US3124686A - Goorissen - Google Patents

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Publication number
US3124686A
US3124686A US3124686DA US3124686A US 3124686 A US3124686 A US 3124686A US 3124686D A US3124686D A US 3124686DA US 3124686 A US3124686 A US 3124686A
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United States
Prior art keywords
infra
red
enclosure
radiation
semiconductor material
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    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/52—Means for observation of the coating process
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/28—Controlling or regulating
    • C30B13/30—Stabilisation or shape controlling of the molten zone, e.g. by concentrators, by electromagnetic fields; Controlling the section of the crystal
    • 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
    • C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
    • C30B15/26—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal using television detectors; using photo or X-ray detectors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y10T117/1004—Apparatus with means for measuring, testing, or sensing
    • Y10T117/1008—Apparatus with means for measuring, testing, or sensing with responsive control means
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
    • Y10T117/1076—Apparatus for crystallization from liquid or supercritical state having means for producing a moving solid-liquid-solid zone
    • Y10T117/1088—Apparatus for crystallization from liquid or supercritical state having means for producing a moving solid-liquid-solid zone including heating or cooling details

Definitions

  • the enclosure has a wall made at least in part of a transparent material such as vitreous quartz in order to permit observation.
  • the invention utilizes the property of a semi-conductor material that it transmits infra-red radiation over a certain wavelength range in contradistinction to, for example, a metal, so that infra-red radiation of a wavelength within this range is also transmitted by the deposit of the semi-conductor material on the wall.
  • a conventional transparent wall portion of vitreous quartz is also permeable to such radiation.
  • an infra-red image converter is used for observing the material under treatment.
  • the term infra-red image converter as used herein denotes in general a device capable of converting an infra-red radiation image into an ice image of visible light.
  • the image converter may be an infra-red viewer known in the art, as described in Proceedings of the IRE. 47 (1959), No. 5, page 904, or a flat image intensifier sensitive to infrared radiation.
  • a camera tube sensitive to infra-red radiation may be used according to principles known from television, the signal delivered by this tube being converted into a visible image in a display tube.
  • the infra-red image converter must be sensitive to the infra-red radiation transmitted by the semi-conductor material concerned.
  • the wavelength range of the transmitted radiation is bounded at the short wave end by an absorption boundary of the semi-conductor material which is related to the energy spacing, hereinafter referred to as the band spacing, between the valency band and the conduction band of the semi-conductor material and which is situated at a smaller wavelength according as the band spacing is larger.
  • the heated semi-conductor material itself may serve as the source of infra-red radiation, however, this material may alternatively be irradiated by infra-red radiation.
  • an infra-red image converter may have further advantages, for example when mists occur during the treatment which disperseinfra-red radiation in a materially smaller degree and, if they consist of semi-conductor material, absorb this radiation to a lesser extent than visible radiation. Furthermore, when a layer of semi-conductor material is deposited on a support, the thickness of the layer can be determined during the deposition by means of interference of reflected infra-red radiation and this generally is not possible with visible radiation due to the frequently high absorptive power of the semi-conductor material for visible light.
  • infra-red image converter Although observation by means of an infra-red image converter generally will be satisfactory when using a conventional wall portion of vitreous quartz, use may also be made of wall portions made from other material transmitting infra-red radiation, for example portions consisting of infra-red transmitting glasses or a window made of the same material or of another semi-conductor material having a band spacing equal to or greater than that of the material to be treated.
  • reference numeral 1 denotes a vertical tube of vitreous quartz in which a vertical rod 2 of silicon is arranged.
  • This rod comprises two solid portions 3 and 4 secured at their upper and lower ends respectively in holders (not shown) and an intermediate substantially drop-shaped molten zone 5 heated by means of a high-frequency coil 6. Due to the high surface tension of the melt the molten zone 5 is held in place between the two rod portions 3 and 4-.
  • the vitreous quartz tube 1 and the rod 2 are gradually lowered vertically by means (not shown) in the direction indicated by an arrow, whereas the coil 6 does not change position so that the molten zone 5 passes through the silicon rod 2, the rod portion 3 gradually melting on at its lower end and the rod portion 4 gradually growing at its upper end.
  • the shape and the length of the molten zone 5 and the diameter or" the growing rod portion 4 can be controlled by adjusting the strength of the current in the high-frequency coil, which current is provided by a highfrequency generator (not shown). Owing to the high temperature of the melt, part of the silicon will evaporate from the zone 5 and be partly deposited as an opaque coating 7 on the inside of the vitreous quartz tube 1 so that observation of the zone with the naked eye is impeded.
  • the apparatus also includes an infra-red image converter shown diagrammatically in the drawing as an infra-red viewer 3 comprising a concentrating lens or lens system for infra-red radiation 9 and a vacuum tube ltl consisting of a photo-cathode 11 which is sensitive to infra-red radiation of a wavelength exceeding 1.1 the absorption boundary of silicon, a set of electrodes (not shown) and a cathodoluminescent screen 12.
  • the heated molten zone 5 emits infrared radiation of which the part having wavelengths exceeding 1.1 passes substantially unimpeded through the silicon layer 7 deposited on the inner wall of the vitreous-quartz tube l and can be collected by the infrared viewer 8.
  • An infra-red image of the molten zone 5 is projected onto the photo-cathode 11 by means of the lens or lens system 9.
  • the electrons emitted by the photo-cathode 11 are projected with the aid of the electrodes (not shown) provided in the tube onto the screen 12 so that a visible image of the molten zone 5 is produced on this screen.
  • the observer 13 is enabled to follow the zone-melting process without the use of a crucible and, if required, to control this process, for example by varying the high-frequency current supplied to the coil by the generator, without being impeded by the silicon deposit 7 on the vitreous quartz tube 1.
  • rod portions 3 and 4 are irradiated by infrared radiation, they can also be observed by means of the image converter. It has been found that generally normal daylight contains a sufiicient amount of infra-red radiation for this purpose.
  • an infra-red image converter can also be used in heat treatments of other semi-conductor materials and in further heat treatments, for example zone melting in a crucible, drawing crystals from the melt, deposition of semi-conductor material by sublimation or decomposition of volatile compounds, etc. without departing from the scope of the present invention.
  • a method of treating semiconductor material within an enclosure containing a portion substantially transparent to infra-red radiation and controlling the said treatment comprising the steps of heating the semiconductor material as part of the treatment under conditions at which semiconductor vapors are formed that condense on the substantially transparent enclosure portion forming a layer that is substantially opaque to visible radiation but substantially transparent to infra-red radiation, and utilizing an infra-red image converter located outside the enclosure for detecting through the said substantially transparent enclosure portion and layer an infra-red image of the heated semiconductor material and for converting that infra-red image into a visible image of the heated semiconductor material which can be observed for the purpose of controlling the treatment of the material.
  • a method of zone-melting silicon semiconductor material within an enclosure containing a low-pressure protective atmosphere and including a wall portion substantially transparent to infra-red radiation and controlling the said treatment comprising the steps of heating and melting the semiconductor material as part of the treatrnent whereby vapors of the material are formed within the enclosure that deposit on the said wall portion forming a layer that is substantially opaque to visible radiation but substantially transparent to infra-red radiation, and utilizing an infra-red image converter located outside the enclosure for detecting through the said substantially transparent wallportion and layer an infra-red image of the heated semiconductor material and for converting that infra-red image into a visible image of the heated semiconductor material which can be observed for the purpose of controlling the treatment of the material.
  • Apparatus for heat treatment of a semiconductor material and for controlling that treatment comprising an enclosure in which the semiconductor material is located, said enclosure containing a portion substantially transparent to infra-red radiation, means for controlling the atmosphere within the enclosure, means for heating the semiconductor material while in the enclosure under conditions at which an infra-red image of the heated semiconductor material is generated and vapors are formed that condense on the substantially-transparent enclosure portion forming a layer that is substantially opaque to visible radiation but substantially transparent to infra-red radiation, and means located outside the enclosure but adjacent the said substantially transparent portion for detecting the said infra-red image therethrough and for converting the said infra-red image into a visible imagewhich can be observed for the purpose of controlling the treatment of the material.
  • Apparatus for zone-melting of silicon semiconductor material and for controlling it comprising an enclosure in which the semiconductor material is located, said enclosure being of a material substantially transparent to infra-red radiation, means for providing a low pressure protective atmosphere withinv the enclosure, means for heating the semiconductor material while in the enclosure to a temperature at which the material melts and vapors of the material are formed which deposit on the enclosure walls forming a layer opaque to visible radiation but transparent to infra-red radiation and under the conditions at which an infra-red image of the heated semiconductor material is generated, and means located outside the enclosure but adjacent thereto for detecting the said infra-red image therethrough and for converting the said infra-red image into a visible image which can be observed for the purpose of controlling the zonemelting of the material.

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Electromagnetism (AREA)
  • Thermal Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
US3124686D 1959-09-24 Goorissen Expired - Lifetime US3124686A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
NL243734A NL108788C (de) 1959-09-24 1959-09-24

Publications (1)

Publication Number Publication Date
US3124686A true US3124686A (en) 1964-03-10

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ID=19751951

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US3124686D Expired - Lifetime US3124686A (en) 1959-09-24 Goorissen

Country Status (5)

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US (1) US3124686A (de)
DE (1) DE1146722B (de)
FR (1) FR1268179A (de)
GB (1) GB932668A (de)
NL (1) NL108788C (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3384732A (en) * 1964-01-08 1968-05-21 Taylor Winfield Corp Induction annealing of strip joints

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2054382A (en) * 1935-07-16 1936-09-15 United States Steel Corp Radiation pyrometer device
US2166824A (en) * 1936-01-14 1939-07-18 Gen Electric High temperature pyrometer
US2234328A (en) * 1937-09-24 1941-03-11 Rca Corp Radiant energy receiving device
US2591561A (en) * 1943-04-28 1952-04-01 Elgin Nat Watch Co Apparatus for producing refractory rods
US2692950A (en) * 1952-01-04 1954-10-26 Bell Telephone Labor Inc Valve for infrared energy
US2870309A (en) * 1957-06-11 1959-01-20 Emil R Capita Zone purification device
US2916593A (en) * 1958-07-25 1959-12-08 Gen Electric Induction heating apparatus and its use in silicon production
US2982856A (en) * 1955-06-27 1961-05-02 Rca Corp Tunable infrared apparatus and methods
US2997590A (en) * 1959-06-26 1961-08-22 Ibm Infrared radiation entrance window
US3031576A (en) * 1957-11-06 1962-04-24 Philips Corp Device for measuring and detecting radiations

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2054382A (en) * 1935-07-16 1936-09-15 United States Steel Corp Radiation pyrometer device
US2166824A (en) * 1936-01-14 1939-07-18 Gen Electric High temperature pyrometer
US2234328A (en) * 1937-09-24 1941-03-11 Rca Corp Radiant energy receiving device
US2591561A (en) * 1943-04-28 1952-04-01 Elgin Nat Watch Co Apparatus for producing refractory rods
US2692950A (en) * 1952-01-04 1954-10-26 Bell Telephone Labor Inc Valve for infrared energy
US2982856A (en) * 1955-06-27 1961-05-02 Rca Corp Tunable infrared apparatus and methods
US2870309A (en) * 1957-06-11 1959-01-20 Emil R Capita Zone purification device
US3031576A (en) * 1957-11-06 1962-04-24 Philips Corp Device for measuring and detecting radiations
US2916593A (en) * 1958-07-25 1959-12-08 Gen Electric Induction heating apparatus and its use in silicon production
US2997590A (en) * 1959-06-26 1961-08-22 Ibm Infrared radiation entrance window

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3384732A (en) * 1964-01-08 1968-05-21 Taylor Winfield Corp Induction annealing of strip joints

Also Published As

Publication number Publication date
NL108788C (de) 1964-04-15
GB932668A (en) 1963-07-31
DE1146722B (de) 1963-04-04
FR1268179A (fr) 1961-07-28

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