US3820935A - Method and device for the production of tubular members of silicon - Google Patents

Method and device for the production of tubular members of silicon Download PDF

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Publication number
US3820935A
US3820935A US00291787A US29178772A US3820935A US 3820935 A US3820935 A US 3820935A US 00291787 A US00291787 A US 00291787A US 29178772 A US29178772 A US 29178772A US 3820935 A US3820935 A US 3820935A
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United States
Prior art keywords
carriers
electrodes
tubular
connecting bridge
supporting
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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.)
Expired - Lifetime
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US00291787A
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English (en)
Inventor
W Dietze
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Siemens AG
Siemens Corp
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Siemens Corp
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Publication date
Priority claimed from DE2149526A external-priority patent/DE2149526C3/de
Application filed by Siemens Corp filed Critical Siemens Corp
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • 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
    • C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
    • 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
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape

Definitions

  • ABSTRACT A method and device for the production of silicon tubes by deposition of self-supporting silicon layers from the gas-phase onto tubular heated carriers of graphite whereby two such vertical carriers are supported along the periphery of their lower ends by electrodes and are connected at their upper ends by a bridge of conductive material, whereby the tubular shaped carriers, as well as the supporting electrodes and the connecting bridge are so designed with respect to each other that the respective values for the 7 product of the shortest circumference with the smallest current carrying cross-section and the specific conductivity for the electrodes and connecting bridge are at least five times, preferably ten times as large as the values of such products for the tubular carriers, and stopping the production of such layers when the temi perature differential between the tubular carriers and the supporting elements, i.e., electrodes and connecting bridge, drops to 300C.
  • the invention is directed to a method and device for the production of tubular members of silicon by the de-' position of self-supporting silicon layers from the gasphase upon tubular heated carriers formed, for example, of graphite, from which the silicon layers comprising the desired tubes may be removed.
  • Such device may comprise a pair of parallel carriers, supported in vertical positions by respective electrodes which contact the carriers along the peripheries thereof at their lower ends, with the upper ends of the carriers being connected by a bridge member of conductive material.
  • the reaction container is provided with means for supplying a flowing reaction gas comprising a halogenized silane and hydrogen, as well as an outlet for the exhaust gases, with the two electrodes supporting the respective carriers being adapted to be conductively connected to opposite sides of a suitable current source, which may be either a direct current source or a low frequency alternating current source.
  • a suitable current source which may be either a direct current source or a low frequency alternating current source.
  • U.S. Pat. application No. 1 13,286, now U.S. Pat. No. 3,746,496, generally illustrates a device of this type and the present application is directed to an improvement of such type of device.
  • the tubular carriers, as well as the supporting electrodes and connecting bridge therefore, are so designed that the product of the shortest circumference with the smallest current-conducting cross section and the specific conductivity of the material of the electrodes and connecting bridge are at least five times, preferably at least ten times greater than that of the tubular carriers.
  • such components consist of highly pure conductive carbon, particularly graphite, and in this event, the operational current should be initiated only if the reaction chamber is filled with an inert gas or hydrogen to prevent burning of such components.
  • an alternating current source it should have a sufficiently low frequency that the supplied current has no noticeable skin-effect with respect to the tubular carriers or the electrodes and the connecting bridge. This is generally the case when alternating current from an interconnection is involved.
  • the temperature at the surface of the tubular carriers Upon passage of the operational current, the temperature at the surface of the tubular carriers automatically increases by at least 300C over the surface temperatures of the electrodes and the connecting bridge. Consequently, if a mixture of halogenized silane (especially FiCl FiHClor the corresponding bromine compounds) and hydrogen are employed as the reaction gas, the temperature at the surface of the tubular carriers should be adjusted to not more than l,250C whereby the temperature at the connecting bridge and at the electrodes will be so low that a deposition at the surface of these components cannot occur.
  • halogenized silane especially FiCl FiHClor the corresponding bromine compounds
  • FIGURE illustrates a vertical section through a device constructed in accordance with the present invention.
  • the reference numeral 1 designates a base member or plate, of quartz or other heat-resistant metal or material, which is hermetically connected with a dome-shaped member 2, in effect forming a bell jar which may, for example, be constructed of quartz.
  • a base member or plate of quartz or other heat-resistant metal or material, which is hermetically connected with a dome-shaped member 2, in effect forming a bell jar which may, for example, be constructed of quartz.
  • two vertically extending tubular carriers 3 Disposed in the chamber thus formed are two vertically extending tubular carriers 3 which have their lower end inserted into respective bores 4, formed in supporting electrodes 5, with the electrodes being conductively connected with feed lines 1 1, extending through the base plate 1 in insulated relation with respect thereto and thus with respect to each other.
  • the tubular carriers 3 are connected at their upper ends by a conductive bridge member 6, preferably constructed of the same material as the carriers 3, with the upper ends of the latter being disposed in respective bores 7 formed in the bridge 6.
  • the bores 4 and 7 are each slightly tapered inwardly whereby the side walls of the bores 4 taper downwardly when thoseof the bores 7 taper upwardly.
  • the interior of the tubes 3 may, by means of the bores 7, be open to the reaction chamber, and by disposing the open end of each respective supply line 8 adjacent the outer ends of the respective bores 4 in the electrodes 5, the gas entering the device may flow through the in terior of the carriers 3, to provide a cooling action on the interior surfaces of the latter.
  • the cooling gas may, in this case, be one participating directly in the reducing reaction, or in the form of an inert gas, for example, argon or nitrogen which thus may also function as a diluting medium for the active component of the reaction gas.
  • the reaction gas may consist, for example, of a halogenized in particular chlorinated, silane (for example SiHCl or SiCl and hydrogen.
  • silane for example SiHCl or SiCl and hydrogen.
  • Such gas may enter through a feed line 9 located in the bottom 1 of the reaction chamber, and in the example illustrated, an exhaust tube 10 for the exhausted gas is disposed concen trically to the supply tube 9, the latter however, extending a greater distance into the chamber than the exhaust outlet 10, with both being located between the two tubular carriers 3.
  • the tubular carrier as well as the carrier-supporting electrodes and the connecting bridge are so designed with respect to one another, that the value of the product of the shortest circumference with the smallest current-conducting cross section and the specific conductivity of the electrodes and the connecting bridge are at least 5 times, preferably ten times as large as the value of the corresponding product for the tubular carriers.
  • such parts are constructed of highly pure conductive carbon, particularly graphite, in which case the operational current should be initiated only if the reaction chamber is filled with an inert gas or hydrogen to prevent the burning of such components.
  • an alternating current source it should have a sufficiently low frequency that the supplied alternating current has no noticeable skin-effect in the tubular carriers, electrodes or connecting bridge.
  • the temperature at the tubular carriers is adjusted to not more than 1,250C so that at all times the temperature at the connecting bridge and at the electrodes is so low that a de position on the surface of such components cannot occur.
  • the tubular carriers will be cylindrical or prismatic in which case the circumference of each horizontal cross-section equals the shortest circumference whose value is to be included in the above defined product. This likewise applies to the electrodes 5.
  • the shortest circumference of the connecting bridge will be determined by a comparison of the circumference or peripheries of the cross-sections which extend vertically to the connecting line of the upper ends of the two tubular carriers. In most cases the smallest circumference simultaneously constitutes the circumference of the smallest current-carrying crosssection.
  • the cross-sectional area of the smallest current-carrying cross-section, as well as the tubular carriers, electrodes and connecting bridge are also incorporated in the above mentioned product. In the event that all of these components are constructed from the same material, differences in conductivity of the various arts do not have to be taken into consideration.
  • the connecting bridge and the electrodes have more or less stud-like projections at the connecting points for the tubular carriers, which after assembly of the latter extend somewhat into the interior of the tubular carriers and thus come in contact with the inner walls thereof.
  • This construction results in a lesser heating of the ends of the tubular carriers, and deposition of silicon is thus avoided at these points. This likewise results in an improvement in separating the tubular layers from the carriers following the depositions.
  • the wall thickness of the tubular carriers 3 is, for example 3 mm while the minimum wall thickness of the electrodes 5, as well as that of the connecting bridge 6 are 20 mm,- so that upon adjustment of the temperature at the surface of the tubular carriers to l,200C, the temperature at the surfaces of the connecting bridge and the electrodes will not exceed 800C, whereby deposition will not take place thereon.
  • the bridge 6 is in the form of a relatively massive member in which the crosssection thereof may be considered the wall thickness.
  • such current-conductive connecting bridge is provided with a hollow interior forming a connecting chamber for inert gas whereby the same may flow from one carrier, through the chamber into the other carrier, thus further reducing the temperature of the bridge.
  • the deposited silicon layers can be readily separated from the tubular carriers irrespective of whether the deposition was effected on the external or internal walls of the carrier.
  • a device for the production of tubular members of silicon by deposition of self-supporting silicon layers from the gas phase upon heated tubular carriers from which the silicon layers forming the desired tubes are removed comprising a reaction vessel in which are disposed a pair of parallel tubular carriers supported in vertical position by electrodes which contact the carriers along their periphery at their lower ends, a bridge of conductive material connecting said carriers at their upper ends, means in the reaction container for supplying thereto a reaction gas flow comprising halogenized silane and hydrogen, and means forming a discharge for exhausted gas, the two electrodes supporting the carriers being adapted to be conductively connected to opposite sides of a current supply source, the values of the products of the shortest circumference with the smallest current conducting cross-section and the specific conductivity of the connecting electrodes and connecting bridge respectively being at least five times,
  • tubular carriers, connecting bridge and electrodes supporting the carriers are constructed of conductive carbon.
  • tubular carriers connecting bridge and electrodes are constructed of highly pure graphite.

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Chemical Vapour Deposition (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
US00291787A 1971-10-04 1972-09-25 Method and device for the production of tubular members of silicon Expired - Lifetime US3820935A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE2149526A DE2149526C3 (de) 1970-10-12 1971-10-04 Vorrichtung zum Herstellen von Rohren aus Silicium

Publications (1)

Publication Number Publication Date
US3820935A true US3820935A (en) 1974-06-28

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US00291787A Expired - Lifetime US3820935A (en) 1971-10-04 1972-09-25 Method and device for the production of tubular members of silicon

Country Status (6)

Country Link
US (1) US3820935A (OSRAM)
JP (1) JPS4844159A (OSRAM)
CS (1) CS188126B4 (OSRAM)
DD (1) DD99550A5 (OSRAM)
DK (1) DK145064C (OSRAM)
IT (1) IT1012045B (OSRAM)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4023520A (en) * 1975-04-28 1977-05-17 Siemens Aktiengesellschaft Reaction container for deposition of elemental silicon
US5233163A (en) * 1990-07-05 1993-08-03 Fujitsu Limited Graphite columnar heating body for semiconductor wafer heating
US20070248521A1 (en) * 2006-04-13 2007-10-25 Cabot Corporation Production of silicon through a closed-loop process
US20090165704A1 (en) * 2007-12-28 2009-07-02 Mitsubishi Materials Corporation Silicon seed rod assembly of polycrystalline silicon, method of forming the same, polycrystalline silicon producing apparatus, and method of producing polycrystalline silicon
CN103158200A (zh) * 2011-12-09 2013-06-19 洛阳金诺机械工程有限公司 一种c形硅芯的搭接方法
CN103158201A (zh) * 2011-12-09 2013-06-19 洛阳金诺机械工程有限公司 一种空心硅芯与实心硅芯的搭接方法
CN103158202A (zh) * 2011-12-09 2013-06-19 洛阳金诺机械工程有限公司 一种空心硅芯的搭接方法
CN101392408B (zh) * 2007-09-20 2014-03-05 三菱麻铁里亚尔株式会社 多晶硅反应炉和多晶硅的制备方法
US10100439B2 (en) 2015-05-08 2018-10-16 Sunpower Corporation High throughput chemical vapor deposition electrode

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9683286B2 (en) * 2006-04-28 2017-06-20 Gtat Corporation Increased polysilicon deposition in a CVD reactor
KR101064176B1 (ko) * 2009-01-15 2011-09-15 주식회사수성기술 다결정 실리콘 로드 제조용 시드 필라멘트

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4023520A (en) * 1975-04-28 1977-05-17 Siemens Aktiengesellschaft Reaction container for deposition of elemental silicon
US5233163A (en) * 1990-07-05 1993-08-03 Fujitsu Limited Graphite columnar heating body for semiconductor wafer heating
US7780938B2 (en) 2006-04-13 2010-08-24 Cabot Corporation Production of silicon through a closed-loop process
US20070248521A1 (en) * 2006-04-13 2007-10-25 Cabot Corporation Production of silicon through a closed-loop process
CN101392408B (zh) * 2007-09-20 2014-03-05 三菱麻铁里亚尔株式会社 多晶硅反应炉和多晶硅的制备方法
US20090165704A1 (en) * 2007-12-28 2009-07-02 Mitsubishi Materials Corporation Silicon seed rod assembly of polycrystalline silicon, method of forming the same, polycrystalline silicon producing apparatus, and method of producing polycrystalline silicon
EP2075233A3 (en) * 2007-12-28 2009-07-29 Mitsubishi Materials Corporation Silicon seed rod assembly of polycrystalline silicon, method of forming the same, polycrystalline silicon producing apparatus, and method of producing polycrystalline silicon
US9090962B2 (en) 2007-12-28 2015-07-28 Mitsubishi Materials Corporation Silicon seed rod assembly of polycrystalline silicon, method of forming the same, polycrystalline silicon producing apparatus, and method of producing polycrystalline silicon
CN103158200A (zh) * 2011-12-09 2013-06-19 洛阳金诺机械工程有限公司 一种c形硅芯的搭接方法
CN103158201A (zh) * 2011-12-09 2013-06-19 洛阳金诺机械工程有限公司 一种空心硅芯与实心硅芯的搭接方法
CN103158202A (zh) * 2011-12-09 2013-06-19 洛阳金诺机械工程有限公司 一种空心硅芯的搭接方法
CN103158201B (zh) * 2011-12-09 2016-03-02 洛阳金诺机械工程有限公司 一种空心硅芯与实心硅芯的搭接方法
CN103158202B (zh) * 2011-12-09 2016-07-06 洛阳金诺机械工程有限公司 一种空心硅芯的搭接方法
CN103158200B (zh) * 2011-12-09 2016-07-06 洛阳金诺机械工程有限公司 一种c形硅芯的搭接方法
US10100439B2 (en) 2015-05-08 2018-10-16 Sunpower Corporation High throughput chemical vapor deposition electrode

Also Published As

Publication number Publication date
IT1012045B (it) 1977-03-10
JPS4844159A (OSRAM) 1973-06-25
DK145064C (da) 1983-01-24
CS188126B4 (en) 1979-02-28
DD99550A5 (OSRAM) 1973-08-12
DK145064B (da) 1982-08-16

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