US3501406A - Method for producing rod-shaped silicon monocrystals with homogeneous antimony doping over the entire rod length - Google Patents

Method for producing rod-shaped silicon monocrystals with homogeneous antimony doping over the entire rod length Download PDF

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Publication number
US3501406A
US3501406A US644638A US3501406DA US3501406A US 3501406 A US3501406 A US 3501406A US 644638 A US644638 A US 644638A US 3501406D A US3501406D A US 3501406DA US 3501406 A US3501406 A US 3501406A
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Prior art keywords
rod
antimony
homogeneous
melt
pressure
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Expired - Lifetime
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US644638A
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English (en)
Inventor
Rudolf Kappelmeyer
Max Hugo Kellerbauer
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Siemens AG
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Siemens AG
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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
    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20—Controlling or regulating

Definitions

  • the present invention relates to a method of producing rod-shaped silicon monocrystals with homogeneous antimony doping over the entire rod length by pulling from a melt.
  • the present invention utilizes a method whereby the monocrystal is pulled by a crystal seed from a melt held in a crucible containing an appropriate amount of antimony. During the growth of the crystal, a portion of the antimony contained in the melt is vapor-deposited at such amounts that the increase in antimony concentration caused by the distribution coefficient is compensated for, by means of vaporization of the antimony.
  • the present method is characterized by the fact that the pulling process is carried out in an evacuable reaction vessel, under a protective atmosphere and at a decreased pressure, whereby the atmosphere is preferably comprised of argon.
  • an argon pressure of about torr (10 mm. Hg) is adjusted in the reaction vessel, after the crystal seed has been dipped into the melt.
  • This pressure during the further course of the 3,501,406 Patented Mar. 17, 1970 pulling process, may either be maintained at the same value, or may be lowered to a pressure of about 3 torr.
  • silicon is preferably first melted in a high vacuum, at pressures of less than 10 torr, and is thereby freed from volatile contaminations.
  • the silicon monocrystals produced in accordance with the present invention, are particularly suitable for the production of carrier crystals for epitactic growth layers. Directly following the coating process, they may be processed into semiconductor components such as transistors, rectifiers and the like, or they may be processed directly into such semiconductor components as transistors, diodes or solid state integrated circuits.
  • a crystal seed 1 is inserted into a holder 2 which is connected to a driving device, not shown.
  • the connection between the holder 2 and the driving device is through an intermediary member 3.
  • the crystal seed 1 together with the monocrystalline silicon rod 4, growing thereon may be rotated around its longitudinal axis and may be pulled, in accordance with the crystal growth, upward from the melt 5 which is contained in quartz vessel 6.
  • the quartz vessel 6 is arranged within graphite vessel 7, which is heated by high-frequency coil 8, positioned outside the reaction vessel 10. The heating action of the highfrequency coil 8 is amplified by the energy concentrator 9.
  • the quartz vessel is heated by a heat transfer from the graphite vessel 7.
  • the temperature of the melt is determined by means of a Pt/Pt-Rh thermoelement 11, which is contained in a protective tube 12 of aluminum oxide or quartz.
  • the thermoelement 11 may be connected to a regulating control circuit, not shown in the figure, to control the energy supply and thereby the melting temperature.
  • the lower seal of the reaction vessel 10 is the bottom plate 13 through which the tubular vessel holder 14 and the rod-shaped holder 15 for the energy concentrator 9 are hermetically led.
  • an inlet nozzle 16 has been provided through which the protective gas, e.g. argon, from a storage vessel 17 is introduced to the reaction vessel 10, via dosing valve 18.
  • a head portion 20 equipped with a cooling jacket is provided as the upper seal for the reaction vessel 10.
  • the inlet and outlet for the cooling water are through openings 21 and 22.
  • the rod holder 2 which is coupled with the connecting piece 3 is hermetically led through the head 20. Seals 23 and 24 are further provided for sealing the reaction vessel.
  • the under-pressure in the reaction vessel is produced by the pumping aggregate consisting of the diffusion pump 25 and the circulating pump 26.
  • the block valve 27 is also installed into the pump line. The pressure is measured by manometer 28 and Penning measuring tube 29.
  • Two modes of operation are particularly suitable for carrying out the method of the present invention.
  • the silicon is first melted at a reduced pressure, for example at 10- torr.
  • the melting temperature is about l400-l450 C.
  • the temperature of the melt is then reduced to the point that the melt remains just about liquid.
  • argon i introduced from the storage vessel into the reaction vessel and the gas pressure is adjusted in the vessel to approximately 500760 torr.
  • the crystal seed is dipped in and melted on, the pulling of the crystal is initiated.
  • the antimony, serving as the doping material is thrown in small pieces, e.g. balls of equal weight, into the silicon melt, prior to or following the dipping in of the crystal seed.
  • the pulling speed is approximately 13 mm./min.
  • the gas pressure in the reaction vessel is adjusted to a value of about torr. This value is either maintained or reduced to approximately 3 torr.
  • the pumping capacity is preferably so adjusted that the flow rate of the gas is at least 3 l./ min.
  • the amount of material to be used depends on the required doping concentration and may be calculated without difficulty from the known distribution coefficients of the employed materials as well as from the vaporization rate of the doping material.
  • a pre-alloying of antimony and silicon is effected. This is then melted at a pressure of about 760 torr. This may be done by putting pure antimony, together with the silicon, into the crucible and melting it. Subsequently, the crystal seed is dipped into said melt and melted on. The crystal pulling is effected in the manner described in the previous example. Temperature and pressure as well as the travelling speed of the gas are adjusted analogously.
  • a method of producing rod-shaped silicon monocrystals having homogeneous antimony doping over the entire rod length, by pulling from a melt which comprises pulling a monocrystal by means of a crystal seed from a melt with an appropriately selected antimony content, contained in a crucible, whereby a portion of the antimony present in the melt is vaporized during the growth of the crystal, said pulling process being carried out in an evacuable reaction vessel in which is a gaseous atmosphere at a pressure under about 10 torr.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
US644638A 1966-06-13 1967-06-08 Method for producing rod-shaped silicon monocrystals with homogeneous antimony doping over the entire rod length Expired - Lifetime US3501406A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DES0104258 1966-06-13

Publications (1)

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US3501406A true US3501406A (en) 1970-03-17

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US644638A Expired - Lifetime US3501406A (en) 1966-06-13 1967-06-08 Method for producing rod-shaped silicon monocrystals with homogeneous antimony doping over the entire rod length

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US (1) US3501406A (de)
AT (1) AT270750B (de)
CH (1) CH503518A (de)
DE (1) DE1544292C3 (de)
GB (1) GB1140656A (de)
NL (1) NL6707642A (de)
SE (1) SE326160B (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3615261A (en) * 1969-04-02 1971-10-26 Motorola Inc Method of producing single semiconductor crystals
US3865554A (en) * 1971-09-23 1975-02-11 Little Inc A Pressure-and temperature-controlled apparatus for large-scale production of crystals by the czochralski technique
US4911896A (en) * 1986-07-24 1990-03-27 General Electric Company Fused quartz member for use in semiconductor manufacture
EP0435440A1 (de) * 1989-11-24 1991-07-03 Shin-Etsu Handotai Company Limited Verfahren zur Züchtung von Antimon-dotierten Silizium-Einkristallen
WO2023051702A1 (zh) * 2021-09-30 2023-04-06 西安奕斯伟材料科技有限公司 一种用于制造掺氮单晶硅的设备及方法

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4789596A (en) * 1987-11-27 1988-12-06 Ethyl Corporation Dopant coated bead-like silicon particles
NO335110B1 (no) * 2011-10-06 2014-09-15 Elkem Solar As Fremgangsmåte for fremstilling av silisiummonokrystall og multikrystalline silisiumingoter

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2981687A (en) * 1958-04-03 1961-04-25 British Thomson Houston Co Ltd Production of mono-crystal semiconductor bodies
US3167512A (en) * 1958-05-21 1965-01-26 Sicmens & Halske Ag Method of controlling the distribution of doping substance in crucible-free zone-melting operations
US3296036A (en) * 1965-03-19 1967-01-03 Siemens Ag Apparatus and method of producing semiconductor rods by pulling the same from a melt

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2981687A (en) * 1958-04-03 1961-04-25 British Thomson Houston Co Ltd Production of mono-crystal semiconductor bodies
US3167512A (en) * 1958-05-21 1965-01-26 Sicmens & Halske Ag Method of controlling the distribution of doping substance in crucible-free zone-melting operations
US3296036A (en) * 1965-03-19 1967-01-03 Siemens Ag Apparatus and method of producing semiconductor rods by pulling the same from a melt

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3615261A (en) * 1969-04-02 1971-10-26 Motorola Inc Method of producing single semiconductor crystals
US3865554A (en) * 1971-09-23 1975-02-11 Little Inc A Pressure-and temperature-controlled apparatus for large-scale production of crystals by the czochralski technique
US4911896A (en) * 1986-07-24 1990-03-27 General Electric Company Fused quartz member for use in semiconductor manufacture
EP0435440A1 (de) * 1989-11-24 1991-07-03 Shin-Etsu Handotai Company Limited Verfahren zur Züchtung von Antimon-dotierten Silizium-Einkristallen
US5423283A (en) * 1989-11-24 1995-06-13 Shin-Etsu Handotai Co., Ltd. Method for growing antimony-doped silicon single crystal
WO2023051702A1 (zh) * 2021-09-30 2023-04-06 西安奕斯伟材料科技有限公司 一种用于制造掺氮单晶硅的设备及方法

Also Published As

Publication number Publication date
DE1544292B2 (de) 1975-05-28
SE326160B (de) 1970-07-20
GB1140656A (en) 1969-01-22
DE1544292A1 (de) 1970-07-02
CH503518A (de) 1971-02-28
AT270750B (de) 1969-05-12
NL6707642A (de) 1967-12-14
DE1544292C3 (de) 1976-01-08

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