US3716345A - Czochralski crystallization of gallium arsenide using a boron oxide sealed device - Google Patents

Czochralski crystallization of gallium arsenide using a boron oxide sealed device Download PDF

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Publication number
US3716345A
US3716345A US00019289A US3716345DA US3716345A US 3716345 A US3716345 A US 3716345A US 00019289 A US00019289 A US 00019289A US 3716345D A US3716345D A US 3716345DA US 3716345 A US3716345 A US 3716345A
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Prior art keywords
melt
gallium arsenide
crucible
bell
crystal
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US00019289A
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English (en)
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J Grabmaier
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Siemens AG
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Siemens AG
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Priority claimed from DE19691913682 external-priority patent/DE1913682C3/de
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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
    • C30B29/42—Gallium arsenide
    • 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
    • C30B15/10—Crucibles or containers for supporting the melt
    • 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
    • C30B15/14—Heating of the melt or the crystallised materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N80/00—Bulk negative-resistance effect devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C2208/00—Plastics; Synthetic resins, e.g. rubbers
    • F16C2208/80—Thermosetting resins
    • F16C2208/90—Phenolic resin
    • 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
    • Y10T117/1032—Seed pulling
    • Y10T117/1052—Seed pulling including a sectioned crucible [e.g., double crucible, baffle]
    • 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
    • Y10T117/1032—Seed pulling
    • Y10T117/1068—Seed pulling including heating or cooling details [e.g., shield configuration]

Definitions

  • a method is known, for example, based on the idea that a given equilibrium vapor pressure of the melting compound in the crucible is maintained by providing a base member of the readily fugitive component, such as arsenic, for example, during the process of hardening in the crucible.
  • Another known method calls for regulating the vapor pressure by balancing the components instead of by providing a base member.
  • a further possibility for producing semiconductive compounds readily decomposable at the melting point thereof by employing lower than stoichiometric ratios of the components, i.e. a base member is employed as in the first known method described hereinabove and, in fact, in a way that the melt is not entirely stoichiometrically adjusted but rather, for example, in the production of gallium arsenide compounds, the gallium is present with an excess of several percent.
  • the same problems that are encountered in the production of the semiconductive compounds also occur in the crystal-pulling thereof.
  • the known methods are suitably modified therefor.
  • the starting point of the monocrystal-pulling for the semiconductive compounds, especially for gallium arsenide is the Czochralski method.
  • a difficulty encountered therein is to maintain at a high temperature a space completely sealed on all sides, in the interior of which the seed is to be displaced. If no special precautions are taken, the readily fugitive component of the compound, for example arsenic of gallium arsenide, vaporizes out of the melt and deposits on cold locations of the crucible.
  • the vaporization can be avoided by melting the compound in a closed vessel, and all surfaces which define the vaporization chamber in the closed vessel are held at a temperature which is higher than the condensation or sublimation temperature of the readily fugitive component. Pulling of the crystal from the melt is then indeed rendered more difficult because the pulling motion must be transmitted into the closed vessel while all parts of the vessel must be maintained at a relatively high temperature.
  • This problem is solvable by using a magnet system which permits the seed to be displaced. In this method which is quite difficult technically to carry out, it is generally impossible to prevent the formation of a thick layer of the semiconductive compound on the inner surface of the quartz vessel, which greatly obstructs the transparency of the vessel during melting processes that are carried over long periods of time- From the Journal Phys. Chem.
  • a protective gas atmosphere for example, argon at about 1 atmosphere excess pressure
  • argon at about 1 atmosphere excess pressure can forestall dissociation and prevent vaporization of the arsenic.
  • a monocrystal of a semiconductive compound relatively readily decomposable at the melting point thereof which comprises surrounding a crucible containing a melt producing of the semiconductive compound with a fluid medium extending to a level below the edge of the crucible, immersing a bell, which is axially rotatable and vertically displaceable and which has a crystal seed axially suspended therewithin, into the fluid medium so as to close off a volume above the surface of the melt, lowering the bell farther into the fluid medium until the crystal seed is immersed in the melt, and thereafter raising the bell so as to pull the seed crystal and a monocrystalline rod of the semiconductive compound out of the melt.
  • the fluid medium has a low melting point compared to that of the semiconductive compound and has a relatively low vapor pressure.
  • substances suitable as the fluid medium are boron oxide, gallium fused salt baths such as calcium chloride, for example.
  • I provide an outer crucible for receiving therein the fluid medium surrounding the crucible containing the melt, and including inductively coupling the outer crucible so that it serves as a susceptance for heating the crucible containing the melt.
  • the outer crucible is made of iridium, rhodium, platinum or graphite.
  • the bell is formed of quartz.
  • other impervious substances that are chemically resistant to molten boron oxide are also suitable for the bell.
  • the crystal pulling process is carried out in a protective gas atmosphere, such as in an argon or nitrogen current; but it is also possible, in accordance with the invention, to carry out the process in a closed system under high vacuum.
  • a protective gas atmosphere such as in an argon or nitrogen current
  • the method is capable of being carried out relatively simply.
  • I add dopant additive to the semiconductive melt.
  • the crystal pulling method of my invention is applicable to all substances that dissociate at the melting point thereof and yield readily fugitive components.
  • a crystal pulling system including a first crucible for receiving molten substance therein, the first crucible being received in a second and outer crucible having a diameter greater than that of the first crucible so that the first crucible is able to be surrounded by a fluid medium received in the second crucible and extending up to a level below the upper edge of the first crucible, a bell which is axially rotatable and vertically displaceable and which has a crystal seed axially suspended therewithin is coaxially disposed over the first crucible, the bell having a maximum diameter greater than the diameter of the first crucible, in-
  • FIGURE of the drawing shows schematically and insectional view the device for carrying out the monocrystal producing method of my invention.
  • a reaction vessel 1 wherein a crystal pulling process is to be carried out, the vessel 1 being a quartz tube which is connected, for example, to a vacuum pump or to a source of protective gas, such as argon or nitrogen.
  • the quartz tube 1 there is located on a crucible pedestal 2 a crucible 3 of platinum which simultaneously serves as an inductively coupled susceptance which, by means of an induction coil 4 surrounding the quartz tube 1 and connected by leads l4 and 15 to an electrical source (not shown), which heats a melt 6 received in a crucible 5 formed of quartz.
  • the crucible 5 is surrounded during the crystal pulling process with a fluid medium 7 having a low melting point compared to that of the melt 6 proper.
  • the fluid medium most advantageously consists of boron oxide (B 0 which, in addition to a low melting point and a low vapor pressure, has the advantage, that it is not miscible with the gallium arsenide.
  • the bell 8 is rotatable about an axial shaft 9 (as shown by the arrow 10) and is vertically displaceable (as shown by the double-headed arrow 11).
  • a crystal seed 12 is secured to the shaft 9 of the bell 8 within the latter and, as the bell 8 is lowered in the fluid medium 7, the crystal seed 12 is immersed in the gallium arsenide melt 6 and as the bell 8 is raised, a monocrystal rod 13, adhering to and growing from the crystal seed 12, is pulled from the melt 6.
  • the crystal pulling process is performed according to the well known principles of the Czochralski method either in protective gas atmosphere or in high vacuum. Adjustment of the parameters which are otherwise conventional for crystal pulling, such as pulling speed, rotation and crucible supply are effected in a conventional manner.
  • Method of producing, in accordance with the Czochralski principle, a monocrystal of gallium arsenide, which is relatively readily decomposable at the melting point thereof which comprises inserting an inner crucible containing a melt of the gallium arsenide into an outer crucible containing a fluid medium consisting of a melt of boron oxide extending to a level below the upper edge of the inner crucible and above the bottom of the inner crucible, inductively coupling the outer crucible so that it serves as a susceptance for heating the inner crucible containing the gallium arsenide melt, immersing a quartz bell, which is axially rotatable and vertically displaceable and which has a crystal seen axially suspended therewithin, into the boron oxide melt so as to close off a volume above the surface of the gallium arsenide melt, lowering the quartz bell farther into the boron oxide melt until the crystal seed is immersed in the gallium arsenide melt and thereafter raisingthe quartz bell
  • first crucible and means for forming a protective environment within said crystal pulling system.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
US00019289A 1969-03-18 1970-03-13 Czochralski crystallization of gallium arsenide using a boron oxide sealed device Expired - Lifetime US3716345A (en)

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Application Number Priority Date Filing Date Title
DE19691913682 DE1913682C3 (de) 1969-03-18 Vorrichtung zum Herstellen von Einkristallen aus halbleitenden Verbindungen

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US (1) US3716345A (US08177716-20120515-C00003.png)
AT (1) AT323236B (US08177716-20120515-C00003.png)
CA (1) CA933070A (US08177716-20120515-C00003.png)
CH (1) CH541989A (US08177716-20120515-C00003.png)
FR (1) FR2039601A5 (US08177716-20120515-C00003.png)
GB (1) GB1243930A (US08177716-20120515-C00003.png)
NL (1) NL6917398A (US08177716-20120515-C00003.png)
SE (1) SE363244B (US08177716-20120515-C00003.png)

Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3857679A (en) * 1973-02-05 1974-12-31 Univ Southern California Crystal grower
US3915656A (en) * 1971-06-01 1975-10-28 Tyco Laboratories Inc Apparatus for growing crystalline bodies from the melt
US4019645A (en) * 1972-12-04 1977-04-26 Heraeus-Schott Quarzschmelze Gmbh Crucible of fused vitreous silica
US4045181A (en) * 1976-12-27 1977-08-30 Monsanto Company Apparatus for zone refining
US4258009A (en) * 1977-08-22 1981-03-24 Topsil A/S Large crystal float zone apparatus
US4330361A (en) * 1980-02-14 1982-05-18 Wacker-Chemitronic Gesellschaft Fur Elektronic-Grundstoffe Mbh Process for the manufacture of high-purity monocrystals
US4596700A (en) * 1983-11-22 1986-06-24 Sumitomo Electric Industries, Ltd. Apparatus for producing single crystal
US4664742A (en) * 1984-05-25 1987-05-12 Kenji Tomizawa Method for growing single crystals of dissociative compounds
US4704257A (en) * 1983-08-31 1987-11-03 Research Development Corporation Of Japan Apparatus for growing single crystals of dissociative compounds
US4750969A (en) * 1985-06-27 1988-06-14 Research Development Corporation Of Japan Method for growing single crystals of dissociative compound semiconductor
US4873062A (en) * 1983-08-06 1989-10-10 Sumitomo Electric Industries, Ltd. Apparatus for the growth of single crystals
US4957713A (en) * 1986-11-26 1990-09-18 Kravetsky Dmitry Y Apparatus for growing shaped single crystals
US5021225A (en) * 1988-02-22 1991-06-04 Kabushiki Kaisha Toshiba Crystal pulling apparatus and crystal pulling method using the same
US5034200A (en) * 1988-01-27 1991-07-23 Kabushiki Kaisha Toshiba Crystal pulling apparatus and crystal pulling method
US5047112A (en) * 1990-08-14 1991-09-10 The United States Of America As Represented By The United States Department Of Energy Method for preparing homogeneous single crystal ternary III-V alloys
US5308947A (en) * 1992-01-30 1994-05-03 At&T Bell Laboratories Iridium fiber draw induction furnace
US5524571A (en) * 1984-12-28 1996-06-11 Sumitomo Electric Industries, Ltd. Method for synthesizing compound semiconductor polycrystals and apparatus therefor
US6059876A (en) * 1997-02-06 2000-05-09 William H. Robinson Method and apparatus for growing crystals
US6171395B1 (en) * 1997-12-02 2001-01-09 Wacker Siltronic Gesellschaft f{umlaut over (u)}r Halbleitermaterialien AG Process and heating device for melting semiconductor material
US20070111489A1 (en) * 2005-11-17 2007-05-17 Crabtree Geoffrey Jude Methods of producing a semiconductor body and of producing a semiconductor device
US20080203361A1 (en) * 2004-09-01 2008-08-28 Rensselaer Polytechnic Institute Method and Apparatus for Growth of Multi-Component Single Crystals
US20100050930A1 (en) * 2008-09-02 2010-03-04 Siemens Medical Solutions Usa, Inc. Crucible For A Crystal Pulling Apparatus
US20130163967A1 (en) * 2011-12-21 2013-06-27 Freiberger Compound Materials Gmbh Device and method of evaporating a material from a metal melt
US11434138B2 (en) 2017-10-27 2022-09-06 Kevin Allan Dooley Inc. System and method for manufacturing high purity silicon

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS545798B2 (US08177716-20120515-C00003.png) * 1973-02-12 1979-03-20
GB8718643D0 (en) * 1987-08-06 1987-09-09 Atomic Energy Authority Uk Single crystal pulling

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2892739A (en) * 1954-10-01 1959-06-30 Honeywell Regulator Co Crystal growing procedure
US3078151A (en) * 1958-11-17 1963-02-19 Siemens Ag Apparatus for drawing semiconductor bodies from a melt
US3088853A (en) * 1959-11-17 1963-05-07 Texas Instruments Inc Method of purifying gallium by recrystallization
US3198606A (en) * 1961-01-23 1965-08-03 Ibm Apparatus for growing crystals
US3235339A (en) * 1961-12-22 1966-02-15 Philips Corp Device for floating zone melting

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2892739A (en) * 1954-10-01 1959-06-30 Honeywell Regulator Co Crystal growing procedure
US3078151A (en) * 1958-11-17 1963-02-19 Siemens Ag Apparatus for drawing semiconductor bodies from a melt
US3088853A (en) * 1959-11-17 1963-05-07 Texas Instruments Inc Method of purifying gallium by recrystallization
US3198606A (en) * 1961-01-23 1965-08-03 Ibm Apparatus for growing crystals
US3235339A (en) * 1961-12-22 1966-02-15 Philips Corp Device for floating zone melting

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Richards, et al., Journal of Scientific Instruments, Vol. 34, July 1957, pp. 289 90 *

Cited By (29)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3915656A (en) * 1971-06-01 1975-10-28 Tyco Laboratories Inc Apparatus for growing crystalline bodies from the melt
US4019645A (en) * 1972-12-04 1977-04-26 Heraeus-Schott Quarzschmelze Gmbh Crucible of fused vitreous silica
US3857679A (en) * 1973-02-05 1974-12-31 Univ Southern California Crystal grower
US4045181A (en) * 1976-12-27 1977-08-30 Monsanto Company Apparatus for zone refining
US4258009A (en) * 1977-08-22 1981-03-24 Topsil A/S Large crystal float zone apparatus
US4330361A (en) * 1980-02-14 1982-05-18 Wacker-Chemitronic Gesellschaft Fur Elektronic-Grundstoffe Mbh Process for the manufacture of high-purity monocrystals
US4873062A (en) * 1983-08-06 1989-10-10 Sumitomo Electric Industries, Ltd. Apparatus for the growth of single crystals
US4704257A (en) * 1983-08-31 1987-11-03 Research Development Corporation Of Japan Apparatus for growing single crystals of dissociative compounds
US4596700A (en) * 1983-11-22 1986-06-24 Sumitomo Electric Industries, Ltd. Apparatus for producing single crystal
US4664742A (en) * 1984-05-25 1987-05-12 Kenji Tomizawa Method for growing single crystals of dissociative compounds
US5524571A (en) * 1984-12-28 1996-06-11 Sumitomo Electric Industries, Ltd. Method for synthesizing compound semiconductor polycrystals and apparatus therefor
US4750969A (en) * 1985-06-27 1988-06-14 Research Development Corporation Of Japan Method for growing single crystals of dissociative compound semiconductor
US4957713A (en) * 1986-11-26 1990-09-18 Kravetsky Dmitry Y Apparatus for growing shaped single crystals
US5034200A (en) * 1988-01-27 1991-07-23 Kabushiki Kaisha Toshiba Crystal pulling apparatus and crystal pulling method
US5021225A (en) * 1988-02-22 1991-06-04 Kabushiki Kaisha Toshiba Crystal pulling apparatus and crystal pulling method using the same
US5047112A (en) * 1990-08-14 1991-09-10 The United States Of America As Represented By The United States Department Of Energy Method for preparing homogeneous single crystal ternary III-V alloys
US5308947A (en) * 1992-01-30 1994-05-03 At&T Bell Laboratories Iridium fiber draw induction furnace
US6059876A (en) * 1997-02-06 2000-05-09 William H. Robinson Method and apparatus for growing crystals
US6171395B1 (en) * 1997-12-02 2001-01-09 Wacker Siltronic Gesellschaft f{umlaut over (u)}r Halbleitermaterialien AG Process and heating device for melting semiconductor material
US8940095B2 (en) 2004-09-01 2015-01-27 Rensselaer Polytechnic Institute Apparatus for growth of single crystals including a solute feeder
US20080203361A1 (en) * 2004-09-01 2008-08-28 Rensselaer Polytechnic Institute Method and Apparatus for Growth of Multi-Component Single Crystals
US7641733B2 (en) * 2004-09-01 2010-01-05 Rensselaer Polytechnic Institute Method and apparatus for growth of multi-component single crystals
US20100129657A1 (en) * 2004-09-01 2010-05-27 Rensselaer Polytechnic Institute Method and apparatus for growth of multi-component single crystals
US20070111489A1 (en) * 2005-11-17 2007-05-17 Crabtree Geoffrey Jude Methods of producing a semiconductor body and of producing a semiconductor device
US20100050930A1 (en) * 2008-09-02 2010-03-04 Siemens Medical Solutions Usa, Inc. Crucible For A Crystal Pulling Apparatus
US8114218B2 (en) * 2008-09-02 2012-02-14 Siemens Medical Solutions Usa, Inc. Crucible for a crystal pulling apparatus
US20130163967A1 (en) * 2011-12-21 2013-06-27 Freiberger Compound Materials Gmbh Device and method of evaporating a material from a metal melt
US10767255B2 (en) * 2011-12-21 2020-09-08 Freiberger Compound Materials Gmbh Device and method of evaporating a material from a metal melt
US11434138B2 (en) 2017-10-27 2022-09-06 Kevin Allan Dooley Inc. System and method for manufacturing high purity silicon

Also Published As

Publication number Publication date
DE1913682B2 (de) 1975-07-03
NL6917398A (US08177716-20120515-C00003.png) 1970-09-22
CH541989A (de) 1973-09-30
FR2039601A5 (US08177716-20120515-C00003.png) 1971-01-15
SE363244B (US08177716-20120515-C00003.png) 1974-01-14
AT323236B (de) 1975-06-25
CA933070A (en) 1973-09-04
DE1913682A1 (de) 1970-10-15
GB1243930A (en) 1971-08-25

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