US3341360A - Method of precipitating crystalline layers of highly pure, brittle materials - Google Patents

Method of precipitating crystalline layers of highly pure, brittle materials Download PDF

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US3341360A
US3341360A US302810A US30281063A US3341360A US 3341360 A US3341360 A US 3341360A US 302810 A US302810 A US 302810A US 30281063 A US30281063 A US 30281063A US 3341360 A US3341360 A US 3341360A
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vapor
carrier
vessel
precipitation
precipitated
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US302810A
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English (en)
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Nickl Julius
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Siemens and Halske 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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • 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
    • C23C14/24—Vacuum evaporation
    • 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
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P95/00—Generic processes or apparatus for manufacture or treatments not covered by the other groups of this subclass
    • 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
    • Y10S148/065—Gp III-V generic compounds-processing
    • 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
    • Y10S148/104—Mask, movable
    • 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
    • Y10S148/169—Vacuum deposition, e.g. including molecular beam epitaxy
    • 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
    • Y10S438/00—Semiconductor device manufacturing: process
    • Y10S438/935—Gas flow control

Definitions

  • United States Patent s 341 360 METHOD OF PRlfCIP ITATING CRYSTAL- LINE LAYERS or HIGHLY PURE, BRIT- My invention relates to a method of producing thin and highly pure crystalline layers of brittle materials, the term brittle being applied to materials which on account of a rigid crystal structure-having a lattice energy in the order of magnitude of about 200 kcal./moleare distinguished due to a slight mobility of their atoms under normal temperature conditions.
  • this group of substances for example are silicon, germanium, carbon, boron, and A B semiconductor compounds such as gallium arsenide. Since atoms are only slowly built into the crystal lattice due to the slight mobility, it is diflicult to obtain thin monocrystalline layers from such materials.
  • the precipitating material forms a thin layer upon the carrier which is of monocrystalline constitution and which no longer exhibits a tendency to scale 01f.
  • the layer thicknesses thus obtainable are in the order of magnitude of several powers of microns, for example 0.1 to 100 microns.
  • Vaporization of the brittle material is elfected in a precipitation vessel under reduced pressure, for example by heating a rod of the material to be vaporized at one end until a melt is produced.
  • the heating of the rod is preferably effected by means of a high-frequency induction coil.
  • the carrier In order to direct the vapor onto the carrier, it is of advantage to mount one or more diaphragms, preferably of molybdenum or quartz glass, between the vapor source and the carrier, so that the jet of vapor is directed through the openings of the diaphragm onto the carrier surface which is to be coated with a layer of the condensing material.
  • one or more diaphragms preferably of molybdenum or quartz glass
  • the temperature of the vapor source for this process is chosen so that it corresponds to a partial pressure of 1 mm. Hg at most of the material to be vapor-deposited. In other words, the vapor-deposition process is performed under relatively high negative pressure.
  • the partial pressures of the gaseous addition substances that are also present in the precipitation vessel are in a range of 10- to 10- mm. Hg, preferably in the range of 10- to 10* mm. Hg, and these gaseous addition substances are preferablyalso produced by vaporizing or boiling.
  • the control or regulation of the total pressure obtaining in the precipitation vessel is preferably effected by means of a vacuum pump or simply with the aid of a cooling trap.
  • a monocrystalline material of the same or similar lattice type as the one being precipitated is preferably used as carrier for the precipitating layers.
  • an inert carrier material preferably quartz glass, may also be employed.
  • the carrier is heated to a temperature promoting the crystallization of the vapor-deposited material, for example to a few hundred degrees C., this temperature not being critical.
  • a crystallizing method of this invention in the favorable for crystallization of the precipitated material, for example at a temperature of several hundred degrees centigrade, such as 200 to 900 C.
  • the melt 2 which constitutes the source of the silicon vapor, and the carrier 7 are two diaphragms 5 and 6 of heatresistant material, preferably quartz glass or molybdenum.
  • the diaphragm openings are aligned in such position that the evaporating material is directed in the shape of a limited vapor jet upon the carrier, thus preventing a vapor-deposition in the remaining processing space.
  • the precipitation vessel is formed with a downward continuation or extension 9 which receives a suitable halogen compound 20, such as silicon tetrachloride.
  • a suitable halogen compound 20 such as silicon tetrachloride.
  • the extension 9 is immersed in the liquid bath 21 of a thermostat which permits heating and maintaining the liquid halogen compound at the temperature required for converting the amount of liquid into the gaseous phase needed for the required partial pressure of the halogen compound, for example 10 to 10- mm. Hg.
  • the vessel is further provided with a suction nipple 23 for connection with a vacuum pump or cooling trap (both not illustrated).
  • the modified embodiment of processing equipment shown in FIG. 2 is to some extent similar to that described above with reference to FIG. 1, corresponding components being denoted by the same reference numerals respectively in both illustrations.
  • the apparatus shown in FIG. 2 permits the production of thin layers of A B compounds.
  • two rods 1 and 11 are vertically mounted on a holder 14, these rods consisting of the two constituent elements of the compound, for example gallium and arsenic respectively.
  • Thin layers of A B compounds in addition to GaAs, such as InAs, InSb and GaSb can be similarly formed by utilizing rods 1 and 11 made of the respective constituent elements of these compounds.
  • the liquid 20 in the extension 9 of the precipitation vessel is provided with halogen compounds of both constituent elements, or with a halogen compound of one of the two elements.
  • the molten mounds 2 and 12 on top of the respective rods 1 and 11 can be produced by a single heating device.
  • two separate induction heater coils 3 and 13 are provided for this purpose. Separate openings are provided in the diaphragm 15 for the vapor emanating from each of the melts 2, 12, and an enlarged opening is provided in the diaphragm 16 to accommodate the vapor issuing from both openings in diaphragm 15.
  • the equipment and the performance of the precipitation method is analogous to the embodiment described with reference to FIG. 1
  • the following processing example was performed with apparatus according to FIG. 1.
  • a silicon rod 1 having a diameter of 12 mm. and a length of 5 cm. was used.
  • the top of the rod was heated by induction-heater coil 3 energized by alternating current of 4 megacycles per second, thus producing a self-supporting molten mound 2.
  • the evolving jet of vapor was kept away from the carrier 7 by means of a lid (not shown) beneath the carrier 7.
  • the thermostat 21 was filled with liquid air. After a period of about 1 minute, the thermostat was replaced by a vessel containing a temperature bath of -30 C.
  • silicon tetrachloride contained in the extension 9 slowly commenced to convert to the gaseous phase.
  • the resulting current of silicon tetrachloride gas was continuously exhausted through the nipple 23 with the aid of a mercury diffusion pump (not shown). This operation lasted about 5 minutes.
  • the above-mentioned covering lid was turned aside, thus exposing the carrier to the vapor jet issuing through the openings of the diaphragms 5 and 6, and the vapordeposition proper began to take place. During this stage the electric power supplied to the high-frequency coil was kept constant.
  • the layers thus produced were suitable for the production of transistors, particularly mesa transistors.
  • the above-described process using equipment such as is shown in FIG. 1 can also be performed by substituting silicochloroform SiI-ICl for the above-mentioned silicon tetrachloride, or by using analogous silicon com ounds of iodine or bromine.
  • the liquid 20 used in the equipment according to FIG. 1 may consist of @301 GeHCl or other germanium-chlorine compounds. Germanium compounds of iodine and bromine are likewise applicable.
  • the method of precipitating crystalline, particularly monocrystalline layers of highly pure semiconductor material and other brittle materials whereby the material to be precipitated is vaporized in a reaction vessel and precipitated on a carrier of similar lattice type, located in the same vessel, which comprises directing the material to be precipitated in the form of a vapor jet upon the carrier to be coated, executing the vaporization process by maintaining the gas pressure in the precipitation vessel such that the free path length of the vapor particles lies in the order of magnitude of the distance between the vapor source and the carrier and adding gaseous halide substances of the same vaporization material whose partial pressures amount to 10" to 10* mm. Hg to the vapor of the material to be precipitated.
  • the semiconductor material is elemental substance selected from the group consisting of silicon and germanium, and said gaseous substance consisting essentially of halogen compound of said elemental substance.
  • the method of precipitating crystalline, particularly monocrystalline, layers of pure semiconducting and other brittle materials upon crystalline carriers of similar lattice type which comprises heating a source of the material in a precipitation vessel under negative pressure to vaporizing temperature to produce a Vapor with a partial vapor pressure maximum of about 1 mm. Hg, mounting the carrier at a cooler location of the vaporization zone in the vessel to cause precipitation of the material upon the carrier, and gasifying a halogen-containing substance to admiX the resulting gas, to the vapor, at a gas partial pressure between and 10* mm. Hg.
  • the precipitation method according to claim 7, which comprises maintaining during precipitation the vessel space under a negative pressure at which the free path length of the vapor is in the order of magnitude corresponding to the distance between the source and the carrier.
  • the precipitation method according to claim 7, which comprises using a monocrystalline substrate of the same crystal lattice as the semiconductor material being precipitated, and precipitating a layer of 0.1 to 100 microns thickness upon the substrate.
  • the method of precipitating crystalline, particularly monocrystalline, layers of pure semiconducting and other brittle materials upon crystalline carriers of similar lattice type which comprises heating a source of the material in a precipitation vessel under negative pressure to vaporizing temperature and directing a jet of the evolving vapor from below onto the surface of the carrier to cause precipitation of the material; and gasifying, in communication with the vessel, a halogen-containing substance at a temperature corresponding to a partial pressure of the gas lower than that of the vapor, thus admixing the gas to the vapor from which the precipitation takes place.
  • the method of precipitating crystalline, particularly monocrystalline, layers of pure semiconducting and other brittle materials upon crystalline carriers of similar lattice type which comprises vertically mounting a rod of the material in a precipitation vessel and heating the top of the rod to melting and vaporizing temperature; directing a jet of the resulting vapor from below onto the surface of the carrier to cause precipitation of the material; and gasifying, in communication with the vessel, a halogencon-taining substance at a temperature corresponding to a partial pressure of the gas lower than that of the vapor,
  • the vapor-deposition method according to claim 15, which comprises passing the vapor from the rod top to the substrate surface through diaphragm means of inert material to obtain a vapor jet impinging substantially only on said substrate surface.
  • the method of precipitating crystalline, particularly Inonocrystalline layers of highly pure semiconductor material and other brittle materials whereby the material to be precipitated is vaporized in a reaction vessel and precipitated on a carrier of similar lattice type, located in the same vessel, which comprises directing the material to be precipitated in the form of a vapor jet upon the carrier to be coated, executing the vaporization process by maintaining the gas pressure in the precipitation vessel such that the free path length of the vapor particles lies in the order of magnitude of the distance between the vapor source and the carrier and that during the production of thin layers of A B compounds, the vapor of the precipitating material receives an addition of gaseous halide substances of a component of the vaporization material, whose partial pressures lie in the range of 10- to .10-

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
  • Chemical Vapour Deposition (AREA)
US302810A 1962-08-27 1963-08-19 Method of precipitating crystalline layers of highly pure, brittle materials Expired - Lifetime US3341360A (en)

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Application Number Priority Date Filing Date Title
DES81124A DE1278800B (de) 1962-08-27 1962-08-27 Verfahren zum schichtweisen kristallinen Vakuumaufdampfen hochreinen sproeden Materials

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3419417A (en) * 1966-02-01 1968-12-31 Ohio Crankshaft Co Apparatus and method of growing a crystal from a vapor
US3607067A (en) * 1970-02-09 1971-09-21 Siemens Ag Method of producing filamentary monocrystals
US3661637A (en) * 1969-01-02 1972-05-09 Siemens Ag Method for epitactic precipitation of silicon at low temperatures
US4330932A (en) * 1978-07-20 1982-05-25 The United States Of America As Represented By The Secretary Of The Navy Process for preparing isolated junctions in thin-film semiconductors utilizing shadow masked deposition to form graded-side mesas
US4523051A (en) * 1983-09-27 1985-06-11 The Boeing Company Thin films of mixed metal compounds
US4720373A (en) * 1984-07-13 1988-01-19 Research Corporation Solids refining apparatus
US20090117717A1 (en) * 2007-11-05 2009-05-07 Asm America, Inc. Methods of selectively depositing silicon-containing films

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1124028B (de) * 1960-01-15 1962-02-22 Siemens Ag Verfahren zum Herstellen von einkristallinem Silicium
US3178313A (en) * 1961-07-05 1965-04-13 Bell Telephone Labor Inc Epitaxial growth of binary semiconductors
US3224911A (en) * 1961-03-02 1965-12-21 Monsanto Co Use of hydrogen halide as carrier gas in forming iii-v compound from a crude iii-v compound

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL180750B (nl) * 1952-08-20 Bristol Myers Co Werkwijze voor het bereiden van een 7-amino-3-cefem-4-carbonzuur derivaat door een 7-acylamino-3-cefem-4-carbonzuur derivaat om te zetten.
DE1057845B (de) * 1954-03-10 1959-05-21 Licentia Gmbh Verfahren zur Herstellung von einkristallinen halbleitenden Verbindungen
DE1098316B (de) * 1957-06-26 1961-01-26 Union Carbide Corp Verfahren zum Herstellen einkristalliner UEberzuege aus dotierten Halbleitergrundstoffen durch Aufdampfen im Vakuum

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1124028B (de) * 1960-01-15 1962-02-22 Siemens Ag Verfahren zum Herstellen von einkristallinem Silicium
US3224911A (en) * 1961-03-02 1965-12-21 Monsanto Co Use of hydrogen halide as carrier gas in forming iii-v compound from a crude iii-v compound
US3178313A (en) * 1961-07-05 1965-04-13 Bell Telephone Labor Inc Epitaxial growth of binary semiconductors

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3419417A (en) * 1966-02-01 1968-12-31 Ohio Crankshaft Co Apparatus and method of growing a crystal from a vapor
US3661637A (en) * 1969-01-02 1972-05-09 Siemens Ag Method for epitactic precipitation of silicon at low temperatures
US3607067A (en) * 1970-02-09 1971-09-21 Siemens Ag Method of producing filamentary monocrystals
US4330932A (en) * 1978-07-20 1982-05-25 The United States Of America As Represented By The Secretary Of The Navy Process for preparing isolated junctions in thin-film semiconductors utilizing shadow masked deposition to form graded-side mesas
US4523051A (en) * 1983-09-27 1985-06-11 The Boeing Company Thin films of mixed metal compounds
US4720373A (en) * 1984-07-13 1988-01-19 Research Corporation Solids refining apparatus
US20090117717A1 (en) * 2007-11-05 2009-05-07 Asm America, Inc. Methods of selectively depositing silicon-containing films
US7772097B2 (en) 2007-11-05 2010-08-10 Asm America, Inc. Methods of selectively depositing silicon-containing films

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GB1013094A (en) 1965-12-15
DE1278800B (de) 1968-09-26

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