EP2945908A1 - Verfahren zur abscheidung von polykristallinem silicium - Google Patents

Verfahren zur abscheidung von polykristallinem silicium

Info

Publication number
EP2945908A1
EP2945908A1 EP14700836.1A EP14700836A EP2945908A1 EP 2945908 A1 EP2945908 A1 EP 2945908A1 EP 14700836 A EP14700836 A EP 14700836A EP 2945908 A1 EP2945908 A1 EP 2945908A1
Authority
EP
European Patent Office
Prior art keywords
reactor
deposition
opened
medium
bell
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Withdrawn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
EP14700836.1A
Other languages
German (de)
English (en)
French (fr)
Inventor
Barbara MÜLLER
Thomas Koch
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
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 Wacker Chemie AG filed Critical Wacker Chemie AG
Publication of EP2945908A1 publication Critical patent/EP2945908A1/de
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • 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
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD

Definitions

  • the invention relates to a method for the deposition of polycrystalline silicon.
  • Polycrystalline silicon serves as
  • Multicrystalline silicon after various drawing and casting processes for the production of solar cells for photovoltaics.
  • Polycrystalline silicon is usually produced in batches in the Siemens process.
  • a silicon-containing reaction gas is thermally decomposed or by hydrogen
  • the silicon-containing component of the reaction gas is usually monosilane or a halosilane of the general
  • Chlorosilane more preferably trichlorosilane.
  • the Siemens process is in a separation reactor
  • the deposition reactor comprises a metallic bottom plate and a coolable bell, which is placed on the bottom plate, so that a reaction space is formed inside the bell.
  • the mostly bell-shaped separation reactor must be gas-tight, because the reaction gases are corrosive act in combination with air for spontaneous combustion, or tend to explode.
  • the bottom plate is provided with one or more feed openings and one or more discharge openings for the gaseous reaction gases and with holders, by means of which the thin rods are held in the reaction space.
  • two adjacent bars are connected at their free, the held foot ends opposite ends by a bridge to a U-shaped support body.
  • the U-shaped support body are by direct current passage on the
  • Polysilicon a shut-off valve for the reaction gas flowing to the reactor and a shut-off valve for the exhaust gas flowing from the reactor to open.
  • the reaction gas flows through a feed opening of the bottom plate into the closed one
  • Deposition reactor There, the deposition of silicon on the heated by direct current passage thin rods. The resulting in the reactor, hot exhaust gas leaves the reactor through a discharge opening in the bottom plate and can
  • the halogen-containing silicon compounds for example trichlorosilane
  • the deposition is stopped and the resulting polysilicon rods cooled to room temperature.
  • Main constituents containing the elements Si, Cl and O comes through halosilane radicals, for example unreacted reaction gas, or in the process formed halosilanes or polysilanes, to form corrosive hydrogen halides, such as hydrogen chloride. These corrosive gases can escape from the separation reactor into the production hall and lead there, for example, to corrosion on pipes, fittings, technical components.
  • the hydrogen halide corrodes reactor components, as well as the supply and discharge into the reactor.
  • Corrosion process cause damage in the form of rusting on steel surfaces at e.g. Components of the separation plants
  • Aluminum and arsenic are introduced in the subsequent deposition, especially at the beginning of deposition, in an increased degree in the deposited silicon and on the Rod surface of Polysiliciumstäben located in the production room are attached.
  • Particularly corroded steel can be used when opening the
  • Inert gas purging for purging a closed reactor during the running process is carried out for inerting or to avoid explosive gas mixtures (oxygen removal).
  • the introduction of inert gas into the reactor as shown in the prior art during the process or after opening the reactor does not solve the problem of venting the bell pad. Also, the problem of impurity entry in the reaction space and on the rod surfaces in the process of reactor opening is not resolved.
  • US 2012/0100302 A1 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 introduced into the reactor containing at least one thin rod is irradiated by UV light, whereby halogen and hydrogen radicals are formed and the forming volatile halides and hydrides are removed from the reactor. This will be the
  • the object of the present invention was to provide the
  • the object is achieved by a method for the deposition of polycrystalline silicon, comprising introducing a
  • the method is characterized in that after completion of the
  • Separation of the reactor is opened for a certain period of time and vented before the rod expansion begins. This period of venting begins with the first opening of the reactor after the deposition of a batch of polycrystalline silicon and includes the period of time after completion of the
  • the diameter of the carrier body increases.
  • the result is an exhaust gas, which is removed by a discharge line from the deposition reactor.
  • the deposition is completed, the carrier body cooled to room temperature, the inner surface of the deposition reactor open to the environment and the carrier body from the deposition reactor
  • Separating reactor is attached.
  • the invention deviates from, from reaching the desired target diameter of the carrier body and completion of the deposition, the
  • the reactor is opened by lifting the reactor bell over the bottom plate.
  • the reactor is opened by a
  • the reactor is opened by opening of flange, Switzerlandas-, exhaust pipes.
  • a medium is fed into the reactor and then discharged again.
  • the supply of the medium via a
  • Sight glass wherein the medium via exhaust ports or a second sight glass is discharged again.
  • the medium is supplied and discharged via the same opening.
  • the supplied medium to air, nitrogen, moisture in each case individually or in combination.
  • the supplied and discharged gases are discharged, from the Abreagieren the bell pad
  • the deposition reactor After completion of the chemical reaction (the deposition), the deposition reactor is opened, so that subsequently the polysilicon rods can be removed from the deposition reactor with little contamination.
  • the inner surface of the deposition reactor is opened under defined conditions.
  • the inner surface of the deposition reactor includes those shown in FIG.
  • Fig. 1 shows a standing on a bottom plate 1
  • the inner surface comprises the surface 3 facing the interior of the reactor.
  • the inner surface of the deposition reactor can be any material.
  • the bell can be lifted from the bottom plate so that a medium for reacting the bell pad can be supplied via the resulting gap.
  • FIG. 2 shows a separation reactor, the bell 2 (shot and hood) is raised when venting from the bottom plate 1.
  • This medium is gaseous and may contain different levels of moisture at a defined temperature.
  • Supports can be installed between the bottom plate and the bell of the separator reactor.
  • the resulting gap used for ventilation and media supply is 0.5% to 15% of the total height of the
  • the period of the process step aeration makes up less than one tenth of the process step deposition
  • Volume flow of the medium is 50 - 2000 m 3 / h and preferably 100 - 500 m 3 / h, more preferably 150 - 300 m 3 / h.
  • Fig. 3 shows possibilities for aerating the deposition apparatus before the batch change, namely via one or more sight glasses 6 or other openings, e.g. Flanges or water-cooled flanges and / or exclusively via the exhaust opening 4.
  • the bell 2 remains on the bottom plate.
  • Suitable media include air, synthetic air, air conditioning air, nitrogen, argon, helium, protective gases, etc.
  • the media used can be preconditioned, for example, by the targeted introduction of moisture. Even a more accurate control of the flow velocity of the incoming and outflowing medium is possible.
  • humidified nitrogen and / or air (also in the form of climate air) is introduced as a medium for aerating the separation plant in the deposition reactor and the reaction of the bell pad over the amount of resulting hydrogen chloride gas monitored by online monitoring and depending on to reach a limit concentration of the process ended.
  • the possible process time to be saved is marked in FIG. 4 with At.
  • the termination of the process to a target size is possible, so that the process step lasts only as long as it is technically necessary.
  • Time At can be saved by using online monitoring in comparison to defining a specific fixed process time.
  • the intended protection includes the process step of aerating the separation plants after completion of the deposition time and before removing the polysilicon rods.

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Physics & Mathematics (AREA)
  • Power Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Chemical Vapour Deposition (AREA)
EP14700836.1A 2013-01-17 2014-01-13 Verfahren zur abscheidung von polykristallinem silicium Withdrawn EP2945908A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102013200660.8A DE102013200660A1 (de) 2013-01-17 2013-01-17 Verfahren zur Abscheidung von polykristallinem Silicium
PCT/EP2014/050437 WO2014111326A1 (de) 2013-01-17 2014-01-13 Verfahren zur abscheidung von polykristallinem silicium

Publications (1)

Publication Number Publication Date
EP2945908A1 true EP2945908A1 (de) 2015-11-25

Family

ID=49998238

Family Applications (1)

Application Number Title Priority Date Filing Date
EP14700836.1A Withdrawn EP2945908A1 (de) 2013-01-17 2014-01-13 Verfahren zur abscheidung von polykristallinem silicium

Country Status (10)

Country Link
US (1) US9620359B2 (zh)
EP (1) EP2945908A1 (zh)
JP (1) JP6046269B2 (zh)
KR (1) KR101731410B1 (zh)
CN (1) CN104918883B (zh)
DE (1) DE102013200660A1 (zh)
MY (1) MY170523A (zh)
SA (1) SA515360699B1 (zh)
TW (1) TWI505988B (zh)
WO (1) WO2014111326A1 (zh)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2808086T3 (es) 2016-02-10 2021-02-25 Yoshino Gypsum Co Aparato de fabricación de panel basado en yeso
CN109562951A (zh) * 2016-12-14 2019-04-02 瓦克化学股份公司 用于制备多晶硅的方法
US11655541B2 (en) * 2018-12-17 2023-05-23 Wacker Chemie Ag Process for producing polycrystalline silicon
CN112203755A (zh) 2019-04-15 2021-01-08 M技术株式会社 搅拌机
JP6601862B1 (ja) 2019-04-15 2019-11-06 エム・テクニック株式会社 攪拌機
JP7217720B2 (ja) * 2020-03-10 2023-02-03 信越化学工業株式会社 ベースプレートの汚染防止方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2105409A1 (en) * 2008-03-28 2009-09-30 Mitsubishi Materials Corporation Polymer inactivation method for polycrystalline silicon manufacturing device

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US3491720A (en) * 1965-07-29 1970-01-27 Monsanto Co Epitaxial deposition reactor
GB1532649A (en) 1974-12-26 1978-11-15 Monsanto Co Production of polycrystalline silicon
JPS56114815A (en) * 1980-02-08 1981-09-09 Koujiyundo Silicon Kk Preliminary washing method of reaction furnace for preparing polycrystalline silicon
DE102006037020A1 (de) 2006-08-08 2008-02-14 Wacker Chemie Ag Verfahren und Vorrichtung zur Herstellung von hochreinem polykristallinem Silicium mit reduziertem Dotierstoffgehalt
EP2150491A4 (en) * 2007-04-25 2011-11-30 Kagan Ceran HIGH-PURITY SILICON DEPOSITION BY GAS-SOLID OR GAS-LIQUID INTERFACES WITH HIGH SPECIFIC AREA AND LIQUID RECOVERY
JP5509578B2 (ja) 2007-11-28 2014-06-04 三菱マテリアル株式会社 多結晶シリコン製造装置及び製造方法
US8399072B2 (en) * 2009-04-24 2013-03-19 Savi Research, Inc. Process for improved chemcial vapor deposition of polysilicon
JP5308288B2 (ja) * 2009-09-14 2013-10-09 信越化学工業株式会社 多結晶シリコン製造用反応炉、多結晶シリコン製造システム、および多結晶シリコンの製造方法
DE102010042869A1 (de) 2010-10-25 2012-04-26 Wacker Chemie Ag Verfahren zur Herstellung von polykristallinen Siliciumstäben
DE102011089449A1 (de) * 2011-12-21 2013-06-27 Wacker Chemie Ag Polykristalliner Siliciumstab und Verfahren zur Herstellung von Polysilicium

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2105409A1 (en) * 2008-03-28 2009-09-30 Mitsubishi Materials Corporation Polymer inactivation method for polycrystalline silicon manufacturing device

Also Published As

Publication number Publication date
MY170523A (en) 2019-08-09
SA515360699B1 (ar) 2018-02-26
WO2014111326A1 (de) 2014-07-24
KR101731410B1 (ko) 2017-04-28
TWI505988B (zh) 2015-11-01
US20150364323A1 (en) 2015-12-17
JP2016506357A (ja) 2016-03-03
KR20150093209A (ko) 2015-08-17
CN104918883B (zh) 2017-06-16
DE102013200660A1 (de) 2014-07-17
TW201429869A (zh) 2014-08-01
US9620359B2 (en) 2017-04-11
CN104918883A (zh) 2015-09-16
JP6046269B2 (ja) 2016-12-14

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