EP0185603A1 - Verbesserung der Lebensdauer von metallvulkanischen Turbinenabdichtungen - Google Patents

Verbesserung der Lebensdauer von metallvulkanischen Turbinenabdichtungen Download PDF

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Publication number
EP0185603A1
EP0185603A1 EP85630204A EP85630204A EP0185603A1 EP 0185603 A1 EP0185603 A1 EP 0185603A1 EP 85630204 A EP85630204 A EP 85630204A EP 85630204 A EP85630204 A EP 85630204A EP 0185603 A1 EP0185603 A1 EP 0185603A1
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EP
European Patent Office
Prior art keywords
ceramic
ranges
metallic
seal
materials
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP85630204A
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English (en)
French (fr)
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EP0185603B1 (de
Inventor
Harry Edwin Eaton
Richard Charles Novak
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RTX Corp
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United Technologies Corp
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Publication date
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Publication of EP0185603A1 publication Critical patent/EP0185603A1/de
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Publication of EP0185603B1 publication Critical patent/EP0185603B1/de
Expired legal-status Critical Current

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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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • C23C4/11—Oxides
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01D—NON-POSITIVE DISPLACEMENT MACHINES OR ENGINES, e.g. STEAM TURBINES
    • F01D11/00—Preventing or minimising internal leakage of working-fluid, e.g. between stages
    • F01D11/08—Preventing or minimising internal leakage of working-fluid, e.g. between stages for sealing space between rotor blade tips and stator
    • F01D11/12—Preventing or minimising internal leakage of working-fluid, e.g. between stages for sealing space between rotor blade tips and stator using a rubstrip, e.g. erodible. deformable or resiliently-biased part
    • F01D11/122—Preventing or minimising internal leakage of working-fluid, e.g. between stages for sealing space between rotor blade tips and stator using a rubstrip, e.g. erodible. deformable or resiliently-biased part with erodable or abradable material

Definitions

  • the field of the invention is that of gas turbine engine air seals and also the field of plasma spraying of mixed metal-ceramic materials.
  • a shroud termed an outer air seal, circumscribes each row of turbine blading to inhibit the leakage of working medium gases over the blade tips.
  • the limitation of the leakage of the working medium gases is crucial to the achievement of high efficiencies in such engines.
  • the graded ceramic seals described herein were developed for specific application in gas turbine outer air seals, although other applications are clearly possible. Durable seals capable of long-term, reliable service in the hostile turbine environment were required. Specifically sought were high temperature capability and good resistance to thermal shock.
  • the seal material must have adequate surface abradability to prevent destructive interference upon occurrence of rubbing contact of the seals by the circumscribed turbine blading.
  • discrete graded layer seals of the type described in U.S. Patent No. 4,481,237 or continuously graded metal-ceramic seals of the type described in copending U.S. Application Serial No. 675 806 "Method for Producing Continuously Graded Air Seals", filed on even date herewith, are afforded substantially enhanced performance by employing as a ceramic material in the graded portion, a material having a low oxygen permeability at elevated temperatures such as alumina, mullite, or the M g 0'A1 2 0 3 spinel.
  • oxidation resistant metallic materials are employed, particularly those of the MCrAlY type (where M is Fe, Ni or Co) and related materials.
  • One such method involves reducing the surface area of the metallic constituent by either limiting the powder size to be relatively coarse and uniform (i.e., reducing the high surface area fine particle content) and/or employing plasma deposition parameters under which the metallic constituent does not melt completely so that upon impact it remains in a rounded form rather than assuming a high surface area splat configuration.
  • Another approach is to preoxidize the metallic constituent.
  • the final concept relates to minimizing the swelling resulting from oxidation of the metallic constituent by deliberately inducing porosity into the material by cospraying a fugitive material along with the metallic-ceramic material.
  • the invention also teaches the use of a thin 100% alumina layer on the mixed layer for purposes of affording total resistance to oxygen penetration and the use of a abradable ceramic layer such as zirconia as the outer seal constituent to provide abradable rubbing contact upon interaction with the moving turbine blading and to provide improved temperature capabilities.
  • the requirements for producing a successful graded metal-ceramic seal may be organized in two categories.
  • the first is the physical requirements of the seal, particularly composition.
  • the second relates to the residual strain which may be built into the system through control of substrate temperature during plasma deposition.
  • This invention is directed at the first category, namely, the physical properties of the graded metal-ceramic layer.
  • Aspects of the second category, namely the control of residual strain will be described as necessary to permit an understanding of the best mode of practicing the invention. These strain control aspects are described in U.S. Patent No. 4,481,237 (which is incorporated herein by reference) for the discrete layer case and in U.S. Patent Application Serial No. 675 806 filed on even date herewith (which is incorporated herein by reference) for the case of continuous grading.
  • Figure 1 illustrates the composition versus thickness of the best seal known to the inventors at the time of the filing of this application.
  • the X axis shows seal thickness in mils and the total seal thickness is approximately 150 mils. Since the seal is deposited by a plasma deposition, the seal thickness will actually vary in a stepwise fashion from one layer to the next, however, since each layer is in the order of 1 mil thick the continuous curve of Figure 1 is a more than adequate description of the seal composition.
  • an initial metallic bond coat of a composition known as Metco 443 which is a commercially available material formed from an agglomeration of nickel chromium powder and aluminum powder which upon plasma spraying undergoes an exothermic reaction which is believed to aid in the adherence of the bond coat to the substrate.
  • Metco 443 a composition known as Metco 443 which is a commercially available material formed from an agglomeration of nickel chromium powder and aluminum powder which upon plasma spraying undergoes an exothermic reaction which is believed to aid in the adherence of the bond coat to the substrate.
  • the next 20 mils are of a constant composition of 60% CoCrAlY (nominal composition of Co-23Cr-13Al-0.65Y) having a particle size of -100+325 U.S. Standard Sieve and 40% alumina.
  • continuous grading occurs over the next 25 mils or so until a composition of 20% CoCrAlY and 80% alumina is reached.
  • This composition is maintained constant for about 10 mils then the grading process continues until a composition of 100% alumina is achieved.
  • One layer (1+.5 mil) of 100% alumina is then deposited, it has been found that the absence of all alumina layer detracts from oxidation performance but that multiple layers are detrimental to mechanical behavior.
  • an outer layer of zirconia is applied to provide abradability and temperature capability (A1 2 0 3 melts at ⁇ 2000°C while ZrO 2 melts at -2700 0 C).
  • Alumina is a harder, stronger material than zirconia and alumina as the outer layer would not have the desired abradable qualities.
  • Figure 2 is a photomicrograph of the resultant structure.
  • the metallic constituent is light in color
  • the alumina is dark gray
  • the zirconia is light gray
  • the porosity is black.
  • Figure 3 is a schematic of a turbine air seal showing the arrangement or layers, the plasma torch and the substrate heating.
  • Figure 4 illustrates the temperature control of the substrate which is employed during plasma spraying to attain the desired and necessary substrate prestrain conditions.
  • the substrate temperature is maintained at a relatively high level during deposition of the bond coat and is then reduced. Thereafter the substrate temperature is increased generally in parallel with the ceramic content and eventually reaches a level above that employed during deposition of the bond coat and then tapers off during the deposition of the outer abradable ceramic material.
  • a primary aspect of this invention is the substitution of a material which is resistant to the diffusion of oxygen at elevated temperatures.
  • Three such materials have been identified for seal application. These are alumina, mullite and the MgO'Al 2 O 3 spinel.
  • Figure 5 shows the permeability of stabilized zirconia and alumina over a temperature range at 50 Torr partial pressure of oxygen. It can be seen that at 1600°C the permeability of oxygen in alumina is less than about 10 and it is about 3 orders of magnitude less than the permeability of oxygen in zirconia at the same temperature.
  • oxidation resistant materials selected from the group consisting of the MCr materials where chromium ranges from about 20 to about 40%; the MCrAl materials where chromium ranges from about 15 to about 45% and aluminum ranges from about 7 to about 15%; the MCrAlY materials where chromium ranges from about 15 to about 45%, aluminum ranges from about 6 to about 20% and yttrium ranges from about 0.1 to about 5%; and the MCrAlHf materials where chromium ranges from about 15 to about 45%, aluminum ranges from about 7 to about 15% and hafnium ranges from about 0.5 to about 7%
  • M is selected from the group consisting of nickel, cobalt,iron and mixtures thereof with mixtures of nickel and cobalt being particularly favored
  • the yttrium when present
  • the yttrium may be partly or wholly replaced by lanthanum, cerium, Misch metal and mixtures thereof, additionally, up to 10% of a material selected from the group consisting of
  • Table I presents oxidation data for two compositions based on ceramic-CoCrAlY materials.
  • the ceramic is zirconia and the other the ceramic is alumina, in both compositions the CoCrAlY content was the same volume percent. These materials were tested at 1900°F for 150 hours. The results are presented in the table. It can be seen that the zirconia base material gained 3.3% in weight due to oxidation of the metallic constituent and underwent a longitudinal expansion of 3.4% due to swelling of the material caused by the oxidation of the metallic constituent. Under the same condition the alumina based material gained 2.1% in weight, (a reduction of 37% compared to the zirconia based material), and shrank 0.5% in length.
  • the information in Table I supports the basic premise of the invention which that the substitution of alumina for the commonly used zirconia material in mixed metal-ceramic systems provides substantial seal performance benefits.
  • Table II shows the benefit obtained through minimizing the surface area of the metallic constituent by sieving out the fine particles.
  • both compositions were based on the zirconia ceramic which serves as a valid baseline for demonstrating the benefits obtained by employing coarse particles.
  • Table II shows the weight change results of two materials both of which had the same composition of 85% zirconia, 15% CoCrAlY, the difference between the two samples being that one was produced from a wide size range metallic powder composition of -100+325 mesh while the other was produced from metallic material having -100+200 mesh (the mesh sizes referred to are those described in the U.S.
  • Table III presents basic information on the effect of including deliberate porosity on the performance of alumina-CoCrAlY composites produced by plasma spraying. From Table III it is evident that material which contained 4% polyester and therefore contains some amount of porosity (about 2%) exhibited slightly increased weight change due to oxidation but rather significantly decreased dimensional changes. Thus, the deliberate inclusion of porosity is an area which will require careful attention by the skilled artisan.
  • the final suggested technique for reducing oxidation and resultant swelling is to perform the plasma spraying under conditions which do not entirely melt the metallic constituent so that the metallic constituent will retain a more nearly spheroidal configuration within the graded coating rather than assuming a completely flattened splat configuration which will result if total melting occurs.
  • Observed aspect ratios (length:thickness) in totally melted materials are from about 5:1 to about 10:1, reduced surface areas result when aspect ratios of about 3:1 or less are produced. This result may be accomplished by adjusting the position within the plasma torch where the metallic constituent is injected so that the metallic constituent has a short residence time within the plasma zone and does not melt completely.
  • the use of coarse particles also assists in controlling aspect ratio.
  • the essentials of the system are accurate measurements of carrier gas flow and pressure coupled with x-ray measurements of the gas plus powder stream, these measurements are supplied to a controlling microcomputer which generates signals necessary to control the flow of gas and the flow of the various powders.
  • U.S. Patent Application Serial No. 6 7 5 8 0 1 deals with the powder flow gauging techniques which are used to measure the actual powder streams and to control their flow
  • the x-ray gauging system uses flow and pressure sensors to provide accurate measurements of carrier gas flow and uses a transmission x-ray apparatus to give an indication of the total mass flow of powder plus carrier gas. From these measurements the mass flow rate can be accurately calculated. Knowing the actual powder mass flow rate one can employ control circuitry to control and constrain the powder flow rate to follow a predetermined schedule.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Coating By Spraying Or Casting (AREA)
  • Turbine Rotor Nozzle Sealing (AREA)
EP85630204A 1984-11-28 1985-11-27 Verbesserung der Lebensdauer von metallvulkanischen Turbinenabdichtungen Expired EP0185603B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US67579784A 1984-11-28 1984-11-28
US675797 1984-11-28

Publications (2)

Publication Number Publication Date
EP0185603A1 true EP0185603A1 (de) 1986-06-25
EP0185603B1 EP0185603B1 (de) 1989-11-08

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EP85630204A Expired EP0185603B1 (de) 1984-11-28 1985-11-27 Verbesserung der Lebensdauer von metallvulkanischen Turbinenabdichtungen

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EP (1) EP0185603B1 (de)
JP (1) JPS61153269A (de)
DE (1) DE3574168D1 (de)

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT396119B (de) * 1988-04-08 1993-06-25 Stangl Kurt Dipl Ing Verfahren zum beschriften heisser stahlbloecke
AT396120B (de) * 1988-04-13 1993-06-25 Stangl Kurt Dipl Ing Verfahren zum beschriften heisser stahlbloecke
EP0605196A1 (de) * 1992-12-29 1994-07-06 General Electric Company Verfahren zum Aufbringen einer Wärmedämmschicht
WO1996034128A1 (en) * 1995-04-25 1996-10-31 Siemens Aktiengesellschaft Metal substrate with an oxide layer and an anchoring layer
WO1998004759A1 (en) * 1996-04-12 1998-02-05 Siemens Aktiengesellschaft Metal substrate with an oxide layer and an improved anchoring layer
GB2380492A (en) * 2001-09-05 2003-04-09 Trw Ltd Friction member with graded coating
EP1382707A1 (de) * 2002-07-17 2004-01-21 Siemens Aktiengesellschaft Schichtsystem
DE102013213386B3 (de) * 2013-07-09 2014-08-14 MTU Aero Engines AG Strömungsmaschinen-Keramikbauteil
EP3133251A1 (de) * 2015-08-17 2017-02-22 United Technologies Corporation Äussere laufschaufelluftdichtungskomponente mit unterschiedlichen wärmeausdehnungskoeffizienten
EP3421732A3 (de) * 2017-06-30 2019-01-09 United Technologies Corporation Turbinenmotordichtung für umgebung mit hoher erosion
US10309002B2 (en) 2013-12-05 2019-06-04 General Electric Company Coating methods and a template for use with the coating methods
US10385725B2 (en) 2012-08-07 2019-08-20 Safran Aircraft Engines Abradable coating made of a material having a low surface roughness

Families Citing this family (8)

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Publication number Priority date Publication date Assignee Title
DE3538390A1 (de) * 1985-10-29 1987-04-30 Deutsche Forsch Luft Raumfahrt Beschichtung fuer ein substrat und verfahren zu dessen herstellung
US4743462A (en) * 1986-07-14 1988-05-10 United Technologies Corporation Method for preventing closure of cooling holes in hollow, air cooled turbine engine components during application of a plasma spray coating
GB8706951D0 (en) * 1987-03-24 1988-04-27 Baj Ltd Overlay coating
DE4103994A1 (de) * 1991-02-11 1992-08-13 Inst Elektroswarki Patona Schutzueberzug vom typ metall-keramik fuer einzelteile aus hitzebestaendigen legierungen
WO1993024672A1 (en) * 1992-05-29 1993-12-09 United Technologies Corporation Ceramic thermal barrier coating for rapid thermal cycling applications
DE59801547D1 (de) * 1997-11-03 2001-10-25 Siemens Ag Erzeugnis, insbesondere bauteil einer gasturbine, mit keramischer wärmedämmschicht
SG72959A1 (en) * 1998-06-18 2000-05-23 United Technologies Corp Article having durable ceramic coating with localized abradable portion
JP5210984B2 (ja) * 2009-06-29 2013-06-12 株式会社日立製作所 タービン用高信頼性メタルシール材

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FR918141A (fr) * 1944-12-01 1947-01-30 Bbc Brown Boveri & Cie Ailette de turbine faite au moins partiellement en poudre frittée de métal et de matière céramique, pour machines travaillant à haute température
US3091548A (en) * 1959-12-15 1963-05-28 Union Carbide Corp High temperature coatings
US3758233A (en) * 1972-01-17 1973-09-11 Gen Motors Corp Vibration damping coatings
FR2190754A1 (de) * 1972-05-11 1974-02-01 Asahi Glass Co Ltd
WO1982001898A1 (en) * 1980-12-05 1982-06-10 Kvernes Ingard Method for coating a metal with a protection layer resistant to hot gas corrosion
CH648358A5 (en) * 1980-12-05 1985-03-15 Castolin Sa Process for producing a protective layer, resistant to corrosion by hot gas, on metal components

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US4255495A (en) * 1979-10-31 1981-03-10 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Corrosion resistant thermal barrier coating
JPS6026964B2 (ja) * 1980-08-20 1985-06-26 ファナック株式会社 警報回路を有するパルスエンコ−ダ装置
DE3137731A1 (de) * 1981-09-23 1983-04-14 Battelle-Institut E.V., 6000 Frankfurt Hochtemperatur- und thermoschockbestaendige kompaktwerkstoffe und beschichtungen
US4481237A (en) * 1981-12-14 1984-11-06 United Technologies Corporation Method of applying ceramic coatings on a metallic substrate
JPS58167764A (ja) * 1982-03-26 1983-10-04 Toyo Eng Corp 耐熱合金基材の被覆法

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FR918141A (fr) * 1944-12-01 1947-01-30 Bbc Brown Boveri & Cie Ailette de turbine faite au moins partiellement en poudre frittée de métal et de matière céramique, pour machines travaillant à haute température
US3091548A (en) * 1959-12-15 1963-05-28 Union Carbide Corp High temperature coatings
US3758233A (en) * 1972-01-17 1973-09-11 Gen Motors Corp Vibration damping coatings
FR2190754A1 (de) * 1972-05-11 1974-02-01 Asahi Glass Co Ltd
WO1982001898A1 (en) * 1980-12-05 1982-06-10 Kvernes Ingard Method for coating a metal with a protection layer resistant to hot gas corrosion
CH648358A5 (en) * 1980-12-05 1985-03-15 Castolin Sa Process for producing a protective layer, resistant to corrosion by hot gas, on metal components

Non-Patent Citations (3)

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Title
PATENTS ABSTRACTS OF JAPAN, vol. 4, no. 174, 2nd December 1980; & JP - A - 55 113 880 (TOKYO SHIBAURA DENKI K.K.) 02-09-1980 *
PATENTS ABSTRACTS OF JAPAN, vol. 7, no. 139 (C-171)[1284], 17th June 1983; & JP - A - 58 52 469 (NIPPON KOKAN K.K.) 28-03-1983 *
SOVIET POWDER METALLURGY AND METAL CERAMICS, vol. 11, no. 3, March 1972, page 253, Consultants Bureau, New York, US; D.M. KARPINOS et al.: "Improving the adhesion of plasma-sprayed coatings to articles" *

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT396119B (de) * 1988-04-08 1993-06-25 Stangl Kurt Dipl Ing Verfahren zum beschriften heisser stahlbloecke
AT396120B (de) * 1988-04-13 1993-06-25 Stangl Kurt Dipl Ing Verfahren zum beschriften heisser stahlbloecke
EP0605196A1 (de) * 1992-12-29 1994-07-06 General Electric Company Verfahren zum Aufbringen einer Wärmedämmschicht
WO1996034128A1 (en) * 1995-04-25 1996-10-31 Siemens Aktiengesellschaft Metal substrate with an oxide layer and an anchoring layer
WO1998004759A1 (en) * 1996-04-12 1998-02-05 Siemens Aktiengesellschaft Metal substrate with an oxide layer and an improved anchoring layer
US6127048A (en) * 1996-07-25 2000-10-03 Siemens Aktiengesellschaft Article of manufacture having a metal substrate with an oxide layer and an improved anchoring layer and method of bonding the same
GB2380492A (en) * 2001-09-05 2003-04-09 Trw Ltd Friction member with graded coating
WO2004007787A1 (de) * 2002-07-17 2004-01-22 Siemens Aktiengesellschaft Schichtsystem
EP1382707A1 (de) * 2002-07-17 2004-01-21 Siemens Aktiengesellschaft Schichtsystem
US10385725B2 (en) 2012-08-07 2019-08-20 Safran Aircraft Engines Abradable coating made of a material having a low surface roughness
US10989066B2 (en) 2012-08-07 2021-04-27 Safran Aircraft Engines Abradable coating made of a material having a low surface roughness
DE102013213386B3 (de) * 2013-07-09 2014-08-14 MTU Aero Engines AG Strömungsmaschinen-Keramikbauteil
EP2824281A1 (de) * 2013-07-09 2015-01-14 MTU Aero Engines GmbH Strömungsmaschinen-Keramikbauteil
US10024192B2 (en) 2013-07-09 2018-07-17 MTU Aero Engines AG & Co. KG Ceramic component for a turbomachine
US10309002B2 (en) 2013-12-05 2019-06-04 General Electric Company Coating methods and a template for use with the coating methods
EP3133251A1 (de) * 2015-08-17 2017-02-22 United Technologies Corporation Äussere laufschaufelluftdichtungskomponente mit unterschiedlichen wärmeausdehnungskoeffizienten
EP3421732A3 (de) * 2017-06-30 2019-01-09 United Technologies Corporation Turbinenmotordichtung für umgebung mit hoher erosion
US10294962B2 (en) 2017-06-30 2019-05-21 United Technologies Corporation Turbine engine seal for high erosion environment

Also Published As

Publication number Publication date
EP0185603B1 (de) 1989-11-08
JPH0340105B2 (de) 1991-06-17
DE3574168D1 (en) 1989-12-14
JPS61153269A (ja) 1986-07-11

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