EP0083043A1 - Wearing part - Google Patents
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- EP0083043A1 EP0083043A1 EP82111762A EP82111762A EP0083043A1 EP 0083043 A1 EP0083043 A1 EP 0083043A1 EP 82111762 A EP82111762 A EP 82111762A EP 82111762 A EP82111762 A EP 82111762A EP 0083043 A1 EP0083043 A1 EP 0083043A1
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- layer
- layers
- wearing part
- boron
- titanium
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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
- C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
- C23C30/005—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process on hard metal substrates
Definitions
- the invention relates to a wearing part, in particular a hard metal cutting insert for machining, with a multilayer hard material coating, at least one layer being designed as an oxide layer.
- Such a wear part is known from DE-AS 22 53 745, the inner layer of the carbide base body which is initially located and consists of one or more carbides and / or nitrides of the elements Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Si and / or B and whose outer layer consists of one or more extremely wear-resistant deposits made of aluminum oxide and / or zirconium oxide.
- a disadvantage of this wearing part is that cracks can occur in the pure oxide cover layers and that in many cases the oxide layers have an insufficient adhesive strength and flake off.
- the brittleness of the oxide layer increases rapidly with increasing layer thickness.
- the structure changes very disadvantageously, so that in practice such wear parts require the use of a comparatively very thin layer of a few micrometers in thickness is limited or a thicker layer has no additional advantages; wrestles. This in turn decisively limits the service life of wearing parts, for example indexable inserts for cutting machining newspapers.
- DE-OS 23 17 447 which represents an additional application to DE-AS 22 53 745 mentioned at the outset, describes a wearing part whose outer cover layer consists of one or more deposits of Kerawian oxides, the oxides in particular being in addition to the oxides mentioned in the main patent the elements Si, B, Ca, Mg, Ti and / or Hf are enumerated and the formation of mixed oxides is generally included in the application. Individual mixed oxides are not particularly emphasized.
- DE-AS 28 51 584 discloses a composite body, preferably with a hard metal base body, in which one or more layers of one or more carbides and / or nitrides of the elements Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Si, B and on this layer or layers one or more layers of a mixture of at least one oxide and at least one nitride and / or of at least one oxynitride of the elements Cr, Al, Ca, Mg , Th, Sc, Y, La, Ti, Hf, V, Nb, Ta are arranged, the nitrogen content of the outermost layer being 0.1 to 30 atom%, preferably 0.2 to 15 atom%.
- the only example describes the following layer structure on hard metal: TiC, 4 / um + Al 2 O 2.8 N 0.2 , 2 - 3 / um.
- the object on which the invention is based is to create a wearing part, in particular a hard metal cutting insert for machining with a multilayer hard material coating, at least one layer being embodied as an oxide layer, which has improved wear resistance and improved wear compared to known wearing parts Has adhesive strength of the hard material coating.
- the coating applied directly or via an underlayer on the base body consists of one or more layers of oxycarbides and / or oxycarbonitrides and / or oxynitrides and / or oxiborides and / or oxibornitrides and / or oxiborocarbonitrides of the elements Ti , Zr, Hf, B, Si, Al with an oxygen content of 0.1 to 5 wt.% Each alternating with one or more layers of aluminum-boron mixed oxides with boron contents of 0.01 to 1 wt.% .
- the wearing part according to the invention has a significantly increased wear resistance as well as an excellent adhesive strength of the hard material coating compared to known multi-layer coated wearing parts, so that the service life of the wearing part is considerably increased.
- These unexpectedly good properties are achieved by the incorporation of boron in the aluminum oxide layers with the simultaneous incorporation of oxygen components in the oxycarbide, oxycarbonitride, oxynitride, oxiboride, oxibornitride and oxiborocarbonitride intermediate layers.
- the oxygen and boron contents of the individual layers are within the specified limits. Below 0.1% by weight, the influence of oxygen can practically no longer be determined. At higher oxygen contents than in the specified range, the hardness of the intermediate layers drops very quickly and does not increase the wear resistance of the layer structure according to the invention. Likewise, only a boron content within the limits according to the invention in aluminum oxide leads to an abrupt increase in wear resistance. On the contrary, it was not even to be expected that the addition of boron to aluminum oxide could lead to an increase in wear resistance, since pure boron oxide is very soft and completely unsuitable as a wear protection layer.
- the boron content within the specified limits causes the deposition of the aluminum-boron mixed oxide layer, less dust is generated in the coating chamber and thus also on the surface of the coating material. This results in fewer shift errors and more even shifts.
- an underlayer between the base body and the cover according to the invention.
- This underlayer preferably has a single or multi-layer structure consisting of one or more carbides, nitrides, carbonitrides, borides or boron nitrides of the elements of IV. To VI. Group of the periodic table.
- titanium oxycarbonitride and / or titanium oxynitride with a layer thickness of 0.05 to 1 ⁇ m directly on a base body made of hard metal or over an underlayer and then a single aluminum-boron mixed oxide layer with a layer Layer thickness from 2 to 10 / to apply.
- a particularly preferred embodiment of the invention provides that a coating consisting of a layer of titanium oxycarbonitride and / or titanium oxynitride with a layer thickness of 0.1 to 1 .mu.m and then of 2 to 8 aluminum-boron mixed oxide layers with layer thicknesses of 0.3 to 2 / um in alternation with 1 to 7 layers of titanium oxycarbonitride and / or titanium oxynitride with layer thicknesses of 0.05 to 0.5 / um are applied.
- the titanium oxycarbonitride and / or titanium oxynitride layers preferably have an oxygen content of 0.5 to 3% by weight, while the aluminum-boron mixed oxide layers preferably have a boron content of 0.2 to 2% by weight.
- this multilayered layer structure according to the invention leads to a further increase in the toughness of the coating with an excellent adhesive strength of the individual layers and thus to an unexpected increase in the wear resistance under impact stress compared to a layer structure according to the invention which contains only one aluminum-boron mixed oxide layer of the wearing part.
- a particularly preferred backing comprises of a base body of hard metal, starting the layer sequence titanium carbide and / or titanium carbonitride and / or titanium nitride having a total layer thickness of 1 to 10 / .mu.m.
- the aluminum-boron mixed oxides partially contain titanium, zirconium, hafnium, niobium, chromium and / or magnesium oxides.
- the mixed oxides can also have a nitrogen content of 0.2 to 4 atom%.
- the hard material coating of the wearing part according to the invention is preferably carried out by the CVD method, the chemical composition of the individual layers being determined by appropriate mixing ratios of the reaction gases.
- Another preferred method for producing the wearing part according to the invention is that the individual layers of appropriate chemical composition are produced both by deposition using the CVD method and by interdiffusion between adjacent layers.
- the introduction of the oxygen fractions into the oxycarbide, oxycarbonitride, oxynitride, oxiboride, oxibornitride and / or oxiborocarbonitride layers can take place both via an appropriate gas mixture composition, for example C0 2 H 2 O vapor, air, 0 2 or contain other oxidizing gases, as well as by interdiffusion from the adjacent aluminum-boron mixed oxide layers.
- This interdiffusion can be carried out, for example, by a temperature treatment between or after the individual coating runs at a temperature which is above the coating temperature, or during the coating travel of the aluminum-boron mixed oxide layers by means of an increased supply of oxygen in the gas mixture.
- indexable inserts made of hard metal of the U10T grade / composition 6% Co, 5% TiC, 5% (TaC + NbC), 84% WC coatings corresponded to ISO application group M10 / and the shape SPGN 120308 EN in 5 different layer construction variants applied according to the table below.
- the indexable inserts were cleaned, installed in the coating chamber of a prototype system from the applicant, heated to the coating temperature under protective gas and coated under the following coating conditions.
- Variants 4 and 5 are provided with a layer structure according to the invention. These variants are compared with variants 1 to 3, which have a layer structure which differs from the invention and is known in one case, in a machining test.
- Al 2 O 3 layer or Al-B mixed oxide layer Al 2 O 3 layer or Al-B mixed oxide layer:
- the wear mark width v B of the flank wear was measured after a rotation time of 5 min.
- Example 2 In contrast to Example 1, the single-layer Al 2 0 3 or aluminum-boron mixed oxide layer is replaced by 4 layers which are connected by 3 Ti (C, N) or 3 Ti (C, N, 0) intermediate layers .
- Al 2 O 3 layers or aluminum-boron mixed oxide layers are Al 2 O 3 layers or aluminum-boron mixed oxide layers:
- the multilayer structure of the aluminum oxide or aluminum-boron mixed oxide layer according to Example 2 compared to the single-layer structure according to Example 1 shows a further increase in wear resistance can be achieved.
- the increase in wear resistance in the layer structure according to the invention is substantially greater than in the layer structure according to variants 1 to 3.
- a Ti (C 0.6 , N 0.4 ) layer was deposited on indexable inserts of the same type as in Example 1 and a TiN layer was deposited thereon.
- the further layer structure was carried out in two variants, variant 2 representing a layer structure according to the invention.
- the coating was carried out under reduced pressure. The wear resistance of the individual variants was again compared with one another in a machining test.
- hard metal was used as the base body.
- the invention is not limited to hard metal base bodies.
- the layer structure according to the invention also leads to other base materials such as with high-speed steel, stellite or other heat-resistant alloys to an unexpectedly large increase in wear resistance.
- the invention is not limited to machining tools. Rather, it also extends to tools for non-cutting machining, such as drawing dies and the like, and to tools which are mainly exposed to erosive wear, such as Rock drilling.
Abstract
Ein Verschleißteil, insbesondere ein Hartmetall-Schneideinsatz zur spanabhebenden Bearbeitung, ist mit einem mehrschichtigen Hartstoffüberzug versehen. Der unmittelbar oder über eine Unterlagsschicht auf dem Grundkörper aufgebrachte Überzug besteht aus je einer oder mehreren Schichten von Oxikarbiden und/oder Oxikarbonitriden und/oder Oxinitriden und/oder Oxiboriden und/oder Oxibornitriden und/oder Oxiborkarbonitriden der Elemente Ti, Zr, Hf, B, Si, Al mit einem Sauerstoff-Gehalt von 0,1 bis 5 Gew.%, die jeweils im Wechsel mit einer oder mehreren Schichten von Aluminium-Bor-Mischoxiden mit Bor-Gehalten von 0,01 bis 1 Gew.% aufgebracht werden. Das Verschleißteil weist gegenüber bekannten mehrlagig beschichteten Verschleißteilen eine wesentlich höhere Verschleißfestigkeit sowie eine ausgezeichnete Haftfestigkeit der Hartstoff-Beschichtung auf.A wearing part, in particular a hard metal cutting insert for machining, is provided with a multi-layer hard material coating. The coating applied directly or via an underlayer to the base body consists of one or more layers of oxycarbides and / or oxycarbonitrides and / or oxynitrides and / or oxiborides and / or oxibornitrides and / or oxiborocarbonitrides of the elements Ti, Zr, Hf, B, Si, Al with an oxygen content of 0.1 to 5% by weight, which are applied alternately with one or more layers of aluminum-boron mixed oxides with boron contents of 0.01 to 1% by weight. Compared to known multi-layer coated wear parts, the wear part has a significantly higher wear resistance and an excellent adhesive strength of the hard material coating.
Description
Die Erfindung betrifft ein Verschleißteil, insbesondere einen Hartmetall-Schneideinsatz zur spanabhebenden Bearbeitung, mit einem mehrschichtigen Hartstoff-Überzug, wobei mindestens eine Schicht als Oxidschicht ausgeführt ist.The invention relates to a wearing part, in particular a hard metal cutting insert for machining, with a multilayer hard material coating, at least one layer being designed as an oxide layer.
Aus der DE-AS 22 53 745 ist ein derartiges Verschleißteil bekannt, dessen dem Hartmetall-Grundkörper zunächst liegende innere Schicht aus einem oder mehreren Karbiden und/oder Nitriden der Elemente Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Si und/oder B besteht und dessen äußere Schicht aus einer oder mehreren extrem verschleißfesten Ablagerungen aus Aluminium-Oxid und/oder Zirkon-Oxid besteht.Such a wear part is known from DE-AS 22 53 745, the inner layer of the carbide base body which is initially located and consists of one or more carbides and / or nitrides of the elements Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Si and / or B and whose outer layer consists of one or more extremely wear-resistant deposits made of aluminum oxide and / or zirconium oxide.
Nachteilig bei diesem Verschleißteil ist, daß es in den reinen Oxid-Deckschichten zu Rissen kommen kann und daß die Oxid-Schichten in vielen Fällen eine ungenügende Haftfestigkeit aufweisen und abplatzen. Die Sprödigkeit der Oxidschicht nimmt mit wachsender Schichtdicke rasch zu. Dabei verändert sich das Gefüge sehr nachteilig, so daß man bei derartigen Verschleißteilen in der Praxis auf die Verwendung einer vergleichsweise sehr dünnen Schicht von wenigen Mikrometern Dicke beschränkt ist bzw. eine dickere Schicht keine zusätzlichen Vorteile ;ringt. Dieser Umstand beschränkt wiederum die Standzeit von Verschleißteilen, z.B. von Wendeschneidplatten zur spanabhebenden Bearzeitung, entscheidend.A disadvantage of this wearing part is that cracks can occur in the pure oxide cover layers and that in many cases the oxide layers have an insufficient adhesive strength and flake off. The brittleness of the oxide layer increases rapidly with increasing layer thickness. The structure changes very disadvantageously, so that in practice such wear parts require the use of a comparatively very thin layer of a few micrometers in thickness is limited or a thicker layer has no additional advantages; wrestles. This in turn decisively limits the service life of wearing parts, for example indexable inserts for cutting machining newspapers.
In der DE-OS 23 17 447, die eine Zusatzanmeldung zur eingangs erwähnten DE-AS 22 53 745 darstellt, ist ein Verschleißteil beschrieben, dessen äußere Deckschicht aus einer oder mehreren Ablagerungen kerawischer Oxide besteht, wobei neben den im Hauptpatent genannten Oxiden insbesondere die Oxide der Elemente Si, B, Ca, Mg, Ti und/oder Hf aufgezählt sind und auch die Ausbildung von Mischoxiden in der Anmeldung allgemein mit eingeschlossen ist. Einzelne Mischoxide sind nicht besonders hervorgehoben.DE-OS 23 17 447, which represents an additional application to DE-AS 22 53 745 mentioned at the outset, describes a wearing part whose outer cover layer consists of one or more deposits of Kerawian oxides, the oxides in particular being in addition to the oxides mentioned in the main patent the elements Si, B, Ca, Mg, Ti and / or Hf are enumerated and the formation of mixed oxides is generally included in the application. Individual mixed oxides are not particularly emphasized.
Soweit zu einzelnen Ausgestaltungsmöglichkeiten praktische Erfahrungen vorliegen, ist auch in diesen Fällen das Auftreten von Rissen und die Haftfestigkeit der Oxid-Deckschichten nicht zufriedenstellend.Insofar as there is practical experience with individual design options, the occurrence of cracks and the adhesive strength of the oxide cover layers are also unsatisfactory in these cases.
Aus der DE-AS 28 51 584 ist ein Verbundkörper, vorzugsweise mit einem Hartmetall-Grundkörper bekannt, bei dem auf dem Grundkörper eine oder mehrere Schichten aus einem oder mehreren Karbiden und/oder Nitriden der Elemente Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Si, B und auf dieser Schicht bzw. Schichten eine oder mehrere Schichten aus einem Gemenge von mindestens einem Oxid und mindestens einem Nitrid und/oder aus mindestens einem Oxinitrid der der Elemente Cr, Al, Ca, Mg, Th, Sc, Y, La, Ti, Hf, V, Nb, Ta angeordnet sind, wobei der Stickstoff-Gehalt der äußersten Schicht 0,1 bis 30 Atom %, vorzugsweise 0,2 bis 15 Atom % beträgt. Das einzige Beispiel beschreibt folgenden Schichtaufbau auf Hartmetall: TiC, 4/um + Al2O2,8N0,2, 2 - 3/um.DE-AS 28 51 584 discloses a composite body, preferably with a hard metal base body, in which one or more layers of one or more carbides and / or nitrides of the elements Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Si, B and on this layer or layers one or more layers of a mixture of at least one oxide and at least one nitride and / or of at least one oxynitride of the elements Cr, Al, Ca, Mg , Th, Sc, Y, La, Ti, Hf, V, Nb, Ta are arranged, the nitrogen content of the outermost layer being 0.1 to 30 atom%, preferably 0.2 to 15 atom%. The only example describes the following layer structure on hard metal: TiC, 4 / um + Al 2 O 2.8 N 0.2 , 2 - 3 / um.
In der Praxis wurden vor allem Hartmetall-Verschleißteile bekannt, bei denen die äußere Schicht aus sehr vielen Lagen von abwechselnd Ti(C,N) und A12(O,N) besteht, wobei diese Ausführung zusätzlich in den Schutzumfang der DE-AS 29 17 348 fällt.In practice, hard metal wear parts have become known, in which the outer layer consists of a large number of layers of alternating Ti (C, N) and A1 2 (O, N) 17 348 falls.
Auch bei diesem Verbundkörper sind die erzielbaren Verschleißfestigkeiten für viele Anwendungsfälle nicht befriedigend. Zudem ist eine zu große Anzahl von einzelnen Lagen - das einzige Beispiel der DE-AS 29 17 348 beschreibt 38 Einzellagen - in der Fertigung nicht mehr wirtschaftlich.With this composite body too, the achievable wear resistance is unsatisfactory for many applications. In addition, a too large number of individual layers - the only example of DE-AS 29 17 348 describes 38 individual layers - is no longer economical to manufacture.
Die der Erfindung zugrunde liegende Aufgabe liegt nun darin, ein Verschleißteil, insbesondere einen Hartmetall-Schneideinsatz zur spanabhebenden Bearbeitung mit einem mehrschichtigen Hartstoff-Überzug, wobei mindestens eine Schicht als Oxidschicht ausgeführt ist, zu schaffen, das gegenüber bekannten Verschleißteilen eine verbesserte Verschleißfestigkeit und eine verbesserte Haftfestigkeit der Hartstoff-Beschichtung aufweist.The object on which the invention is based is to create a wearing part, in particular a hard metal cutting insert for machining with a multilayer hard material coating, at least one layer being embodied as an oxide layer, which has improved wear resistance and improved wear compared to known wearing parts Has adhesive strength of the hard material coating.
Diese Aufgabe wird erfindungsgemäß dadurch gelöst, daß der unmittelbar oder über eine Unterlagsschicht auf dem Grundkörper aufgebrachte Überzug aus je einer oder mehreren Schichten von Oxikarbiden und/oder Oxikarbonitriden und/oder Oxinitriden und/oder Oxiboriden und/oder Oxibornitriden und/oder Oxiborkarbonitriden der Elemente Ti, Zr, Hf, B, Si, Al mit einem Sauerstoffgehalt von 0,1 bis 5 Gew.% jeweils im Wechsel mit einer oder mehreren Schichten von Aluminium-Bor-Mischoxiden mit Bor-Gehalten von 0,01 bis 1 Gew.% besteht.This object is achieved according to the invention in that the coating applied directly or via an underlayer on the base body consists of one or more layers of oxycarbides and / or oxycarbonitrides and / or oxynitrides and / or oxiborides and / or oxibornitrides and / or oxiborocarbonitrides of the elements Ti , Zr, Hf, B, Si, Al with an oxygen content of 0.1 to 5 wt.% Each alternating with one or more layers of aluminum-boron mixed oxides with boron contents of 0.01 to 1 wt.% .
Das erfindungsgemäße Verschleißteil weist gegenüber bekannten mehrlagig beschichteten Verschleißteilen eine wesentlich erhöhte Verschleißfestigkeit sowie eine ausgezeichnete Haftfestigkeit der Hartstoff-Beschichtung auf, so daß sich erheblich vergrößerte Standzeiten des Verschleißteiles ergeben. Diese unerwartet guten Eigenschaften werden durch den Einbau von Bor in die Aluminiumoxid-Schichten bei gleichzeitigem Einbau von Sauerstoff-Anteilen in die Oxikarbid-, Oxikarbonitrid-, Oxinitrid-, Oxiborid-, Oxibornitrid- und Oxiborkarbonitrid-Zwischenschichten erreicht. Es war insbesondere völlig überraschend - wie nachfolgend an Hand der Beispiele belegt wird - daß lediglich der gleichzeitige Einbau der Sauerstoff-Anteile in den Zwischenschichten und des Bors in den Aluminiumoxid-Schichten eine wesentliche Steigerung der Verschleißfestigkeit bewirkte.The wearing part according to the invention has a significantly increased wear resistance as well as an excellent adhesive strength of the hard material coating compared to known multi-layer coated wearing parts, so that the service life of the wearing part is considerably increased. These unexpectedly good properties are achieved by the incorporation of boron in the aluminum oxide layers with the simultaneous incorporation of oxygen components in the oxycarbide, oxycarbonitride, oxynitride, oxiboride, oxibornitride and oxiborocarbonitride intermediate layers. In particular, it was completely surprising - as will be demonstrated below using the examples - that only the simultaneous incorporation of the oxygen fractions in the intermediate layers and of the boron in the aluminum oxide layers brought about a substantial increase in the wear resistance.
Es ist dabei wichtig, daß die Sauerstoff- und Bor-Gehalte der einzelnen Schichten innerhalb der angegebenen Grenzen liegen. Unterhalb 0,1 Gew.% ist der Einfluß des Sauerstoffs praktisch nicht mehr feststellbar. Bei höheren Sauerstoff-Gehalten als in dem angegebenen Bereich fällt die Härte der Zwischenschichten sehr rasch ab und bewirkt keine Verschleißfestigkeitssteigerung des erfindungsgemäßen Schichtaufbaues. Desgleichen führt auch lediglich ein Bor-Gehalt innerhalb der erfindungsgemäBen Grenzen im Aluminiumoxid zu einer sprunghaften Verschleißfestigkeitssteigerung. Es war im Gegenteil sogar nicht zu erwarten, daß es bei der Zugabe von Bor zu Aluminiumoxid überhaupt zu einer Verschleißfestigkeitssteigerung kommen kann, da reines Boroxid sehr weich und als Verschleißschutzschicht völlig ungeeignet ist.It is important that the oxygen and boron contents of the individual layers are within the specified limits. Below 0.1% by weight, the influence of oxygen can practically no longer be determined. At higher oxygen contents than in the specified range, the hardness of the intermediate layers drops very quickly and does not increase the wear resistance of the layer structure according to the invention. Likewise, only a boron content within the limits according to the invention in aluminum oxide leads to an abrupt increase in wear resistance. On the contrary, it was not even to be expected that the addition of boron to aluminum oxide could lead to an increase in wear resistance, since pure boron oxide is very soft and completely unsuitable as a wear protection layer.
Zusätzlich bewirkt der Bor-Gehalt in den angegebenen Grenzen bei der Abscheidung der Aluminum-Bor-Mischoxid-Schicht eine geringere Staubentwicklung in der Beschichtungskammer und damit auch auf der Oberfläche des Beschichtungsgutes. Dadurch fallen weniger Schichtfehler an und es ergeben sich gleichmäßigere Schichten.In addition, the boron content within the specified limits causes the deposition of the aluminum-boron mixed oxide layer, less dust is generated in the coating chamber and thus also on the surface of the coating material. This results in fewer shift errors and more even shifts.
In gewissen Anwendungsfällen ist es zweckmäßig, eine Unterlagsschicht zwischen dem Grundkörper und dem erfindungsgemäßen Überzug anzuordnen. Diese Unterlagsschicht weist vorzugsweise einen ein- oder mehrlagigen Schichtaufbau aus einem oder mehreren Karbiden, Nitriden, Karbonitriden, Boriden oder Bornitriden der Elemente der IV. bis VI. Gruppe des Periodensystems auf.In certain applications, it is expedient to arrange an underlayer between the base body and the cover according to the invention. This underlayer preferably has a single or multi-layer structure consisting of one or more carbides, nitrides, carbonitrides, borides or boron nitrides of the elements of IV. To VI. Group of the periodic table.
Weiters ist es in gewissen Anwendungsfällen vorteilhaft, unmittelbar auf einem Grundkörper aus Hartmetall oder über eine Unterlagsschicht eine einzige Schicht aus Titanoxikarbonitrid und/oder Titanoxinitrid mit einer Schichtdicke von 0,05 bis 1,um und anschließend daran eine einzige Aluminium-Bor-Mischoxidschicht mit einer Schichtdicke von 2 bis 10/um aufzubringen.Furthermore, in certain applications it is advantageous to place a single layer of titanium oxycarbonitride and / or titanium oxynitride with a layer thickness of 0.05 to 1 μm directly on a base body made of hard metal or over an underlayer and then a single aluminum-boron mixed oxide layer with a layer Layer thickness from 2 to 10 / to apply.
Eine besonders bevorzugte Ausgestaltung der Erfindung sieht vor, daß unmittelbar auf einem Grundkörper aus Hartmetall oder über eine Unterlagsschicht ein Überzugs, bestehend aus einer Schicht aus Titanoxikarbonitrid und/oder Titanoxinitrid mit einer Schichtdicke von 0,1 bis 1 /um und anschließend daran aus 2 bis 8 Aluminium-Bor-Mischoxidschichten mit Schichtdicken von 0,3 bis 2/um jeweils im Wechsel mit 1 bis 7 Schichten aus Titanoxikarbonitrid und/oder Titanoxinitrid der Schichtdicken 0,05 bis 0,5/um aufgebracht sind. Die Titanoxikarbonitrid-und/oder Titanoxinitrid-Schichten weisen dabei vorzugsweise einen Sauerstoff-Gehalt von 0,5 bis 3 Gew.% auf, während die Aluminum-Bor-Mischoxidschichten vorzugsweise einen Bor-Gehalt von 0,2 bis 2 Gew.% aufweisen.A particularly preferred embodiment of the invention provides that a coating consisting of a layer of titanium oxycarbonitride and / or titanium oxynitride with a layer thickness of 0.1 to 1 .mu.m and then of 2 to 8 aluminum-boron mixed oxide layers with layer thicknesses of 0.3 to 2 / um in alternation with 1 to 7 layers of titanium oxycarbonitride and / or titanium oxynitride with layer thicknesses of 0.05 to 0.5 / um are applied. The titanium oxycarbonitride and / or titanium oxynitride layers preferably have an oxygen content of 0.5 to 3% by weight, while the aluminum-boron mixed oxide layers preferably have a boron content of 0.2 to 2% by weight.
Insbesondere durch diesen mehrschichtigen erfindungsgemäßen Schichtaufbau kommt es gegenüber einem erfindungsgemäßen Schichtaufbau, der nur eine Aluminium-Bor-Mischoxid-Schicht enthält, zu einer weiteren Steigerung der Zähigkeit des Überzuges bei gleichzeitig ausgezeichneter Haftfestigkeit der einzelnen Schichten und damit zu einer unerwarteten Steigerung der Verschleißfestigkeit unter Schlagbeanspruchung des Verschleißteiles.In particular, this multilayered layer structure according to the invention leads to a further increase in the toughness of the coating with an excellent adhesive strength of the individual layers and thus to an unexpected increase in the wear resistance under impact stress compared to a layer structure according to the invention which contains only one aluminum-boron mixed oxide layer of the wearing part.
Eine besonders bevorzugte Unterlagsschicht weist von einem Grundkörper aus Hartmetall ausgehend die Schichtfolge Titankarbid und/oder Titankarbonitrid und/oder Titannitrid mit einer Gesamtschichtdicke von 1 bis 10/um auf.A particularly preferred backing comprises of a base body of hard metal, starting the layer sequence titanium carbide and / or titanium carbonitride and / or titanium nitride having a total layer thickness of 1 to 10 / .mu.m.
Weiters kann es vorteilhaft sein, wenn die Aluminium-Bor-Mischoxide teilweise Titan, Zirkonium, Hafnium, Niob, Chrom- und/oder Magnesium-Oxide enthalten. Daneben können die Mischoxide auch einen Stickstoff-Gehalt von 0,2 bis 4 Atom % aufweisen.Furthermore, it can be advantageous if the aluminum-boron mixed oxides partially contain titanium, zirconium, hafnium, niobium, chromium and / or magnesium oxides. In addition, the mixed oxides can also have a nitrogen content of 0.2 to 4 atom%.
Die Hartstoff-Beschichtung des erfindungsgemäBen Verschleißteiles erfolgt vorzugsweise nach dem CVD-Verfahren, wobei die chemische Zusammensetzung der einzelnen Schichten durch entsprechende Mischungsverhältnisse der Reaktionsgase festgelegt wird.The hard material coating of the wearing part according to the invention is preferably carried out by the CVD method, the chemical composition of the individual layers being determined by appropriate mixing ratios of the reaction gases.
Ein weiteres bevorzugtes Verfahren zur Herstellung des erfindungsgemäßen Verschleißteiles besteht darin, daß die Herstellung der einzelnen Schichten entsprechender chemischer Zusammensetzung sowohl über die Abscheidung nach dem CVD-Verfahren als auch durch Interdiffusion zwischen angerenzenden Schichten erfolgt.Another preferred method for producing the wearing part according to the invention is that the individual layers of appropriate chemical composition are produced both by deposition using the CVD method and by interdiffusion between adjacent layers.
Insbesondere kann die Einbringung der Sauerstoff-Anteile in die Oxikarbid-, Oxikarbonitrid-, Oxinitrid-, Oxiborid-, Oxibornitrid-und/oder Oxiborkarbonitrid-Schichten sowohl über eine entsprechende Gasmischungszusammensetzung, die z.B. C02 H2O-Dampf, Luft, 02 oder andere oxidierende Gase enthalten kann, als auch durch Interdiffusion aus den angrenzenden Aluminium-Bor-Mischoxid-Schichten erfolgen. Diese Interdiffusion kann z.B. durch eine Temperaturbehandlung zwischen oder nach den einzelnen Beschichtungsfahrten bei einer Temperatur, die über der Beschichtungstemperatur liegt, oder während der Beschichtungsfahrt der Aluminium-Bor-Mischoxid-Schichten durch ein erhöhtes SauerstoffAngebot der Gasmischung durchgeführt werden.In particular, the introduction of the oxygen fractions into the oxycarbide, oxycarbonitride, oxynitride, oxiboride, oxibornitride and / or oxiborocarbonitride layers can take place both via an appropriate gas mixture composition, for example C0 2 H 2 O vapor, air, 0 2 or contain other oxidizing gases, as well as by interdiffusion from the adjacent aluminum-boron mixed oxide layers. This interdiffusion can be carried out, for example, by a temperature treatment between or after the individual coating runs at a temperature which is above the coating temperature, or during the coating travel of the aluminum-boron mixed oxide layers by means of an increased supply of oxygen in the gas mixture.
Der Gegenstand der Erfindung wird nachfolgend an Hand von Beispielen näher erläutert.The subject matter of the invention is explained in more detail below with the aid of examples.
Auf Wendeschneidplatten aus Hartmetall der Sorte U10T /Zusammensetzung 6 % Co, 5 % TiC, 5 % (TaC + NbC), 84 % WC, entspricht der ISO-Anwendungsgruppe M10/ und der Form SPGN 120308 EN wurden Überzüge in 5 verschiedenen Schichtaufbau-Varianten entsprechend nachstehender Tabelle aufgebracht. Die Wendeschneidplatten wurden dazu gereinigt, in die Beschichtungskammer einer Prototypenanlage des Anmelders eingebaut, unter Schutzgas auf die Beschichtungstemperatur aufgeheizt und unter den nachfolgenden Beschichtungsbedingungen beschichtet.On indexable inserts made of hard metal of the U10T grade / composition 6% Co, 5% TiC, 5% (TaC + NbC), 84% WC, coatings corresponded to ISO application group M10 / and the shape SPGN 120308 EN in 5 different layer construction variants applied according to the table below. For this purpose, the indexable inserts were cleaned, installed in the coating chamber of a prototype system from the applicant, heated to the coating temperature under protective gas and coated under the following coating conditions.
Die Varianten 4 und 5 sind mit einem Schichtaufbau entsprechend der Erfindung versehen. Diese Varianten werden mit den Varianten 1 bis 3, die einen von der Erfindung abweichenden, in einem Fall vorbekannten Schichtaufbau aufweisen, in einem Zerspanungstest verglichen.Variants 4 and 5 are provided with a layer structure according to the invention. These variants are compared with variants 1 to 3, which have a layer structure which differs from the invention and is known in one case, in a machining test.
Bei allen Varianten liegt eine Unterlagsschicht bestehend aus 2/um Titankarbid gefolgt von 2/um Titankarbonitrid (mit ca. 40 % TiC- und 60 % TiN-Anteil) vor. Bei den Varianten 1 bis 4 wurde Stickstoff als Trägergas verwendet, die Aluminiumoxid- bzw. die Aluminium-Bor-Mischoxidschicht enthält daher ca. 3 Atom % N. Bei Variante 5 ist die Aluminium-Bor-Mischoxidschicht frei von Stickstoff.In all variants there is an underlayer consisting of 2 / um titanium carbide followed by 2 / um titanium carbonitride (with approx. 40% TiC and 60% TiN content). In variants 1 to 4, nitrogen was used as the carrier gas; the aluminum oxide or aluminum-boron mixed oxide layer therefore contains approximately 3 atomic percent N. In variant 5, the aluminum-boron mixed oxide layer is free of nitrogen.
Gasdruck in allen Fällen: Atmosphärendruck (ca. 1 bar absolut)
Temperatur: 1060°Temperature: 1060 °
Mit den beschichteten Wendeschneidplatten wurden unter Verwendung eines Werkzeuges HDP 7225 Drehversuche auf 2 Wellen aus unterschiedlichen Materialien mit unterschiedlichen Schnittbedingungen durchgeführt:
- 1. Werkstoff: Baustahl - Werkstoffnummer 1.1231
- 2. Werkstoff: Grauguß
- 1.Material: mild steel - material number 1.1231
- 2. Material: gray cast iron
Härte: 215 HB Schnittgeschwindigkeit: v = 80 m /min Vorschub: s = 0,28 mm/U Spantiefe: a = 2 mmHardness: 215 HB Cutting speed: v = 80 m / min Feed: s = 0.28 mm / rev chip depth: a = 2 mm
Die Verschleißmarkenbreite vB des Freiflächenverschleisses wurde jeweils nach einer Drehzeit von 5 min gemessen.
Das Standzeitende war bei allen Varianten durch Kolkverschleiß gegeben.The end of the service life was due to scour wear in all variants.
Ein Vergleich der Verschleißergebnisse zeigt, daß lediglich durch den erfindungsgemäßen Schichtaufbau entsprechend den Varianten 4 und 5, wo gleichzeitig ein Bor-Anteil in der Aluminiumoxidschicht und ein Sauerstoff-Anteil in der Ti(C,N)-Schicht vorhanden sind, eine merkliche Verschleißfestigkeitssteigerung gegenüber der Variante 1, die in etwa einen zur Zeit auf dem Markt befindlichen Schichtaufbau aufweist, erzielt wird. Der alternative Einbau von Bor in der Aluminiumoxidschicht (Variante 2) oder von Sauerstoff in der Ti(C,N)-Schicht (Variante 3) ergibt hingegen keine wesentlichen Verschleißfestigkeitssteigerungen gegenüber der Variante 1.A comparison of the wear results shows that only through the layer structure according to the invention according to variants 4 and 5, where there is a boron content in the aluminum oxide layer and an oxygen content in the Ti (C, N) layer at the same time, there is a noticeable increase in wear resistance Variant 1, which has approximately one layer structure currently on the market, is achieved. The alternative incorporation of boron in the aluminum oxide layer (variant 2) or oxygen in the Ti (C, N) layer (variant 3), on the other hand, does not result in any significant increases in wear resistance compared to variant 1.
Aus dem Vergleich der Varianten 4 und 5 ist zu ersehen, daß ein gewisser Stickstoff-Anteil in der Aluminium-Bor-Mischoxidschicht, der z.B. durch die Verwendung von Stickstoff als Trägergas beim Beschichtungsvorgang zustande kommt, nur einen unwesentlichen Einfluß auf die Verschleißfestigkeitswerte hat.From the comparison of variants 4 and 5 it can be seen that a certain nitrogen content in the aluminum-boron mixed oxide layer, e.g. due to the use of nitrogen as carrier gas in the coating process, has only an insignificant influence on the wear resistance values.
Zum Unterschied von Beispiel 1 wird die einlagige Al203- bzw. Aluminium-Bor-Mischoxidschicht durch 4 Schichten ersetzt, die durch 3 Ti(C,N)- bzw. 3 Ti(C,N,0)-Zwischenschichten verbunden sind.In contrast to Example 1, the single-layer Al 2 0 3 or aluminum-boron mixed oxide layer is replaced by 4 layers which are connected by 3 Ti (C, N) or 3 Ti (C, N, 0) intermediate layers .
Bei den Varianten 1 bis 4 wurde Argon als Trägergas verwendet, die Aluminium-Bor-Mischoxidschicht ist daher frei von Stickstoff.In variants 1 to 4, argon was used as the carrier gas; the aluminum-boron mixed oxide layer is therefore free of nitrogen.
Bei der Variante 5 sind in der Mischoxidschicht 3 Atom % Stickstoff enthalten, da N2 als Trägergas verwendet wurde.In variant 5, 3 atom% of nitrogen are contained in the mixed oxide layer, since N 2 was used as the carrier gas.
Gasdruck in allen Fällen: Atmosphärendruck (ca. 1 bar absolut)
Beschichtungstemperatur und Gaszusammensetzung wie bei 2.Ti(C,N)-Schicht Dauer: 8 min/SchichtCoating temperature and gas composition as for 2.Ti (C, N) layer Duration: 8 min / layer
Beschichtungstemperatur und Gaszusammensetzung wie oben Dauer: 8 min/SchichtCoating temperature and gas composition as above Duration: 8 min / shift
Mit den beschichteten Wendeschneidplatten wurden Drehversuche auf der gleichen Welle aus Baustahl unter den gleichen Schnittbedingungen wie beim Beispiel 1 durchgeführt.
Das Standzeitende war jeweils durch die Grenze des noch tolerierbaren Kolkverschleißes bedingt.The end of the service life was due to the limit of the still tolerable scour wear.
Aus dem Vergleich der Beispiele 1 und 2 läßt sich erkennen, daß sich unter den gegebenen Zerspanungsbedingungen bei insgesamt etwa gleicher Gesamtschichtstärke bei dem mehrschichtigen Aufbau der Aluminiumoxid- bzw. Aluminium-Bor-Mischoxidschicht entsprechend Beispiel 2 gegenüber dem einschichtigen Aufbau gemäß Beispiel 1 eine weitere Verchleißfestigkeitssteigerung erreichen läßt. Die Verschleißfestigkeitssteigerung beim erfindungsgemäßen Schichtaufbau (Varianten 4 und 5) ist wesentlich größer als bei dem Schichtaufbau gemäß der Varianten 1 bis 3.It can be seen from the comparison of Examples 1 and 2 that under the given machining conditions with a total layer thickness of approximately the same total, the multilayer structure of the aluminum oxide or aluminum-boron mixed oxide layer according to Example 2 compared to the single-layer structure according to Example 1 shows a further increase in wear resistance can be achieved. The increase in wear resistance in the layer structure according to the invention (variants 4 and 5) is substantially greater than in the layer structure according to variants 1 to 3.
Auf Wendeschneidplatten der gleichen Art wie in Beispiel 1 wurde als Unterlagsschicht eine Ti(C0,6,N0,4)-Schicht und darauf eine TiN-Schicht abgeschieden. Der weitere Schichtaufbau erfolgte in 2 Varianten, wobei die Variante 2 einen erfindungsgemäßen Schichtaufbau darstellt. Zum Unterschied zu den vorangegangenen Beispielen wurde die Beschichtung bei Unterdruck durchgeführt. Die Verschleißfestigkeit der einzelnen Varianten wurde wiederum in einem Zerspanungstest miteinander verglichen.A Ti (C 0.6 , N 0.4 ) layer was deposited on indexable inserts of the same type as in Example 1 and a TiN layer was deposited thereon. The further layer structure was carried out in two variants, variant 2 representing a layer structure according to the invention. In contrast to the previous examples, the coating was carried out under reduced pressure. The wear resistance of the individual variants was again compared with one another in a machining test.
Mit den beschichteten Platten wurden Drehversuche auf Baustahl unter den in Beispiel 1 genannten Schnitbedingungen und Drehversuche auf Grauguß mit folgenden Schnittbedingungen durchgeführt:
- Werkstoff: Grauguß - Zusammensetzung wie bei Beispiel 1 Härte: 205 HB Schnittgeschwindigkeit: v = 80 m/min Vorschub: s = 0,28 mm/U Spantiefe: a = 2 mm
- Material: gray cast iron - composition as in example 1 hardness: 205 HB cutting speed: v = 80 m / min feed: s = 0.28 mm / rev chip depth: a = 2 mm
Ein Vergleich der Beispiele 1 und 2 mit 3 zeigt, daß kein nenneswerter Unterschied in der Qualität der Verschleißteile mit den jeweiligen Überzügen besteht, ja nachdem ob bei Atmosphärendruck oder im Unterdruckbereich beschichtet wurde.A comparison of Examples 1 and 2 with 3 shows that there is no significant difference in the quality of the wearing parts with the respective coatings, depending on whether coating was carried out at atmospheric pressure or in the vacuum range.
Auf Wendeschneidplatten der gleichen Art wie in den vorhergehenden Beispielen wurde wiederum bei Unterdruck ein erfindungsgemäßer viellagiger Schichtaufbau ohne Unterlagsschicht direkt auf dem Hartmetall aufgebracht (Variante 2). Dieser Schichtaufbau wird wiederum mit einem von der Erfindung abweichenden viellagigen Schichtaufbau der ebenfalls ohne Unterlagsschicht aufgebracht ist (Variante 1) verglichen. Schichtaufbau:
Auf einer Baustahlwelle (0,6 % C, Festigkeit 750 N/mm2) wurden Drehversuche unter folgenden Schnittbedingungen durchgeführt:
- Schnittgeschwindigkeit: v = 200 m/min
- Vorschub: s = 0,41 mm/U
- Spantiefe: a = 2 mm
- Cutting speed: v = 200 m / min
- Feed: s = 0.41 mm / rev
- Cutting depth: a = 2 mm
Das Standzeitende war bei beiden Varianten durch Kolkverschleiß gegeben. Das Standzeitende betrug bei Variante 1 32 min bei der erfindungsgemäßen Variante 2 41 min.In both versions, the end of the service life was due to scour wear. The end of the service life in variant 1 was 32 min in variant 2 according to the invention.
In den Beispielen wurde Hartmetall als Grundkörper verwendet. Die Erfindung ist jedoch nicht auf Hartmetall-Grundkörper beschränkt. Der erfindungsgemäße Schichtaufbau führt ebenso bei anderen Grundkörpermaterialien wie z.B. bei Schnellstahl, Stellit oder anderen warmfesten Legierungen zu einer unerwartet großen Steigerung der Verschleißfestigkeit. Desgleichen ist die Erfindung nicht auf Werkzeuge für die spanabhebende Bearbeitung beschränkt. Sie erstreckt sich vielmehr auch auf Werkzeuge für die spanlose Bearbeitung wie Ziehmatrizen und dgl. sowie auf Werkzeuge, die hauptsächlich erodierendem Verschleiß ausgesetzt sind, wie z.B. Gesteinsbohrern.In the examples, hard metal was used as the base body. However, the invention is not limited to hard metal base bodies. The layer structure according to the invention also leads to other base materials such as with high-speed steel, stellite or other heat-resistant alloys to an unexpectedly large increase in wear resistance. Likewise, the invention is not limited to machining tools. Rather, it also extends to tools for non-cutting machining, such as drawing dies and the like, and to tools which are mainly exposed to erosive wear, such as Rock drilling.
Claims (10)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT0555781A AT377786B (en) | 1981-12-24 | 1981-12-24 | WEARING PART, IN PARTICULAR CARBIDE CUTTING INSERT FOR CHIP-REMOVING |
| AT5557/81 | 1981-12-24 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0083043A1 true EP0083043A1 (en) | 1983-07-06 |
| EP0083043B1 EP0083043B1 (en) | 1985-07-03 |
Family
ID=3577093
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP82111762A Expired EP0083043B1 (en) | 1981-12-24 | 1982-12-17 | Wearing part |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US4599281A (en) |
| EP (1) | EP0083043B1 (en) |
| JP (1) | JPS58115081A (en) |
| AT (1) | AT377786B (en) |
| DE (1) | DE3264591D1 (en) |
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| GB1557470A (en) * | 1975-06-12 | 1979-12-12 | Gen Electric | Coated cemented carbide product and precursor therefor |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0152673A2 (en) * | 1983-08-22 | 1985-08-28 | Ovonic Synthetic Materials Company, Inc. | Adherent and wear-resistant composite coatings |
| EP0152673A3 (en) * | 1983-08-22 | 1988-08-03 | Ovonic Synthetic Materials Company, Inc. | Adherent and wear-resistant composite coatings |
| DE3434616A1 (en) * | 1983-12-19 | 1985-08-29 | Veb Werkzeugkombinat Schmalkalden, Ddr 6080 Schmalkalden | Surface layers comprising titanium-boron-nitride compounds, and process for producing them |
| AT385947B (en) * | 1983-12-22 | 1988-06-10 | Ver Edelstahlwerke Ag | CARBIDE BODY, IN PARTICULAR CARBIDE CUTTING TOOL |
| EP0149449A1 (en) * | 1983-12-22 | 1985-07-24 | Vereinigte Edelstahlwerke Aktiengesellschaft (Vew) | Hard metal body, in particular a cutting tool |
| EP0149318A1 (en) * | 1983-12-23 | 1985-07-24 | Corning Glass Works | Manufacture of extrusion die suitable for fabrication of ceramic honeycomb monolith structure |
| EP0172325A1 (en) * | 1984-06-27 | 1986-02-26 | Ovonic Synthetic Materials Company, Inc. | Steel article having a disordered silicon carboxynitride coating, and method of preparing the coating |
| US4720437A (en) * | 1985-03-27 | 1988-01-19 | Sumitomo Electric Industries, Ltd. | Surface-coated cemented carbide article or part |
| EP0196201A1 (en) * | 1985-03-27 | 1986-10-01 | Sumitomo Electric Industries Limited | A surface-coated cemented carbide article or part |
| EP0283923A1 (en) * | 1987-03-26 | 1988-09-28 | Ppg Industries, Inc. | Sputtered titanium oxynitride films |
| AT387186B (en) * | 1987-05-04 | 1988-12-12 | Ver Edelstahlwerke Ag | COATED CARBIDE BODY |
| EP0302984A1 (en) * | 1987-05-04 | 1989-02-15 | Oskar Dipl.-Ing. Dr. Pacher | Coated hard metal body |
| EP0306077A2 (en) * | 1987-08-31 | 1989-03-08 | Plansee Tizit Gesellschaft M.B.H. | Process for the production of multilayer coated hard metal parts |
| EP0306077A3 (en) * | 1987-08-31 | 1990-02-07 | Plansee Tizit Gesellschaft M.B.H. | Process for the production of multilayer coated hard metal parts |
| GB2310218A (en) * | 1996-02-13 | 1997-08-20 | Marconi Gec Ltd | Oxynitride coatings |
| GB2310218B (en) * | 1996-02-13 | 1999-12-22 | Marconi Gec Ltd | Coatings |
Also Published As
| Publication number | Publication date |
|---|---|
| US4599281A (en) | 1986-07-08 |
| JPS6154114B2 (en) | 1986-11-20 |
| EP0083043B1 (en) | 1985-07-03 |
| ATA555781A (en) | 1984-09-15 |
| AT377786B (en) | 1985-04-25 |
| JPS58115081A (en) | 1983-07-08 |
| DE3264591D1 (en) | 1985-08-08 |
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