EP3102539A1 - Method for producing polycrystalline silicon - Google Patents
Method for producing polycrystalline siliconInfo
- Publication number
- EP3102539A1 EP3102539A1 EP15701014.1A EP15701014A EP3102539A1 EP 3102539 A1 EP3102539 A1 EP 3102539A1 EP 15701014 A EP15701014 A EP 15701014A EP 3102539 A1 EP3102539 A1 EP 3102539A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- silicon
- hydrogen
- reactor
- carrier body
- oxide layer
- 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- Withdrawn
Links
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
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/24—Deposition of silicon only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4408—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber by purging residual gases from the reaction chamber or gas lines
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/90—Other crystal-structural characteristics not specified above
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02524—Group 14 semiconducting materials
- H01L21/02532—Silicon, silicon germanium, germanium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02587—Structure
- H01L21/0259—Microstructure
- H01L21/02595—Microstructure polycrystalline
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
Definitions
- the invention relates to a process for the production of polycrystalline silicon.
- High purity polycrystalline silicon (polysilicon) serves as a starting material for the production of single crystal silicon for semiconductors according to the Czochralski (CZ) or zone melting (FZ) method, as well as for the production of single or multicrystalline silicon by various drawing and casting processes for production from
- Polysilicon is usually produced by means of the Siemens process.
- a reaction gas comprising one or more silicon-containing
- Silane (SiH), monochlorosilane (SiH 3 Cl), dichlorosilane (SiH 2 Cl 2 ), trichlorosilane (SiHCl 3 ), tetrachlorosilane (SiCl 4 ) or mixtures of the substances mentioned are preferably used as silicon-containing components.
- the Siemens process is usually carried out in a separator reactor (also called “Siemens reactor”).
- the reactor comprises a metallic base plate and a coolable bell placed on the base plate so that a reaction space inside the bell
- the base plate is provided with one or more gas inlet openings and one or more exhaust openings for the outgoing reaction gases and with
- Each support body usually consists of two thin filament rods and a bridge, which usually connects adjacent rods at their free ends.
- the filament rods are made of monocrystalline or polycrystalline silicon, less frequently metals or alloys or carbon are used.
- High-purity polysilicon deposits on the heated filament rods and the horizontal bridge, causing their diameter to increase over time. After the desired diameter is reached, the process is terminated by stopping the supply of silicon-containing components.
- US 2013/236642 A1 discloses a process for the production of rod-shaped, polycrystalline silicon with a rod diameter of> 100 mm, by
- Dependent temperature required power is at least 50% of the power at the end of deposition, but not less than 5 kW per 1 m rod length, and the cooled Si rods in the vertical cross-section cracks and / or radial
- the Si rods should during the cooling phase at least up to a
- Rod temperature of 800 ° C are brought into contact with hydrogen.
- the pressure in the reactor should be between 2 and 30 bar.
- the polycrystalline silicon rods receive defined cracks and stresses and can be broken more easily in later processing.
- the examples given were in a Siemens reactor with 8 bars
- the thin rods used were made of hyperpure silicon with a length of 2 m and had a diameter of 5 mm.
- a mixture of hydrogen and trichlorosilane was used for the deposition.
- the temperature of the bars was 1000 ° C throughout the deposition time.
- the pressure in the reactor was 3 bar.
- the deposition ran until the bars reached the diameter of 160 mm.
- the power required at the end of the deposition was about 25 kW per 1 m rod length.
- the pressure was increased to 10 bar or adjusted to ambient pressure (about 1 bar).
- US 2012 / 100302A1 discloses a process for producing polycrystalline silicon rods by depositing silicon on at least one thin rod in a reactor, wherein before the silicon deposition hydrogen halide at a thin rod temperature of 400-1000 ° C in the reactor containing at least one Introduced thin rod, irradiated by UV light, causing halogen and
- the carrier body In order to heat the carrier body to a temperature at which silicon is deposited, they must be ignited.
- several possibilities are known, e.g. Igniting by means of a so-called.
- a high voltage is applied to the carrier body.
- the high voltage leads to a current flow through the silicon carrier body after some time.
- the carrier body ignites.
- the current flow leads to a heating of the carrier body, which in turn leads to a reduction of the resistance and allows higher current flows and thus better heating.
- the oxide layer Before silicon can be deposited on the heated carrier body, the oxide layer must be removed thereon.
- Oxide layer thickness corresponds, removed. Subsequently, the supply of HCl is reduced or stopped. The removal of the oxide layer takes less than 20 minutes.
- the support bodies are heated to 1 150 ° C. In the gas are 30% HCl, 5% TCS and 65%
- the disadvantage is that HCl has to be added to the reaction gas mixture in order to completely remove the native oxide in an acceptable time. Without the addition of HCl, the oxide removal takes more than 1 hour.
- the object of the invention is achieved by a process for producing polycrystalline silicon, in which a reaction gas containing a silicon containing component and hydrogen is introduced into a reactor, wherein the reactor comprises at least one support body made of silicon, which is heated by direct current passage, wherein the silicon-containing component is decomposed and polycrystalline silicon deposited on the at least one support body, characterized in that the at least one carrier body made of silicon has an oxide layer which, before the deposition of
- Polycrystalline silicon on the at least one support body is removed by the at least one support body is heated to a temperature of 1100-1200 ° C and exposed at an installation pressure of 0.1 to 5 barü an atmosphere containing hydrogen by a purge gas containing hydrogen the Reactor is supplied.
- the system pressure is 0, 1 to 1 barü.
- the amount of purge gas based on the reactor volume is 10 - 25 Nm 3 / h per m 3 reactor volume, more preferably 14 to 19 Nm 3 / h per m 3
- the purge gas consists of hydrogen with a purity of 99 to 99.9999999% by volume ("fresh hydrogen").
- the oxide layer can be removed in less than 20 minutes. It is not necessary to add HCl or HF.
- Reactor for the deposition of polycrystalline silicon is removed and cleaned, and small amounts of HCl (0.05 vol%), SiH 4 (0.15 wt .-%) and H 3 SiCl (0.1
- an exhaust gas is produced which is conducted from the reactor to an exhaust gas treatment system, in particular an exhaust gas scrubber, or to a condensation device.
- the remaining after the condensation gaseous portions of the exhaust gas can be fed to adsorption.
- hydrogen is released from
- a condensation system offers advantages, as the consumption of hydrogen is thus 50% lower than when using a scrubber. Consumed hydrogen is preferably replaced by fresh hydrogen. The disadvantage is that the removed with the aid of hydrogen oxide layer lands as an impurity in the gas cycle and thus can adversely affect the product quality of the polycrystalline silicon produced. For this reason, the use of a condensation system is less preferred.
- the rinsing hydrogen is introduced at the outlet of the reactor into an exhaust gas scrubber with liquid absorption medium, preferably water, and then released into the free atmosphere. Depending on regulatory requirements can also be dispensed with an exhaust scrubber and the exhaust gas are discharged directly into the atmosphere.
- the exhaust gas hydrogen chloride at the reactor outlet
- the exhaust gas is gradually cooled and compacted over several stages with different cooling media, such as water, brine, oil, etc.
- the thus purified exhaust gas can be fed back to the reactors as Switzerlandas.
- the system pressure 0.1 -5 barü
- the scrubber pressure is greater than 0.0 bar and less than 0.3 bar.
- the pressure in the condensation is greater than 5.0 barü.
- Table 1 shows the procedures for two comparative examples (scrubber / condensation) and for Examples 1 and 2 according to the invention.
- the comparative examples show two different ways of working, which are not according to the invention.
- Nitrogen atmosphere is lowered under flushing hydrogen, the system pressure to about 0.4 bar overpressure and then raised again to 5.5 bar overpressure. This cycle lasts about 15 minutes and is repeated 3 times.
- Comparative Example 2 compared to Comparative Example 1, 240 Nm 3 / h of hydrogen is saved.
- Nitrogen atmosphere is lowered under flushing hydrogen, the system pressure to about 0.4 bar overpressure and then raised again to 5.5 bar overpressure. This cycle lasts about 15 minutes and is repeated 2.5 times. Thus, the system pressure is at the end at 0.4 barü.
- Nitrogen atmosphere is lowered under flushing hydrogen, the system pressure to about 0.4 bar overpressure and then raised again to 5.5 bar overpressure. This cycle lasts about 15 minutes and is repeated 3.5 times. Thus, the system pressure is at the end at 0.4 barü.
- Example 2 a fourth pressure change takes place (duration 15 min).
- the batch change time is thereby reduced by 68 minutes in Example 1 and by 59 minutes in Example 2. This is associated with corresponding increases in the
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Silicon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102014201893.5A DE102014201893A1 (en) | 2014-02-03 | 2014-02-03 | Process for producing polycrystalline silicon |
PCT/EP2015/051284 WO2015113894A1 (en) | 2014-02-03 | 2015-01-22 | Method for producing polycrystalline silicon |
Publications (1)
Publication Number | Publication Date |
---|---|
EP3102539A1 true EP3102539A1 (en) | 2016-12-14 |
Family
ID=52395076
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP15701014.1A Withdrawn EP3102539A1 (en) | 2014-02-03 | 2015-01-22 | Method for producing polycrystalline silicon |
Country Status (10)
Country | Link |
---|---|
US (1) | US10150675B2 (en) |
EP (1) | EP3102539A1 (en) |
JP (1) | JP6250827B2 (en) |
KR (1) | KR101895700B1 (en) |
CN (1) | CN105980304B (en) |
CA (1) | CA2938453C (en) |
DE (1) | DE102014201893A1 (en) |
MY (1) | MY176276A (en) |
TW (1) | TWI546426B (en) |
WO (1) | WO2015113894A1 (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109562951A (en) * | 2016-12-14 | 2019-04-02 | 瓦克化学股份公司 | The method for being used to prepare polysilicon |
CN110571151B (en) * | 2019-09-02 | 2021-10-26 | 武汉新芯集成电路制造有限公司 | Manufacturing method of polycrystalline silicon layer, flash memory and manufacturing method thereof |
Family Cites Families (22)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1202771B (en) | 1960-01-15 | 1965-10-14 | Siemens Ag | Process for producing high purity single crystal silicon |
US3328199A (en) | 1960-01-15 | 1967-06-27 | Siemens Ag | Method of producing monocrystalline silicon of high purity |
DE1147567B (en) * | 1960-01-15 | 1963-04-25 | Siemens Ag | Process for obtaining, in particular, single-crystal, semiconducting silicon |
DE1202711B (en) * | 1961-12-14 | 1965-10-07 | Rose Brothers Ltd | Device for bringing together and conveying flat pieces of goods, especially pieces of candy |
DE1238449B (en) | 1962-06-15 | 1967-04-13 | Siemens Ag | Process for producing single crystal silicon |
JPS52151616A (en) | 1976-06-12 | 1977-12-16 | Komatsu Denshi Kinzoku Kk | Producing method and apparatus of bar form high purity silicon |
DE2854707C2 (en) | 1978-12-18 | 1985-08-14 | Wacker-Chemitronic Gesellschaft für Elektronik-Grundstoffe mbH, 8263 Burghausen | Device for the thermal decomposition of gaseous compounds and their use |
US5352636A (en) | 1992-01-16 | 1994-10-04 | Applied Materials, Inc. | In situ method for cleaning silicon surface and forming layer thereon in same chamber |
DE19608885B4 (en) | 1996-03-07 | 2006-11-16 | Wacker Chemie Ag | Method and device for heating carrier bodies |
KR100210261B1 (en) * | 1997-03-13 | 1999-07-15 | 이서봉 | Method of production for poly crystal silicon |
JP4150532B2 (en) * | 2002-04-11 | 2008-09-17 | 株式会社大阪チタニウムテクノロジーズ | Polycrystalline silicon |
JP4554435B2 (en) * | 2005-05-23 | 2010-09-29 | 株式会社大阪チタニウムテクノロジーズ | Polycrystalline silicon cleaning method |
DE102006037020A1 (en) * | 2006-08-08 | 2008-02-14 | Wacker Chemie Ag | Method and apparatus for producing high purity polycrystalline silicon with reduced dopant content |
JP5509578B2 (en) | 2007-11-28 | 2014-06-04 | 三菱マテリアル株式会社 | Polycrystalline silicon manufacturing apparatus and manufacturing method |
CN101660210A (en) * | 2009-09-03 | 2010-03-03 | 无锡中彩科技有限公司 | Silicon core cleaning technique |
JP5751748B2 (en) * | 2009-09-16 | 2015-07-22 | 信越化学工業株式会社 | Polycrystalline silicon lump group and method for producing polycrystalline silicon lump group |
DE102009044991A1 (en) | 2009-09-24 | 2011-03-31 | Wacker Chemie Ag | Rod-shaped polysilicon with improved fracture property |
JP2011139987A (en) * | 2010-01-07 | 2011-07-21 | Tokuyama Corp | Method for treating purged exhaust gas and use as hydrogen source |
US20110206842A1 (en) * | 2010-02-25 | 2011-08-25 | Vithal Revankar | CVD-Siemens Reactor Process Hydrogen Recycle System |
DE102010042869A1 (en) | 2010-10-25 | 2012-04-26 | Wacker Chemie Ag | Process for the production of polycrystalline silicon rods |
CN102205967A (en) * | 2011-04-29 | 2011-10-05 | 宁夏阳光硅业有限公司 | Energy-saving polysilicon reduction furnace and manufacturing method for polysilicon |
DE102011078676A1 (en) | 2011-07-05 | 2013-01-10 | Wacker Chemie Ag | Process for the production of polysilicon |
-
2014
- 2014-02-03 DE DE102014201893.5A patent/DE102014201893A1/en not_active Withdrawn
-
2015
- 2015-01-22 WO PCT/EP2015/051284 patent/WO2015113894A1/en active Application Filing
- 2015-01-22 CA CA2938453A patent/CA2938453C/en not_active Expired - Fee Related
- 2015-01-22 MY MYPI2016001342A patent/MY176276A/en unknown
- 2015-01-22 US US15/116,251 patent/US10150675B2/en not_active Expired - Fee Related
- 2015-01-22 KR KR1020167024386A patent/KR101895700B1/en active IP Right Grant
- 2015-01-22 CN CN201580007116.0A patent/CN105980304B/en not_active Expired - Fee Related
- 2015-01-22 EP EP15701014.1A patent/EP3102539A1/en not_active Withdrawn
- 2015-01-22 JP JP2016548356A patent/JP6250827B2/en not_active Expired - Fee Related
- 2015-01-23 TW TW104102178A patent/TWI546426B/en not_active IP Right Cessation
Non-Patent Citations (2)
Title |
---|
None * |
See also references of WO2015113894A1 * |
Also Published As
Publication number | Publication date |
---|---|
CN105980304A (en) | 2016-09-28 |
TWI546426B (en) | 2016-08-21 |
KR101895700B1 (en) | 2018-09-05 |
US10150675B2 (en) | 2018-12-11 |
CA2938453C (en) | 2018-01-02 |
JP2017504557A (en) | 2017-02-09 |
CA2938453A1 (en) | 2015-08-06 |
KR20160117589A (en) | 2016-10-10 |
US20170001869A1 (en) | 2017-01-05 |
WO2015113894A1 (en) | 2015-08-06 |
JP6250827B2 (en) | 2017-12-20 |
DE102014201893A1 (en) | 2015-08-06 |
MY176276A (en) | 2020-07-27 |
TW201531602A (en) | 2015-08-16 |
CN105980304B (en) | 2018-02-09 |
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