US3591347A - Encapsulating a seed crystal for producing monocrystals - Google Patents

Encapsulating a seed crystal for producing monocrystals Download PDF

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Publication number
US3591347A
US3591347A US752651A US3591347DA US3591347A US 3591347 A US3591347 A US 3591347A US 752651 A US752651 A US 752651A US 3591347D A US3591347D A US 3591347DA US 3591347 A US3591347 A US 3591347A
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US
United States
Prior art keywords
seed crystal
melt
crystal
monocrystals
gallium arsenide
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Expired - Lifetime
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US752651A
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English (en)
Inventor
Josef Grabmaier
Barbara Christa Watson
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Siemens AG
Siemens Corp
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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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/36—Single-crystal growth by pulling from a melt, e.g. Czochralski method characterised by the seed, e.g. its crystallographic orientation
    • 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
    • C30B27/00—Single-crystal growth under a protective fluid
    • C30B27/02—Single-crystal growth under a protective fluid by pulling from a melt
    • 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
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S148/00—Metal treatment
    • Y10S148/107—Melt
    • 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
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S148/00—Metal treatment
    • Y10S148/119—Phosphides of gallium or indium

Definitions

  • the seed crystal according to the invention to prevent the evaporation of the more volatile component of the semiconducting compound therefrom, is encased, prior to being installed into the pulling device, with a thin film of B 0
  • Our invention relates to a method of producing monocrystals, preferably gallium arsenide monocrystals, from semiconducting compounds which dissociate at their melting point.
  • the semiconductor material is melted in a crucible, totally encapsulated by a thin layer of boron oxide (B 0 and is pulled from the semiconductor melt using a seed crystal in accordance with the Czochralski method to yield a monocrystal.
  • the semiconductor compounds for example the A B compounds, supplement and enlarge the number of semiconductor materials available over semiconductor materials such as germanium and silicon.
  • Another possibility for producing compounds which easily dissociate at the melting point is to employ sub-stoichiometric conditions of the components, meaning that, as in the first-described method, a bottom body is employed whereby the melt is not quite stoichiometric, but that, for example, during the production of gallium arsenide the gallium is present, for example in several percent excess.
  • the same problems which occur during the production of semiconducting compounds also occur during their monocrystalline growth.
  • the aforementioned methods are appropriately modified.
  • the starting point for monocrystalline growth for semiconducting compounds is the Czochralski method, particularly in connection with producing gallium arsenide.
  • the difficulty consists in keeping all sides of a completely sealed chamber at a high temperature. In the interior of said chamber the seed is to be 359L347 Patented July 6, 1971 moved.
  • the easily volatile component of the compound, such as arsenic in gallium arsenide unless special precautions are utilized, evaporates from the melt and precipitates at the cold places of the melting vessel.
  • This evaporation may be prevented by melting the compound in a sealed vessel and by maintaining all surfaces which are adjacent to the vaporization chamber, at a temperature above the condensation or sublimation temperature of the more easily volatile component.
  • the pulling of the crystal is made more difficult since the pulling movement must now be transmitted into the sealed vessel, while all parts of the vessel are kept at a relatively high temperature.
  • the problem can be solved by using a magnetic system which allows moving the seed. Even employing these quite complicated technical processes, one still cannot prevent the formation of a thick coating of the semiconducting compound on the inside surface of the quartz vessel. During melting processes of longer duration, this coating results in a considerable impairment of permeability (transparency).
  • gallium arsenide crystals are free of heavy metal and are, therefore, particularly suitable for specific semiconductor devices, such as gallium arsenide diodes used for very high frequencies, that is the so-called Gunn diodes.
  • a semiconductor material e.g.
  • the evaporation of the more volatile component of the semiconducting compound from the seed crystal is prevented by encasing the seed crystal, prior to its installation into the crystal pulling device, with a thin film, in the order of 500 ,um., of B 0
  • this is preferably elfected by immersing the seed crystal into a B 0 melt, heated to approximately 1000 C., for at least about five minutes. The immersed crystal subsequently is pulled from the B 0 melt with a velocity of approximately 10 centimeters/hour.
  • the layer thickness of B 0 is preferably 250 p.111.
  • the seed crystal encapsulated with the B 0 film is tempered immediately following the immersing process, for about five hours, at a temperature between 400 and 800 C.
  • both the immersion process and the tempering process be carried out in a protective gas atmosphere, preferably in an argon atmosphere.
  • our invention is particularly suitable for the production of monoerystals comprised of gallium arsenide, which can be further processed for highest frequency use as, for example, Gunn diodes.
  • the drawing shows a seed crystal produced in accordance with the invention.
  • the seed crystal results from the simple immersion of a gallium arsenide crystal 1, suspended by a high melting metal wire, into an anhydrous B 0 melt heated to about 1000 C., and a slow pulling of the crystal from the melt (about cm./hr.) after an immersion of about five minutes.
  • the crystal becomes immediately surrounded With a mirror-smooth, transparent and clear B 0 layer 2 of approximately 250 am. thickness which completely prevents the evaporation of the easily volatile component and makes the crystal seed usable for any desired number of pulling processes.
  • the encased crystal Prior to its first use, the encased crystal is suspended above the hot melt, in a temperature range between 400 and 800 C. and preferably in an argon atmosphere, for about five hours. This results in a better adherence of the B 0 layer.
  • B 0 boron oxide

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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)
US752651A 1967-08-16 1968-08-14 Encapsulating a seed crystal for producing monocrystals Expired - Lifetime US3591347A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DES0111369 1967-08-16

Publications (1)

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US3591347A true US3591347A (en) 1971-07-06

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US752651A Expired - Lifetime US3591347A (en) 1967-08-16 1968-08-14 Encapsulating a seed crystal for producing monocrystals

Country Status (4)

Country Link
US (1) US3591347A (enrdf_load_stackoverflow)
FR (1) FR1582612A (enrdf_load_stackoverflow)
GB (1) GB1202113A (enrdf_load_stackoverflow)
NL (1) NL6810036A (enrdf_load_stackoverflow)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3853596A (en) * 1971-07-07 1974-12-10 G Distler Method of growing a single-crystal on a single-crystal seed
US4265661A (en) * 1978-10-25 1981-05-05 Cambridge Analyzing Instruments Ltd. Direct synthesis of intermetallic compounds
US4277303A (en) * 1978-08-07 1981-07-07 The Harshaw Chemical Company Getter for melt-grown scintillator ingot and method for growing the ingot

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4289570A (en) * 1978-12-13 1981-09-15 United Technologies Corporation Seed and method for epitaxial solidification

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3853596A (en) * 1971-07-07 1974-12-10 G Distler Method of growing a single-crystal on a single-crystal seed
US4277303A (en) * 1978-08-07 1981-07-07 The Harshaw Chemical Company Getter for melt-grown scintillator ingot and method for growing the ingot
US4265661A (en) * 1978-10-25 1981-05-05 Cambridge Analyzing Instruments Ltd. Direct synthesis of intermetallic compounds

Also Published As

Publication number Publication date
NL6810036A (enrdf_load_stackoverflow) 1969-02-18
FR1582612A (enrdf_load_stackoverflow) 1969-10-03
DE1644015B2 (de) 1975-11-27
DE1644015A1 (de) 1970-04-09
GB1202113A (en) 1970-08-12

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