EP0292777B1 - Method for manufacture of a ceramic coated metallic component - Google Patents

Method for manufacture of a ceramic coated metallic component Download PDF

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Publication number
EP0292777B1
EP0292777B1 EP88107493A EP88107493A EP0292777B1 EP 0292777 B1 EP0292777 B1 EP 0292777B1 EP 88107493 A EP88107493 A EP 88107493A EP 88107493 A EP88107493 A EP 88107493A EP 0292777 B1 EP0292777 B1 EP 0292777B1
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EP
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Prior art keywords
process according
layer
ceramic
ceramic layer
aluminium
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EP88107493A
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German (de)
French (fr)
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EP0292777A1 (en
Inventor
Mohamed Dr. Yarahmadi
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Interatom Internationale Atomreaktorbau GmbH
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Interatom Internationale Atomreaktorbau GmbH
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N13/00—Exhaust or silencing apparatus characterised by constructional features ; Exhaust or silencing apparatus, or parts thereof, having pertinent characteristics not provided for in, or of interest apart from, groups F01N1/00 - F01N5/00, F01N9/00, F01N11/00
    • F01N13/16—Selection of particular materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D19/00—Casting in, on, or around objects which form part of the product
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
    • F02B—INTERNAL-COMBUSTION PISTON ENGINES; COMBUSTION ENGINES IN GENERAL
    • F02B77/00—Component parts, details or accessories, not otherwise provided for
    • F02B77/02—Surface coverings of combustion-gas-swept parts
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
    • F05C—INDEXING SCHEME RELATING TO MATERIALS, MATERIAL PROPERTIES OR MATERIAL CHARACTERISTICS FOR MACHINES, ENGINES OR PUMPS OTHER THAN NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES
    • F05C2201/00—Metals
    • F05C2201/04—Heavy metals
    • F05C2201/043—Rare earth metals, e.g. Sc, Y
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
    • F05C—INDEXING SCHEME RELATING TO MATERIALS, MATERIAL PROPERTIES OR MATERIAL CHARACTERISTICS FOR MACHINES, ENGINES OR PUMPS OTHER THAN NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES
    • F05C2203/00—Non-metallic inorganic materials
    • F05C2203/08—Ceramics; Oxides

Definitions

  • the present invention relates to a method for producing a metallic component provided with a ceramic lining in a mold, a first ceramic layer being applied to this.
  • a method for producing a metallic component provided with a ceramic lining in a mold a first ceramic layer being applied to this.
  • the applicant has described a method by means of which castings made of metallic material can be provided with a cast-in smooth lining, e.g. so-called portliner of internal combustion engines.
  • layers are applied successively to a lost core by means of flame or plasma spraying, the composition of which is varied in such a way that a purely ceramic composition gradually becomes a finally purely metallic composition.
  • An arbitrarily thick layer of metal can be cast onto the latter to complete the component.
  • the graded transition from ceramic to metal leads to a gradual reduction of the stresses caused by the different thermal expansion of the two materials in the component.
  • JP-A 6 179 818 a method for producing a composite body is known, in which the different thermal expansions between the metal and the ceramic part are reduced by the fact that, as an intermediate layer, a grid or a fabric made of e.g. stainless steel or a ceramic fiber is introduced; penetration of the melted material into the grid is to be avoided in order to maintain the deformability required for the compensation.
  • this grid does not have a ductility leading to the different parts sliding off one another.
  • the object of the present invention is an alternative solution to the same technical problem, namely a coating of metallic components, preferably on the inside of those components that are hollow.
  • a sliding layer is first applied to the first ceramic layer; then a second ceramic layer divided into individual areas by joints; and finally in that the second ceramic layer is cast in a known manner with metal to form the finished component.
  • the first ceramic layer essentially forms the desired thermal protective layer and must be dimensioned with regard to its thickness and porosity; Layers (which can be produced using several conventional methods) of 2 to 3 mm thick (possibly composed of several partial layers applied one behind the other) appear suitable.
  • the sliding layer in turn only needs to have a thickness of 0.05 to 0.1 mm and, due to its ductility (which is also the case with the use of metal at these small thicknesses), reduces stresses by sliding the two ceramic layers against one another.
  • a layer thickness of 0.1 to 1 mm is recommended for the second ceramic layer. Splitting the same into numerous segments separated by joints of a few hundredths of a millimeter offers a possibility of reducing the stresses that occur after the coating of the metal has been cast around it by its greater thermal contraction during cooling by closing these joints. If the temperature rises again during operation, the second ceramic layer follows by opening it again.
  • a further embodiment of the invention teaches a method of how the required joints in the second ceramic layer can be produced in a defined size and frequency, namely in that they are specified by a grid placed on the sliding layer made of a material that is produced by the process of Applying the layer and / or burned or sublimed by the casting.
  • Various plastics appear suitable for the production of the grid.
  • Preferred materials for the production of the first ceramic layer are aluminum-titanium oxide, magnesium-aluminum-silicate, zirconium silicate or mullite. Like the materials proposed below for the second ceramic layer, they have a low modulus of elasticity, which dampens the transmission of vibrations to the metal parts.
  • the sliding layer consists of molybdenum disulfide or boron nitride.
  • Materials which are suitable according to the invention for the formation of the second ceramic layer and which have the required thermal shock resistance with good mechanical properties and sufficient chemical resistance are aluminum-titanium oxide, zirconium oxide / magnesium oxide, zirconium oxide / yttrium oxide, zirconium silicon oxide and magnesium aluminum -Silicate, aluminum oxide / silicon oxide, quartz material, mullite or spinel.
  • both the ceramic layers and the sliding layer are applied by plasma or flame spraying.
  • These closely related processes are particularly suitable for the production of thin, uniform layers on complexly shaped surfaces. They have a certain roughness on their free surface, which is conducive to better interlinking of the individual layers.
  • the method according to the invention appears particularly suitable for providing the inside of hollow bodies with ceramic protective layers.
  • a core made of glass is used, a very smooth inner surface of the coated component can be achieved. If low-melting metals are used, the glass can be replaced with a suitable plastic.
  • An embodiment of the invention is shown in the drawing, namely in longitudinal section using the example of the exhaust manifold of an internal combustion engine.
  • the thicknesses of the individual layers are greatly exaggerated for the sake of representability.
  • a lost core 1 made of glass was Plasma or flame spraying applied a first ceramic layer 2 several millimeters thick, then a very thin sliding layer 3 made of metal, boron nitride or molybdenum disulfide, and a second ceramic layer 4 on this in turn by the same method.
  • This is divided into individual fields by thin joints 5 ; the joints 5 represent the gaps left by the burning of a lattice that previously took their place.
  • B. cast aluminum or iron and subsequent destruction of the core 1, the component is completed.

Abstract

1. Process for the production of a metallic component provided with a ceramic coating in a mould (1), wherein a first ceramic layer (2) is applied to this mould, characterised by the following steps : a) applying a sliding layer (3) to the first ceramic layer (2), b) applying a second ceramic layer (4) divided by joints (5) into individual zones, c) casting, in known manner, the second ceramic layer (4) with metal (6) to form the finished component.

Description

Die vorliegende Erfindung betrifft ein Verfahren zur Herstellung eines mit einer Keramikauskleidung versehenen metallischen Bauteils in einer Form, wobei auf diese eine erste Keramikschicht aufgebracht wird. In ihrer nicht vorveröffentlichten deutschen Patentanmeldung P 3 705 903.3 hat die Anmelderin ein Verfahren beschrieben, mittels dessen Gußteile aus metallischem Werkstoff mit einer eingegossenen glatten Auskleidung versehen werden können, z.B. sogenannte Portliner von Verbrennungskraftmaschinen. Hier werden auf einen verlorenen Kern mittels Flamm- oder Plasmaspritzen nacheinander Schichten aufgebracht, deren Zusammensetzung so variiert wird, daß allmählich von einer rein keramischen Zusammensetzung zu einer schließlich rein metallischen Zusammensetzung gelangt wird. An letztere kann zur Fertigstellung des Bauteiles eine beliebig dicke Schicht Metall angegossen werden. Durch den gradierten Übergang von Keramik zu Metall wird ein allmählicher Abbau der durch die unterschiedliche Wärmeausdehnung der beiden Werkstoffe im Bauteil hervorgerufenen Spannungen erreicht. Aus der JP-A 6 179 818 ist ein Verfahren zur Herstellung eines Verbundkörpers bekannt, bei dem die unterschiedlichen Wärmedehnungen zwischen dem Metall- und dem Keramikteil dadurch abgebaut werden, daß als Zwischenschicht ein Gitter oder ein Gewebe aus z.B. rostfreiem Stahl oder einer Keramikfaser eingebracht wird; dabei soll ein Eindringen des Schmelzgutes in das Gitter vermieden werden, um seine für den Ausgleich erforderliche Verformbarkeit aufrechtzuerhalten. Eine zu einem Abgleiten der unterschiedlichen Teile voneinander führende Duktilität weist dieses Gitter jedoch nicht auf.The present invention relates to a method for producing a metallic component provided with a ceramic lining in a mold, a first ceramic layer being applied to this. In her unpublished German patent application P 3 705 903.3, the applicant has described a method by means of which castings made of metallic material can be provided with a cast-in smooth lining, e.g. so-called portliner of internal combustion engines. Here layers are applied successively to a lost core by means of flame or plasma spraying, the composition of which is varied in such a way that a purely ceramic composition gradually becomes a finally purely metallic composition. An arbitrarily thick layer of metal can be cast onto the latter to complete the component. The graded transition from ceramic to metal leads to a gradual reduction of the stresses caused by the different thermal expansion of the two materials in the component. From JP-A 6 179 818 a method for producing a composite body is known, in which the different thermal expansions between the metal and the ceramic part are reduced by the fact that, as an intermediate layer, a grid or a fabric made of e.g. stainless steel or a ceramic fiber is introduced; penetration of the melted material into the grid is to be avoided in order to maintain the deformability required for the compensation. However, this grid does not have a ductility leading to the different parts sliding off one another.

Aufgabe der vorliegenden Erfindung ist eine Alternativlösung für das gleiche technische Problem, nämlich eine Beschichtung von metallischen Bauteilen, vorzugsweise auf der Innenseite solcher Bauteile, die hohl sind.The object of the present invention is an alternative solution to the same technical problem, namely a coating of metallic components, preferably on the inside of those components that are hollow.

Die Lösung dieser Aufgabe erfolgt erfindungsgemäß dadurch, daß zunächst auf die erste Keramikschicht eine Gleitschicht aufgebracht wird; auf diese sodann eine zweite, durch Fugen in einzelne Bereiche geteilte Keramikschicht; und schließlich dadurch, daß, die zweite Keramikschicht in an sich bekannter Weise mit Metall zum fertigen Bauteil umgossen wird. Die erste Keramikschicht bildet im wesentlichen die gewünschte thermische Schutzschicht und ist mit Rücksicht hierauf in ihrer Dicke und Porosität zu bemessen; Schichten (die auf mehrere, herkömmliche Verfahrensweisen hergestellt werden können) von 2 bis 3 mm Dicke (ggf. aus mehreren, hintereinander aufgebrachten Teilschichten zusammengesetzt) erscheinen geeignet. Die Gleitschicht ihrerseits braucht nur eine Dicke von 0,05 bis 0,1 mm aufzuweisen und bewirkt vermöge ihrer Duktilität (die bei diesen geringen Dicken auch bei Verwendung von Metall gegeben ist) einen Abbau von Spannungen durch ein Aneinanderabgleiten der beiden Keramikschichten. Für die zweite Keramikschicht empfiehlt sich eine Schichtdicke von 0,1 bis 1 mm. Das Aufteilen derselben auf zahlreiche Segmente, die durch Fugen von wenigen Hundertstel mm voneinander getrennt sind, bietet eine Möglichkeit, die nach dem Umgießen der Schicht mit dem Metall durch dessen größere Wärmekontraktion bei der Abkühlung auftretenden Spannungen durch ein Schließen dieser Fugen zu verringern. Bei späterer erneuter Temperaturerhöhung im Betrieb folgt die zweite Keramikschicht durch erneutes Öffnen derselben.This object is achieved according to the invention in that a sliding layer is first applied to the first ceramic layer; then a second ceramic layer divided into individual areas by joints; and finally in that the second ceramic layer is cast in a known manner with metal to form the finished component. The first ceramic layer essentially forms the desired thermal protective layer and must be dimensioned with regard to its thickness and porosity; Layers (which can be produced using several conventional methods) of 2 to 3 mm thick (possibly composed of several partial layers applied one behind the other) appear suitable. The sliding layer in turn only needs to have a thickness of 0.05 to 0.1 mm and, due to its ductility (which is also the case with the use of metal at these small thicknesses), reduces stresses by sliding the two ceramic layers against one another. A layer thickness of 0.1 to 1 mm is recommended for the second ceramic layer. Splitting the same into numerous segments separated by joints of a few hundredths of a millimeter offers a possibility of reducing the stresses that occur after the coating of the metal has been cast around it by its greater thermal contraction during cooling by closing these joints. If the temperature rises again during operation, the second ceramic layer follows by opening it again.

Eine weitere Ausgestaltung der Erfindung lehrt ein Verfahren, wie die geforderten Fugen in der zweiten Keramikschicht in definierter Größe und Häufigkeit hergestellt werden können, und zwar dadurch, daß sie durch ein auf die Gleitschicht aufgelegtes Gitter aus einem Werkstoff vorgegeben werden, der durch den Vorgang des Aufbringens der Schicht und/oder durch das Umgießen verbrannt oder sublimiert wird. Verschiedene Kunststoffe erscheinen für die Herstellung des Gitters geeignet.A further embodiment of the invention teaches a method of how the required joints in the second ceramic layer can be produced in a defined size and frequency, namely in that they are specified by a grid placed on the sliding layer made of a material that is produced by the process of Applying the layer and / or burned or sublimed by the casting. Various plastics appear suitable for the production of the grid.

Bevorzugte Werkstoffe für die Herstellung der ersten Keramikschicht sind Aluminium-Titan-Oxyd, Magnesium-Aluminium-Silikat, Zirkonsilikat oder Mullit. Sie weisen ebenso wie die weiter unten für die zweite Keramikschicht vorgeschlagenen Werkstoffe einen geringen E-Modul auf, wodurch die Übertragung von Vibrationen auf die Metallteile gedämpft wird.Preferred materials for the production of the first ceramic layer are aluminum-titanium oxide, magnesium-aluminum-silicate, zirconium silicate or mullite. Like the materials proposed below for the second ceramic layer, they have a low modulus of elasticity, which dampens the transmission of vibrations to the metal parts.

Die Gleitschicht besteht in vorteilhaften Weiterbildungen der Erfindung aus Molybdändisulfid oder Bornitrid.In advantageous developments of the invention, the sliding layer consists of molybdenum disulfide or boron nitride.

Für die Bildung der zweiten Keramikschicht erfindungsgemäß geeignete Werkstoffe, die die geforderte Temperaturwechselfestigkeit bei guten mechanischen Eigenschaften und ausreichender chemischer Beständigkeit aufweisen, sind Aluminium-Titan-Oxyd, Zirkonoxyd/Magnesium-Oxyd, Zirkonoxyd/Yttrium-Oxyd, Zirkonsilizium-Oxyd, Magnesium-Aluminium-Silikat, Aluminiumoxyd/Siliziumoxyd, Quarzgut, Mullit oder Spinell.Materials which are suitable according to the invention for the formation of the second ceramic layer and which have the required thermal shock resistance with good mechanical properties and sufficient chemical resistance are aluminum-titanium oxide, zirconium oxide / magnesium oxide, zirconium oxide / yttrium oxide, zirconium silicon oxide and magnesium aluminum -Silicate, aluminum oxide / silicon oxide, quartz material, mullite or spinel.

Sowohl das Aufbringen der Keramikschichten als auch dasjenige der Gleitschicht erfolgt gemäß der Erfindung durch Plasma- oder Flammspritzen. Diese eng verwandten Verfahren eignen sich besonders zur Herstellung dünner, gleichmäßiger Schichten auf kompliziert geformten Oberflächen. An ihrer freien Oberfläche weisen sie eine gewisse Rauhigkeit auf, die der besseren Verzahnung der einzelnen Schichten untereinander dienlich ist.According to the invention, both the ceramic layers and the sliding layer are applied by plasma or flame spraying. These closely related processes are particularly suitable for the production of thin, uniform layers on complexly shaped surfaces. They have a certain roughness on their free surface, which is conducive to better interlinking of the individual layers.

Das erfindungsgemäße Verfahren erscheint besonders geeignet, das Innere von Hohlkörpern mit keramischen Schutzschichten zu versehen. Dazu empfiehlt sich in weiterer Ausgestaltung eine Verwendung verlorener Kerne, von denen ausgehend das Bauteil aufgebaut wird.The method according to the invention appears particularly suitable for providing the inside of hollow bodies with ceramic protective layers. In a further embodiment, it is recommended to use lost cores from which the component is built.

Wird ein Kern aus Glas verwendet, kann eine sehr glatte Innenoberfläche des beschichteten Bauteils erzielt werden. Bei Verwendung niedrigschmelzender Metalle kann das Glas durch einen geeigneten Kunststoff ersetzt werden.If a core made of glass is used, a very smooth inner surface of the coated component can be achieved. If low-melting metals are used, the glass can be replaced with a suitable plastic.

Ein Ausführungsbeispiel der Erfindung ist in der Zeichnung dargestellt, und zwar im Längsschnitt am Beispiel des Abgaskrümmers einer Verbrennungskraftmaschine. Die Dicken der einzelnen Schichten sind der Darstellbarkeit zuliebe stark übertrieben. Auf einen verlorenen Kern 1 aus Glas wurde mittels Plasma- oder Flammspritzen eine mehrere Millimeter dicke erste Keramikschicht 2 aufgebracht, auf diese dann eine sehr dünne Gleitschicht 3 aus Metall, Bornitrid oder Molybdändisulfid und auf diese wiederum nach dem gleichen Verfahren eine zweite Keramikschicht 4. Diese wird durch dünne Fugen 5 in einzelne Felder geteilt; dabei stellen die Fugen 5 die durch das Verbrennen eines vorher ihre Stelle einnehmenden Gitters hinterlassenen Lücken dar. Durch ein Umgießen des so hergestellten Gebildes mit einem den eigentlichen Körper des Bauteils bildenden Metall 6, z. B. Aluminium- oder Eisenguß und anschließende Zerstörung des Kernes 1 wird das Bauteil fertiggestellt.An embodiment of the invention is shown in the drawing, namely in longitudinal section using the example of the exhaust manifold of an internal combustion engine. The thicknesses of the individual layers are greatly exaggerated for the sake of representability. On a lost core 1 made of glass was Plasma or flame spraying applied a first ceramic layer 2 several millimeters thick, then a very thin sliding layer 3 made of metal, boron nitride or molybdenum disulfide, and a second ceramic layer 4 on this in turn by the same method. This is divided into individual fields by thin joints 5 ; the joints 5 represent the gaps left by the burning of a lattice that previously took their place. B. cast aluminum or iron and subsequent destruction of the core 1, the component is completed.

Claims (11)

1. Process for the production of a metallic component provided with a ceramic coating in a mould (1), wherein a first ceramic layer (2) is applied to this mould, characterised by the following steps:
a) applying a sliding layer (3) to the first ceramic layer (2),
b) applying a second ceramic layer (4) divided by joints (5) into individual zones,
c) casting, in known manner, the second ceramic layer (4) with metal (6) to form the finished component.
2. Process according to claim 1, characterised in that the joints (5) in the second ceramic layer (4) are provided by a grid disposed on the sliding layer (3), the grid being made of a material which is combusted or sublimated by the process of applying the layer and/or by casting.
3. Process according to claim 1, characterised in that the first ceramic layer (2) is made of aluminium titanium-oxide, magnesium-aluminium-silicate, zirconium silicate or mullite.
4. Process according to claim 1, characterised in that the sliding layer (3) is made of a metal.
5. Process according to claim 4, characterised in that the sliding layer (3) is made of titanium or a nickelaluminium alloy, a nickel-chromium-alloy, a nickelchromium-aluminium-yttrium-alloy, a nickel- cobaltchromium-aluminium-yttrium-alloy or a cobalt- chromiumaluminium-yttrium alloy.
6. Process according to claim 1, characterised in that the sliding layer (3) comprises molybdenum disulphide or boron nitride.
7. Process according to claim 1, characterised in that the second ceramic layer (4) is made of aluminium titanium oxide, zirconium oxide/magnesium oxide, zirconium oxide/yttrium oxide, zirconium silicon oxide, magnesium-aluminium-silicate, aluminium-ox- ide/silicon oxide, quartz material, mullite or spinel.
8. Process according to claim 1, characterised in that the first and second ceramic layers (2, 4) are applied by plasma spraying or flame spraying.
9. Process according to claim 1, characterised in that the sliding layer (3) is applied by plasma spraying or flame spraying.
10. Process according to claim 1 for producing a hollow component (6) provided on its inner surface with a ceramic coating (2, 4), characterised in that a lost core (1) is used as the mould.
11. Process according to claim 10, characterised in that a core (1) of glass is used.
EP88107493A 1987-05-21 1988-05-09 Method for manufacture of a ceramic coated metallic component Expired - Lifetime EP0292777B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88107493T ATE55565T1 (en) 1987-05-21 1988-05-09 PROCESS FOR MANUFACTURING A CERAMIC-COATED METALLIC COMPONENT.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3717152 1987-05-21
DE3717152 1987-05-21

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EP0292777A1 EP0292777A1 (en) 1988-11-30
EP0292777B1 true EP0292777B1 (en) 1990-08-16

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EP (1) EP0292777B1 (en)
JP (1) JPS63303674A (en)
AT (1) ATE55565T1 (en)
DE (1) DE3860455D1 (en)

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DE3860455D1 (en) 1990-09-20
ATE55565T1 (en) 1990-09-15
US4890663A (en) 1990-01-02
EP0292777A1 (en) 1988-11-30
JPS63303674A (en) 1988-12-12

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