EP0217807B1 - Sintering method - Google Patents
Sintering method Download PDFInfo
- Publication number
- EP0217807B1 EP0217807B1 EP86901044A EP86901044A EP0217807B1 EP 0217807 B1 EP0217807 B1 EP 0217807B1 EP 86901044 A EP86901044 A EP 86901044A EP 86901044 A EP86901044 A EP 86901044A EP 0217807 B1 EP0217807 B1 EP 0217807B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- mixture
- produce
- intermetallic phases
- sintering
- ductility
- 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.)
- Expired - Lifetime
Links
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000005245 sintering Methods 0.000 title claims abstract description 13
- 239000000654 additive Substances 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 15
- 229910045601 alloy Inorganic materials 0.000 claims description 10
- 239000000956 alloy Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000001746 injection moulding Methods 0.000 claims description 4
- 229910000943 NiAl Inorganic materials 0.000 claims description 3
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000007493 shaping process Methods 0.000 claims description 2
- 230000004927 fusion Effects 0.000 claims 1
- 238000001513 hot isostatic pressing Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000010276 construction Methods 0.000 abstract 2
- 239000012190 activator Substances 0.000 abstract 1
- 239000011230 binding agent Substances 0.000 description 5
- 229910010038 TiAl Inorganic materials 0.000 description 4
- 239000000314 lubricant Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- CKQVRZJOMJRTOY-UHFFFAOYSA-N octadecanoic acid;propane-1,2,3-triol Chemical compound OCC(O)CO.CCCCCCCCCCCCCCCCCC(O)=O CKQVRZJOMJRTOY-UHFFFAOYSA-N 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 238000005275 alloying Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/09—Mixtures of metallic powders
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
Definitions
- the invention relates to a method for producing complex-shaped components from sinterable powder of the intermetallic phases TiAl, TiAl 3 or NiAl, Ni 3 Al.
- Sintering processes are known from the documents DE-C-897 921 and GB-A-2 131 457, in which intermetallic phases are first melted and comminuted as a master alloy and then pressed and sintered to form components with an addition of a soft metal powder such as aluminum powder especially withstand pressure and sliding loads.
- These sintering processes have the disadvantage that, owing to the high proportion of soft metal powder in the sintering mixture, no bodies can be sintered for high tensile stress.
- the intermetallic phases, TiAI, TiAI 3 or NiAI, Ni 3 AI have a low specific weight and a high melting point. Materials on this basis are therefore of interest for use in components that are subject to high thermal and mechanical loads, particularly in aircraft engines.
- the materials have so far been produced from the elements by melt metallurgy or by reaction, i.e. e.g. Al powder mixed with Ti powder and Nb powder and heated in a stamp press. When the chemical reaction begins, heat is generated and the desired alloy is formed. With this method it has so far not been possible to produce complicatedly shaped components in a simple manner.
- the object of the invention is to provide a method which makes it possible to produce components from intermetallic phases in a simple manner, which are complicated in shape and which are exposed to high tensile loads and high temperatures and / or chemical stresses during operation, and which allows them to be carried out in a simple manner Way to manufacture.
- a pre-alloy of the intermetallic phase TiAl, TiAl 3 or Ni 3 Al, NiA is assumed which, apart from inevitable impurities, contains only these. This master alloy is melted.
- the master alloy can be ground to a fine powder in a manner known per se (impact mill, ball mill, air jet mill) or atomized (as known per se, e.g. from DE-AS 22 22 830).
- This powder is now mixed with a powder of one or more other elements. It is desirable that these powders be finer than that of the intermetallic phase.
- those which cause an increase in the ductility of the intermetallic phase, namely B for Ni / Al or Nb for Ti / Al with a proportion of 0.5 to 10% by weight.
- Injection molding on the machines commonly used for plastics e.g. with a heated screw conveyor and a mouthpiece or nozzle at the tip of which also injection molding, extrusion, extrusion.
- Lubricants and binders are removed by heat treatment in a manner known per se (heat treatment under vacuum or inert gas up to 600 ° C).
- the sintering takes place in the same atmosphere as the above heat treatment and under conditions known per se, in particular at temperatures above 900 ° C., but less than 95% of the melting temperature.
- the sintering can also take place in several stages.
- the elements B and Nb which were added to increase the ductility also act as a sintering aid, so that sintering can be carried out at a temperature of 70 to 95% (by weight) of the absolute melting point of the intermetallic phase.
- densities of 95 to 99% of the theoretical density are within 0.1 to 24 h reached.
- HIP conditions are also known per se, pressures up to approximately 2500 bar (gas) and temperatures up to approximately 2000 ° C.
- components such as Turbine blades or wheels, turbochargers or other highly stressed parts (hot, rotating and / or chemically stressed), in particular manufactured by turbomachines.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren zur Herstellung von kompliziert geformten Bauteilen aus sinterfähigem Pulver der intermetallischen Phasen TiAl, TiAl3 bzw. NiAl, Ni3Al.The invention relates to a method for producing complex-shaped components from sinterable powder of the intermetallic phases TiAl, TiAl 3 or NiAl, Ni 3 Al.
Aus den Druckschriften DE-C-897 921 und GB-A-2 131 457 sind Sinterverfahren bekannt, bei denen zunächst intermetallische Phasen erschmolzen und als Vorlegierung zerkleinert werden und anschließend mit einem Zusatz von einem Weichmetallpulver wie Aluminiumpulver zu Bauteilen gepreßt und gesintert werden, die besonders Druck- und Gleitbeanspruchungen standhalten. Diese Sinterverfahren haben den Nachteil, daß durch den hohen Anteil an Weichmetallpulver im Sintergemisch keine Körper für hohe Zugbeanspruchung gesintert werden können.Sintering processes are known from the documents DE-C-897 921 and GB-A-2 131 457, in which intermetallic phases are first melted and comminuted as a master alloy and then pressed and sintered to form components with an addition of a soft metal powder such as aluminum powder especially withstand pressure and sliding loads. These sintering processes have the disadvantage that, owing to the high proportion of soft metal powder in the sintering mixture, no bodies can be sintered for high tensile stress.
Die intermetallischen Phasen, TiAI, TiAI3 bzw. NiAI, Ni3AI weisen ein geringes spezifisches Gewicht und einen hohen Schmelzpunkt auf. Werkstoffe auf dieser Basis sind daher für den Einsatz in thermisch und mechanisch hoch belasteten Bauteilen, insbesondere in Flugtriebwerken, interessant.The intermetallic phases, TiAI, TiAI 3 or NiAI, Ni 3 AI have a low specific weight and a high melting point. Materials on this basis are therefore of interest for use in components that are subject to high thermal and mechanical loads, particularly in aircraft engines.
Die Problematik dieser Werkstoffe liegt in ihrer Sprödigkeit. Seit einiger Zeit sind Verfahren bekannt, um die Duktilität der intermetallischen Phasen zu steigern. Dies geschieht durch Zulegieren eines weiteren Elements, z.B. von Nb in TiAI3 oder von B in NiAl.The problem with these materials is their brittleness. Methods for increasing the ductility of the intermetallic phases have been known for some time. This is done by alloying another element, for example Nb in TiAI 3 or B in NiAl.
Die Werkstoffe werden bisher schmelzmetallurgisch oder durch Reaktion aus den Elementen hergestellt, d.h. es wird z.B. AI-Pulver- mit Ti-Pulver und Nb-Pulver gemischt und in einer Stempelpresse erhitzt. Bei der einsetzenden chemischen Reaktion entsteht Wärme und es bildet sich die gewünschte Legierung. Mit diesem Verfahren ist es bisher nicht möglich, auf einfache Weise kompliziert geformte Bauteile herzustellen.The materials have so far been produced from the elements by melt metallurgy or by reaction, i.e. e.g. Al powder mixed with Ti powder and Nb powder and heated in a stamp press. When the chemical reaction begins, heat is generated and the desired alloy is formed. With this method it has so far not been possible to produce complicatedly shaped components in a simple manner.
Aufgabe der Erfindung ist es, ein Verfahren anzugeben, das es gestattet, auf einfache Weise Bauteile aus intermetallischen Phasen herzustellen, die kompliziert geformt sind und die im Betrieb hohen Zugbelastungen sowie hohen Temperaturen und/oder chemischen Beanspruchungen ausgesetzt sind und das es gestattet diese auf einfache Weise herzustellen.The object of the invention is to provide a method which makes it possible to produce components from intermetallic phases in a simple manner, which are complicated in shape and which are exposed to high tensile loads and high temperatures and / or chemical stresses during operation, and which allows them to be carried out in a simple manner Way to manufacture.
Gelöst wird diese Aufgabe durch ein Verfahren mit folgenden Verfahrensschritten:
- a) Erschmelzen einer Vorlegierung der intermetallischen Phasen TiAI, TiAI3 bzw. NiAI, Ni3AI,
- b) Zerkleinern der Vorlegierung zu einem feinen Pulver,
- c) Mischen mit den Duktilisierungszusätzen Nb bzw. B die 0,5 bis 10 Gew.-% der intermetallischen Phasen Ti/AI bzw. Ni/AI ausmachen und gleichzeitig eine Sinterhilfe darstellen,
- d) Formgebung des Gemisches,
- e) Sintern bei einer Temperatur von 70 bis 95% des absoluten Schmelzpunktes der intermetallischen Phase zu einem nachpreßbaren Bauteil gesteigerter Duktilität und einer Dichte von größer als 95% der theoretischen Dichte.
- a) melting of a master alloy of the intermetallic phases TiAI, TiAI 3 or NiAI, Ni 3 AI,
- b) grinding the master alloy into a fine powder,
- c) Mixing with the ductility additives Nb or B which make up 0.5 to 10% by weight of the intermetallic phases Ti / AI or Ni / AI and at the same time represent a sintering aid,
- d) shaping of the mixture,
- e) Sintering at a temperature of 70 to 95% of the absolute melting point of the intermetallic phase to a repressable component of increased ductility and a density of greater than 95% of the theoretical density.
Ausgegangen wird von einer Vorlegierung der intermetallischen Phase TiAl, TiAl3 bzw. Ni3Al, NiA die abgesehen von unvermeidlichen Verunreinigungen nur diese enthält. Diese Vorlegierung wird erschmolzen.A pre-alloy of the intermetallic phase TiAl, TiAl 3 or Ni 3 Al, NiA is assumed which, apart from inevitable impurities, contains only these. This master alloy is melted.
Wegen der Sprödigkeit der intermetallischen Phase läßt sich die Vorlegierung in an sich bekannter Weise zu einem feinen Pulver vermahlen (Prallmühle, Kugelmühle, Luftstrahlmühle) oder verdüsen (wie an sich bekannt, z.B. aus der De-AS 22 22 830).Because of the brittleness of the intermetallic phase, the master alloy can be ground to a fine powder in a manner known per se (impact mill, ball mill, air jet mill) or atomized (as known per se, e.g. from DE-AS 22 22 830).
Korngrößenbereich:
- 0,5 µm bis 50 µm, spez. Oberfläche 1m2/g bis 25m2/g.
- 0.5 µm to 50 µm, spec. Surface 1m 2 / g to 25 m2 / g.
Bevorzugt:
- 3 bis 5m2/g (BET-Oberfläche).
- 3 to 5m 2 / g (BET surface area).
Dieses Pulver wird nun mit einem Pulver von einem oder mehreren weiteren Elementen vermischt. Dabei ist es wünschenswert, daß diese Pulver feiner sind als das der intermetallischen Phase.This powder is now mixed with a powder of one or more other elements. It is desirable that these powders be finer than that of the intermetallic phase.
Als weitere Elemente werden solche verwendet, die eine Zunahme der Duktilität der intermetallischen Phase bewirken und zwar B für Ni/AI bzw. Nb für Ti/AI mit einem Anteil von 0,5 bis 10 Gew.-%.As further elements, those are used which cause an increase in the ductility of the intermetallic phase, namely B for Ni / Al or Nb for Ti / Al with a proportion of 0.5 to 10% by weight.
Die aufbereitete Pulvermischung kann nun, abgesehen von einem Schrumpfmaß von 10 bis 20% (Vol.) mit bekannten Methoden auf die Endform gebracht werden:
- a) Versehen mit einem Bindemittel, kaltisostatisches (CIP) Pressen, Bearbeiten im Grünzustand
- Bindemittel: Wachse, Thermoplaste und/oder Duroplaste CIP siehe z.B. DE 33 28 954
- Bearbeiten durch Schleifen und Polieren auf Endmaße,
- b) Aufbereiten einer spritzgußfähigen Masse mit Hilfe von Gleit- und Bindemitteln, kunststofftechnologisches Spritzgießen.
- Austreibbares Bindemittel wie in a)
- Gleitmittel wie Stearine.
- a) Provided with a binder, cold isostatic (CIP) pressing, processing in the green state
- Binder: waxes, thermoplastics and / or thermosets CIP see e.g. DE 33 28 954
- Machining by grinding and polishing to final dimensions,
- b) Preparation of an injection-moldable mass with the help of lubricants and binders, plastic technology injection molding.
- Expelling binder as in a)
- Lubricants such as stearine.
Spritzgießen auf den für Kunststoffe üblichen Maschinen (z.B. mit beheizbarer Förderschnecke und Mundstück bzw. Düse an deren Spitze auch Spritzpressen, Strangpressen, Extrudieren.Injection molding on the machines commonly used for plastics (e.g. with a heated screw conveyor and a mouthpiece or nozzle at the tip of which also injection molding, extrusion, extrusion.
Dabei werden Gleit- und Bindemittel durch eine Wärmebehandlung in an sich bekannter Weise entfernt (Wärmebehandlung unter Vakuum oder Inertgas bis 600°C). Das Sintern erfolgt in der gleichen Atmosphäre wie die vorstehende Wärmebehandlung und unter an sich bekannten Bedingungen, insbesodere bei Temperaturen über 900°C, jedoch kleiner als 95% der Schmelztemperatur. Das Sintern kann auch mehrstufig erfolgen.Lubricants and binders are removed by heat treatment in a manner known per se (heat treatment under vacuum or inert gas up to 600 ° C). The sintering takes place in the same atmosphere as the above heat treatment and under conditions known per se, in particular at temperatures above 900 ° C., but less than 95% of the melting temperature. The sintering can also take place in several stages.
Die Elemente B bzw. Nb die zur Steigerung der Duktilität zugegeben wurden, wirken zugleich als Sinterhilfe, so daß sich bei einer Temperatur von 70 bis 95% (Gew.) des absoluten Schmelzpunktes der intermetallischen Phase eine Sinterung durchführen läßt. Hierbei werden Dichten von 95 bis 99% der theoretischen Dichte innerhalb von 0,1 bis 24 h erreicht.The elements B and Nb which were added to increase the ductility also act as a sintering aid, so that sintering can be carried out at a temperature of 70 to 95% (by weight) of the absolute melting point of the intermetallic phase. Here densities of 95 to 99% of the theoretical density are within 0.1 to 24 h reached.
Anschließend können die Teile noch heißisostatisch gepreßt werden, um praktisch 100% Dichte zu erzielen. Diese HIP-Bedingungen sind ebenfalls an sich bekannt, Drücke bis etwa 2500 bar (Gas) und Temperaturen bis etwa 2000°C.The parts can then be hot isostatically pressed to achieve practically 100% density. These HIP conditions are also known per se, pressures up to approximately 2500 bar (gas) and temperatures up to approximately 2000 ° C.
Mit diesen Verfahren werden Bauteile wie z.B. Turbinenschaufeln oder -räder, Turbo-Lader oder andere hochbeanspruchte Teile (heiß, rotierend und/oder chemisch beansprucht), insbesondere von Strömungsmaschinen hergestellt.With these processes, components such as Turbine blades or wheels, turbochargers or other highly stressed parts (hot, rotating and / or chemically stressed), in particular manufactured by turbomachines.
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT86901044T ATE51548T1 (en) | 1985-02-16 | 1986-02-07 | SINTERING PROCESS. |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3505481 | 1985-02-16 | ||
| DE19853505481 DE3505481A1 (en) | 1985-02-16 | 1985-02-16 | SINTER PROCEDURE |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0217807A1 EP0217807A1 (en) | 1987-04-15 |
| EP0217807B1 true EP0217807B1 (en) | 1990-04-04 |
Family
ID=6262782
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP86901044A Expired - Lifetime EP0217807B1 (en) | 1985-02-16 | 1986-02-07 | Sintering method |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US4707332A (en) |
| EP (1) | EP0217807B1 (en) |
| JP (1) | JPS62501858A (en) |
| DE (2) | DE3505481A1 (en) |
| WO (1) | WO1986004840A1 (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3822686A1 (en) * | 1988-07-05 | 1990-01-11 | Geesthacht Gkss Forschung | METHOD FOR PRODUCING INTERMETALLIC PHASES FROM POWDER-SHAPED DUCTILE COMPONENTS |
| US4927458A (en) * | 1988-09-01 | 1990-05-22 | United Technologies Corporation | Method for improving the toughness of brittle materials fabricated by powder metallurgy techniques |
| DE3935955C1 (en) * | 1989-10-27 | 1991-01-24 | Mtu Muenchen Gmbh | |
| SE9100675D0 (en) * | 1991-03-06 | 1991-03-06 | Sandvik Ab | CERAMIC WHISKER-REINFORCED CUTTING TOOL WITH PRE-FORMED CHIPBREAKERS FOR MACHINING |
| JP3071118B2 (en) * | 1995-02-09 | 2000-07-31 | 日本原子力研究所 | Method for producing NiAl intermetallic compound to which fine additive element is added |
| DE19537657A1 (en) * | 1995-10-10 | 1997-04-17 | Abb Patent Gmbh | Method and device for producing a contact piece |
| US20100178194A1 (en) * | 2009-01-12 | 2010-07-15 | Accellent, Inc. | Powder extrusion of shaped sections |
| US9061351B2 (en) * | 2011-11-10 | 2015-06-23 | GM Global Technology Operations LLC | Multicomponent titanium aluminide article and method of making |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE897921C (en) * | 1938-02-13 | 1953-11-26 | Metallgesellschaft Ag | Process for the production of bearings from aluminum and its alloys by pressing and sintering the powdery components |
| FR1290458A (en) * | 1960-05-14 | 1962-04-13 | Siemens Ag | Manufacturing process of sintered thermoelectric materials |
| NL268504A (en) * | 1961-01-09 | |||
| DE2258780A1 (en) * | 1971-12-14 | 1973-06-28 | Goldschmidt Ag Th | PROCESS FOR PRODUCING PERMANENT MAGNETS BASED ON COBALT-RARE EARTH ALLOYS |
| DE2227700A1 (en) * | 1972-06-07 | 1974-01-03 | Gen Electric | Stable permanent magnets - sintered cobalt rare earth intermetallic prods |
| US3953205A (en) * | 1973-06-06 | 1976-04-27 | United Technologies Corporation | Production of homogeneous alloy articles from superplastic alloy particles |
| US4347076A (en) * | 1980-10-03 | 1982-08-31 | Marko Materials, Inc. | Aluminum-transition metal alloys made using rapidly solidified powers and method |
| FR2537655A1 (en) * | 1982-12-09 | 1984-06-15 | Cegedur | ENGINE SHAPES BASED ON ALUMINUM ALLOYS AND INTERMETALLIC COMPOUNDS AND METHODS FOR OBTAINING THEM |
| US4624705A (en) * | 1986-04-04 | 1986-11-25 | Inco Alloys International, Inc. | Mechanical alloying |
-
1985
- 1985-02-16 DE DE19853505481 patent/DE3505481A1/en not_active Withdrawn
-
1986
- 1986-02-07 DE DE8686901044T patent/DE3670016D1/en not_active Expired - Lifetime
- 1986-02-07 WO PCT/DE1986/000044 patent/WO1986004840A1/en active IP Right Grant
- 1986-02-07 EP EP86901044A patent/EP0217807B1/en not_active Expired - Lifetime
- 1986-02-07 JP JP61501038A patent/JPS62501858A/en active Pending
- 1986-02-07 US US07/002,403 patent/US4707332A/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62501858A (en) | 1987-07-23 |
| EP0217807A1 (en) | 1987-04-15 |
| US4707332A (en) | 1987-11-17 |
| DE3505481A1 (en) | 1986-08-28 |
| WO1986004840A1 (en) | 1986-08-28 |
| DE3670016D1 (en) | 1990-05-10 |
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