 6-methyl-2-thiouracil, N(phenyl)N- CH3-SH, , N-methyl-2-thioimidazoline, H-N(phenyl)N-CH3-S, phenothiazine, HN-(phenyl-phenyl)S).
- This process also was developed in the second half of the sixties, when a TCS EG purity level around p-type levels of about 1000 ohm-cm was considered sufficient in order to meet the market requirements.
- the solution according to the present invention is to be considered in this context, with the aim of providing a process and a plant for the purification of technical grade trichlorosilane and silicon tetrachloride in order to obtain electronic grade trichlorosilane and silicon tetrachloride, by means of a reaction of complexation of the boron impurities (trichloride BCI3) and other metallic impurities, optionally present, with diphenylthiocarbazone (Ditizone or also DTZ) and triphenylchloromethane (TCM), and subsequent removal of the complexation products and the remaining impurities.
- trichloride BCI3 boron impurities
- other metallic impurities optionally present
- TCM triphenylchloromethane
- the purification process according to the invention can comprise a further distillation step of the bottoms of said second distillation, through which trichlorosilane and/or dichlorosilane free silicon tetrachloride are obtained as tops and phosphorus chlorides PCI3 and phosphorus containing components, arsenic chlorides AsCI3 and arsenic containing compounds, aluminium compounds, antimony compounds and in general all the metals and metalloids and carbon-silanes compounds which are present are obtained as bottoms.
- said complexation step takes place by adding an excess amount, with respect to the stoichiometric amount, of one or both diphenylthiocarbazone and/or triphenylchloromethane.
- said complexation step takes place by adding diphenylthiocarbazone in an amount that is twice the amount of triphenylchloromethane.
- the bottom temperature in said first distillation step is comprised between 38 and
- said first distillation step is initially operated with a total reflux of the tops, in order to allow the boron and other metals impurities complete complexation, preferably for a time period of at least 3 hours, and, following that period of total reflux, the distillation is conducted with a top reflux flow comprised between 0,3 as a minimum and 2,8 as a maximum, preferably 1 ,33 as far as TCS is concerned and between 0,17 as a minimum and 5 as a maximum, preferably 2,5 as far as TET is concerned.
- Said values represents the reflux ratio, i.e. the ratio between the flow of condensate tops returned to the top of the column and the flow of extracted tops (distillate)).
- a plant for the purification of trichlorosilane and/or silicon tetrachloride comprising the following apparatuses for treating technical grade trichlorosilane and/or technical grade silicon tetrachloride:
- trichlorosilane and/or dichlorosilane free silicon tetrachloride are obtained as tops and phosphorus chlorides PCI3, phosphorus containing compounds, arsenic chlorides AsCI3 and arsenic containing compounds, aluminium compounds, antimony compounds and in general all the metals and metalloid and carbon-silanes compounds that are present, together with a certain residual amount of trichlorosilane and/or silicon tetrachloride, are obtained as bottoms.
- the bottom temperature in said complexation and distillation column is comprised between 38 and 48°C (preferably is 42 0 C) for the purification of trichlorosilane and between 65 and 75°C (preferably 69°C) for the purification of silicon tetrachloride, while the thermal fluid temperature of the exchanger at the bottom of the column is comprised between 58 and 73°C (preferably is 60 0 C) for the purification of trichlorosilane and between 75 and 83 0 C (preferably 79°C).
- the purification plant according to the present invention further comprises linking conduits between the different apparatuses, linking conduits to other plants, inlet conduits for the materials to treat and outlet conduits for the treated materials, pumps, adjustment and control instruments.
- TCM and DTZ allow to realise the complexation of TCS and TET impurities also if singularly used (TCM allows the complexation of many metals except boron), the use of these complexing agents together is needed in order to complex all the impurities.
- TCM and DTZ shows optimal complexation efficiency, creating a synergy with respect to the separate and/or sequential use of said two complexing agents.
- the complexation and distillation column 1 is the device wherein boron impurities (trichloride BCI3) and other metallic impurities are removed from trichlorosilane TCS TG and/or from silicon tetrachloride TET TG by means of a batch process constituted by a complexation reaction of said impurities with diphenylthiocarbazone (Ditizone or DTZ) and triphenylchloromethane (TCM).
- DTZ diphenylthiocarbazone
- TCM triphenylchloromethane
- the complexing additives promote the formation of covalent bonds between the impurities and additives themselves, causing the formation of high boiling complex macromolecules.
- the reaction takes place between the big molecules of Ditizone and TCM, rich in available electrons, and the molecules of BCI3 and other boron compounds and possibly other metallic chlorides molecules poor in electrons, forming strong complexes having a very high boiling point.
- the bottom of the complexation and distillation column 1 is heated by means of a heat exchanger 4, inside which a thermal fluid flows, whose temperature is comprised between 58 and 73°C (preferably is equal to 60 0 C), in the case of trichlorosilane purification and between 75 and 83°C (preferably 79°C) for the purification of silicon tetrachloride.
- Heating the bottom of column 1 causes the evaporation of the lowest boiling compounds comprised in the blend to treat. These compounds begins to ascend along column 1 , passing through the different stages in which the column is divided up to the top stage.
- a condenser 5 causes the vapours condensation and their reflux to the column.
- an equilibrium is set between the vapour flow ascending inside column 1 and the liquid flow descending inside the same column 1 and complexed boron impurities separation is obtained, this impurities being removed as bottoms of column 1 together with other complexed metallic impurities.
- column 1 is initially operated with a 100% reflux at the top. After the equilibrium condition are reached, column 1 is operated according to design specifications untill the complete depletion of the batch.
- the tops of column 1 are used to feed an intermediate section of the distillation column 2, in which electronic grade trichlorosilane (and dichlorosilane possibly present) and/or silicon tetrachloride are obtained as tops and phosphorus chlorides PCI3 and phosphorus containing compounds, arsenic chlorides AsCI3 and arsenic containing compounds, aluminium compounds, antimony compounds and in general all the present metals and metalloid and carbon-silanes compounds, together with a certain residual amount of trichlorosilane and/or silicon tetrachloride, are obtained as bottoms.
- electronic grade trichlorosilane (and dichlorosilane possibly present) and/or silicon tetrachloride are obtained as tops and phosphorus chlorides PCI3 and phosphorus containing compounds, arsenic chlorides AsCI3 and arsenic containing compounds, aluminium compounds, antimony compounds and in general all the present metals and metalloid and carbon-silanes compounds
- the distillation column 2 is a common packed column, with a condenser 6 at the top and a reboiler 7 at the bottom.
- an intermediate vessel 8 is shown, in which the tops of column 1 are accumulated in order to constitute a reserve for the feed of the distillation column 2, during the starting phase of the subsequent operative cycle of the complexation and distillation column 1.
- the tops of column 1 can be mixed together with a flow of trichlorosilane, dichlorosilane and various impurities (not comprising boron and/or other metallic impurities), coming from the reactors of a polycrystalline silicon production plant.
- distillation column 2 The bottoms of distillation column 2 are used to feed the intermediate section of a further distillation column 3, which is present in case the electronic grade trichlorosilane has to be used for the deposition of epitaxial layers.
- TCS EG suitable to produce silicon polycrystal contains a certain percentage of dichlorosilane (DCS) that must be removed if the TCS EG is used for the deposition of epitaxial layers.
- DCS dichlorosilane
- the distillation column 3 is also a packed column, with a condenser 9 at the top and a reboiler 10 at the bottom, in which trichlorosilane and/or dichlorosilane free silicon tetrachloride are obtained as tops and phosphorus chlorides PCI3 and phosphorus containing compounds, arsenic chlorides AsCI3 and arsenic containing compounds, aluminium compounds, antimony compounds and in general all the present metals and metalloids and carbon-silanes compounds are obtained as bottoms.
- Table 1 shows the features of TCS TG fed to the complexation and distillation column 1.
- TCS (% by weight) > 99,7 DCS (% by weight) ⁇ 0,1 TET (% by weight) ⁇ 0,2
- Table 2 shows the features of TET TG fed to the complexation and distillation column 1.
- Titanium (mg/kg) ⁇ 0,01 Metals total (mg/kg) ⁇ 0,30 Aluminium (mg/kg) ⁇ 0,10 Boron (mg/kg) ⁇ 0,50 Sodium (mg/kg) ⁇ 0,50
- Complexation and distillation column 1 level above 2500 kg (preferably 6900 kg) for TCS; above 3500 kg (preferably 11500 kg) for TET.
- Complexing agent amount preferably 50 g of TCM and 25 g of DTZ for TCS; 100 g of TCM and 50 g of DTZ for TET.
- Top reflux flow at Total Reflux conditions (during the starting and complexation phase): between 3100 and 3800 kg/h (preferably 3500 kg/h) for TCS; between 3500 and 6000 kg/h (preferably 5000 kg/h) for TET.
- Top extraction flow (distillate after complexation time): between 1000 and 2400 kg/h (preferably 1500 kg/h) for TCS; between 1000 and 3000 kg/h (preferably 2000 kg/h) for TET.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
Description
Claims
Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US11/719,688 US7879198B2 (en) | 2004-11-19 | 2005-11-14 | Processes for the purification of trichlorosilane and silicon tetrachloride |
EP05813212.7A EP1812343B1 (en) | 2004-11-19 | 2005-11-14 | Process and plant for the purification of trichlorosilane and silicon tetrachloride |
CN2005800397157A CN101065324B (en) | 2004-11-19 | 2005-11-14 | Process and plant for the purification of trichlorosilane and silicon tetrachloride |
JP2007542519A JP2008520535A (en) | 2004-11-19 | 2005-11-14 | Method and plant for purifying trichlorosilane and silicon tetrachloride |
NO20073126A NO342558B1 (en) | 2004-11-19 | 2007-06-18 | Process and plant for the purification of trichlorosilane and silicon tetrachloride |
US13/014,532 US8282792B2 (en) | 2004-11-19 | 2011-01-26 | Process and system for the purification of trichlorosilane and silicon tetrachloride |
US13/606,953 US8691055B2 (en) | 2004-11-19 | 2012-09-07 | Processes for the purification of trichlorosilane or silicon tetrachloride |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
ITRM2004A000570 | 2004-11-19 | ||
IT000570A ITRM20040570A1 (en) | 2004-11-19 | 2004-11-19 | PROCEDURE AND PLANT FOR THE PURIFICATION OF TRICHLOROSILANE AND SILICON TETRACLORIDE. |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US11/719,688 A-371-Of-International US7879198B2 (en) | 2004-11-19 | 2005-11-14 | Processes for the purification of trichlorosilane and silicon tetrachloride |
US13/014,532 Continuation US8282792B2 (en) | 2004-11-19 | 2011-01-26 | Process and system for the purification of trichlorosilane and silicon tetrachloride |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2006054325A2 true WO2006054325A2 (en) | 2006-05-26 |
WO2006054325A3 WO2006054325A3 (en) | 2006-07-06 |
Family
ID=36250726
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/IT2005/000662 WO2006054325A2 (en) | 2004-11-19 | 2005-11-14 | Process and plant for the purification of trichlorosilane and silicon tetrachloride |
Country Status (10)
Country | Link |
---|---|
US (3) | US7879198B2 (en) |
EP (2) | EP2634143A3 (en) |
JP (1) | JP2008520535A (en) |
KR (1) | KR100981813B1 (en) |
CN (1) | CN101065324B (en) |
IT (1) | ITRM20040570A1 (en) |
NO (1) | NO342558B1 (en) |
RU (1) | RU2393991C2 (en) |
SG (2) | SG158071A1 (en) |
WO (1) | WO2006054325A2 (en) |
Cited By (9)
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DE102007014107A1 (en) | 2007-03-21 | 2008-09-25 | Evonik Degussa Gmbh | Work-up of boron-containing chlorosilane streams |
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DE102008004396A1 (en) | 2008-01-14 | 2009-07-16 | Evonik Degussa Gmbh | Plant and method for reducing the content of elements, such as boron, in halosilanes |
WO2009126218A1 (en) * | 2008-04-07 | 2009-10-15 | Lord Stephen M | A process for removing aluminum and other metal chlorides from chlorosilanes |
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US8298490B2 (en) | 2009-11-06 | 2012-10-30 | Gtat Corporation | Systems and methods of producing trichlorosilane |
US8535488B2 (en) | 2009-12-28 | 2013-09-17 | Lg Chem, Ltd. | Method and apparatus for purification of trichlorosilane |
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2004
- 2004-11-19 IT IT000570A patent/ITRM20040570A1/en unknown
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2005
- 2005-11-14 CN CN2005800397157A patent/CN101065324B/en active Active
- 2005-11-14 KR KR1020077013735A patent/KR100981813B1/en active IP Right Grant
- 2005-11-14 RU RU2007122758/15A patent/RU2393991C2/en active
- 2005-11-14 EP EP13156857.8A patent/EP2634143A3/en not_active Withdrawn
- 2005-11-14 SG SG200907702-5A patent/SG158071A1/en unknown
- 2005-11-14 US US11/719,688 patent/US7879198B2/en active Active
- 2005-11-14 JP JP2007542519A patent/JP2008520535A/en active Pending
- 2005-11-14 EP EP05813212.7A patent/EP1812343B1/en active Active
- 2005-11-14 WO PCT/IT2005/000662 patent/WO2006054325A2/en active Application Filing
- 2005-11-14 SG SG2013038559A patent/SG191588A1/en unknown
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2007
- 2007-06-18 NO NO20073126A patent/NO342558B1/en unknown
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2011
- 2011-01-26 US US13/014,532 patent/US8282792B2/en active Active
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2012
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Cited By (21)
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DE102007014107A1 (en) | 2007-03-21 | 2008-09-25 | Evonik Degussa Gmbh | Work-up of boron-containing chlorosilane streams |
WO2008113619A2 (en) * | 2007-03-21 | 2008-09-25 | Evonik Degussa Gmbh | Processing of chlorosilane flows containing boron |
WO2008113619A3 (en) * | 2007-03-21 | 2009-04-30 | Evonik Degussa Gmbh | Processing of chlorosilane flows containing boron |
US8246925B2 (en) | 2007-03-21 | 2012-08-21 | Evonik Degussa Gmbh | Processing of chlorosilane flows containing boron |
WO2009089950A2 (en) * | 2008-01-14 | 2009-07-23 | Evonik Degussa Gmbh | Method for reducing the content in elements, such as boron, in halosilanes and installation for carrying out said method |
JP2011514871A (en) * | 2008-01-14 | 2011-05-12 | エボニック デグサ ゲーエムベーハー | Apparatus and method for reducing the content of elements such as boron in halogen silanes |
WO2009089951A2 (en) * | 2008-01-14 | 2009-07-23 | Evonik Degussa Gmbh | Installation and method for reducing the content in elements, such as boron, of halosilanes |
RU2504515C2 (en) * | 2008-01-14 | 2014-01-20 | Эвоник Дегусса Гмбх | Method of reducing content of boron-type elements in halosilanes and apparatus for realising said method |
RU2502669C2 (en) * | 2008-01-14 | 2013-12-27 | Эвоник Дегусса Гмбх | Device and method of reducing content of boron type elements in halosilanes |
WO2009089950A3 (en) * | 2008-01-14 | 2010-01-28 | Evonik Degussa Gmbh | Method for reducing the content in elements, such as boron, in halosilanes and installation for carrying out said method |
DE102008004397A1 (en) | 2008-01-14 | 2009-07-16 | Evonik Degussa Gmbh | Process for reducing the content of elements, such as boron, in halosilanes and plant for carrying out the process |
WO2009089951A3 (en) * | 2008-01-14 | 2011-01-27 | Evonik Degussa Gmbh | Installation and method for reducing the content in elements, such as boron, of halosilanes |
JP2011509907A (en) * | 2008-01-14 | 2011-03-31 | エボニック デグサ ゲーエムベーハー | Method for reducing the content of elements such as boron in halogen silanes and apparatus for carrying out the method |
DE102008004396A1 (en) | 2008-01-14 | 2009-07-16 | Evonik Degussa Gmbh | Plant and method for reducing the content of elements, such as boron, in halosilanes |
US7736614B2 (en) | 2008-04-07 | 2010-06-15 | Lord Ltd., Lp | Process for removing aluminum and other metal chlorides from chlorosilanes |
WO2009126218A1 (en) * | 2008-04-07 | 2009-10-15 | Lord Stephen M | A process for removing aluminum and other metal chlorides from chlorosilanes |
DE102008002537A1 (en) | 2008-06-19 | 2009-12-24 | Evonik Degussa Gmbh | Process for the removal of boron-containing impurities from halosilanes and plant for carrying out the process |
US8298490B2 (en) | 2009-11-06 | 2012-10-30 | Gtat Corporation | Systems and methods of producing trichlorosilane |
US8535488B2 (en) | 2009-12-28 | 2013-09-17 | Lg Chem, Ltd. | Method and apparatus for purification of trichlorosilane |
EP2385017A1 (en) * | 2010-05-05 | 2011-11-09 | Shyang Su | Process for purifying silicon source material by high gravity roating packed beds |
EP2993157A3 (en) * | 2010-10-05 | 2016-06-22 | MEMC Electronic Materials, Inc. | Processes and systems for purifying silane |
Also Published As
Publication number | Publication date |
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SG191588A1 (en) | 2013-07-31 |
SG158071A1 (en) | 2010-01-29 |
KR100981813B1 (en) | 2010-09-13 |
EP1812343B1 (en) | 2016-05-11 |
RU2007122758A (en) | 2008-12-27 |
US8282792B2 (en) | 2012-10-09 |
US20080314728A1 (en) | 2008-12-25 |
NO342558B1 (en) | 2018-06-18 |
EP2634143A3 (en) | 2014-09-10 |
RU2393991C2 (en) | 2010-07-10 |
JP2008520535A (en) | 2008-06-19 |
US20110114469A1 (en) | 2011-05-19 |
ITRM20040570A1 (en) | 2005-02-19 |
NO20073126L (en) | 2007-06-18 |
US8691055B2 (en) | 2014-04-08 |
WO2006054325A3 (en) | 2006-07-06 |
CN101065324A (en) | 2007-10-31 |
EP1812343A2 (en) | 2007-08-01 |
KR20070086356A (en) | 2007-08-27 |
US20120325645A1 (en) | 2012-12-27 |
CN101065324B (en) | 2011-03-16 |
US7879198B2 (en) | 2011-02-01 |
EP2634143A2 (en) | 2013-09-04 |
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