EP0325760A1 - Work piece made of a nickel base superalloy hardened by dispersion of oxides - Google Patents

Work piece made of a nickel base superalloy hardened by dispersion of oxides Download PDF

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EP0325760A1
EP0325760A1 EP88121056A EP88121056A EP0325760A1 EP 0325760 A1 EP0325760 A1 EP 0325760A1 EP 88121056 A EP88121056 A EP 88121056A EP 88121056 A EP88121056 A EP 88121056A EP 0325760 A1 EP0325760 A1 EP 0325760A1
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weight
boron
hardened
oxide dispersion
nickel
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French (fr)
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Pieter Jongenburger
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ABB Asea Brown Boveri Ltd
ABB AB
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ABB Asea Brown Boveri Ltd
Asea Brown Boveri AB
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof

Definitions

  • Oxide dispersion-hardened superalloys based on nickel which thanks to their excellent mechanical properties are used at high temperatures in the construction of thermally and mechanically highly stressed thermal machines. Preferred use as blade materials for gas turbines.
  • the invention relates to the further development of oxide-dispersion-hardened nickel-based superalloys with overall optimal properties, in particular with regard to behavior during secondary recrystallization, in order to achieve coarse-grained structure and for the production of single crystals of large dimensions.
  • It also relates to a method for expanding the temperature range of the secondary recrystallization of an oxide-dispersion-hardened nickel-based superalloy during the coarse grain annealing of a workpiece and during annealing to produce a single crystal of large dimensions with a cross section of at least 5 cm 2.
  • high-temperature super alloys have been developed, particularly for components of thermal machines (gas turbine blades). These are nickel-based alloys that contain finely divided dispersoids in the form of oxides. Most often, the latter are Y2O3 particles.
  • the alloys are used in the state of coarse-grained stem crystals aligned in the longitudinal axis of the component. The coarser the crystals, the better the mechanical high-temperature properties (resistance to creep and fatigue strength with a comparatively low number of load cycles, etc.).
  • the desired structural state is attempted by means of an annealing process of the forged, hot-pressed or mostly extruded, fine-grained semi-finished product, with "zone annealing" playing a dominant role.
  • the workpiece is briefly heated in zones above the recrystallization temperature, the highest possible temperature / displacement gradient having to be achieved during the heating. This applies to the entire workpiece cross section. In the case of large cross sections, this requirement encounters difficulties because of the transverse heat flow required for this. Only the temperature range between recrystallization and solidus temperature (occurrence of the first liquid phase) is available as a "window" for carrying out the annealing process. This area is relatively narrow in the case of the conventional, commercially available oxide-dispersion-hardened nickel-based superalloys and is not sufficient to successfully convert large-diameter workpieces into coarse grains and, ideally, into a single crystal.
  • the alloy with the trade name MA6000 from INCO is cited as prior art and an example of a known conventional precipitation-hardenable, oxide-dispersion-strengthened nickel-base superalloy (cf. DE-A-23 53 971).
  • Corresponding alloys with a comparatively low chromium content are also known (see K.Mino and K.Asakawa, "An oxide dispersion strengthened nickel-base superalloy with excellent high temperature strength", Transactions of the Iron and Steel Institute of Japan, Vol. 27 , p. 823-829, Tokyo 1987).
  • the invention is based on the object of specifying oxide-dispersion-hardened nickel-based superalloys which have a wider range of temperature limits than known alloys for carrying out the annealing required for producing coarse grains (secondary recrystallization).
  • the task consists in particular in specifying a method for expanding the temperature range of the secondary recrystallization, which allows suitable methods Annealing processes (eg "zone annealing") to produce even single crystals of large dimensions (cross section at least 5 cm2).
  • oxide-dispersion-hardened nickel-base superalloy is doped with a boron content of more than 0.011% by weight in the process mentioned at the outset.
  • 1 shows a diagram of the course of the recrystallization temperature and the solidus temperature as a function of the boron content of an oxide-dispersion-hardened nickel-base superalloy with 15% by weight of chromium.
  • 1 is the curve for the course of the recrystallization temperature
  • 2 the curve for the course of the solidus temperature.
  • ⁇ T is the maximum temperature range available for secondary recrystallization. No recrystallization takes place below curve 1 and annealing with the aim of growing coarse grain or even a single crystal is pointless. Liquid phases appear above curve 2 and the crystal structure is destroyed. The dispersoids agglomerate and become ineffective as a hardening factor.
  • curve 2 the solidus temperature decreases slightly with increasing boron content, but the recrystallization temperature according to curve 1 increases significantly, which increases ⁇ T.
  • 3 relates to a diagram of the course of the recrystallization temperature and the solidus temperature as a function of the boron content of an oxide-dispersion-hardened nickel-base superalloy with 17% by weight of chromium.
  • 5 is the curve for the course of the recrystallization temperature, 6 that for the course of the solidus temperature.
  • the temperature range ⁇ T is approx. 145 ° C.
  • FIG. 4 is a diagram of the course of the recrystallization temperature and the solidus temperature as a function of the boron Ge of an oxide dispersion hardened nickel-base superalloy with a low chromium content. In the present case, the latter was approximately 6% by weight. 7 is the curve for the course of the recrystallization temperature, 8 is the curve for the course of the solidus temperature. With a boron content of 0.04% by weight, the temperature range ⁇ T is approx. 140 ° C.
  • a prismatic body 20 mm thick, 50 mm wide and 180 mm long was subjected to a zone annealing process from the above material with 0.04% by weight boron. Longitudinal stem crystals with an average of 25 mm wide, 8 mm thick and 60 mm long could be obtained.
  • the investigation referred to a fine-grained oxide dispersion hardened nickel-base superalloy as delivered.
  • a fine-grained oxide dispersion-hardened nickel-base superalloy extruded in the delivered condition was subjected to the test.
  • a cylindrical body 40 mm in diameter and 200 mm in length was worked out from the above material with 0.035% by weight of boron and subjected to a zone annealing process.
  • the recrystallized structure consisted of longitudinal stem crystals with an average thickness of 10 mm on all sides and 130 mm in length.
  • a fine-grained oxide dispersion-hardened nickel-base superalloy with a row structure that was hot-kneaded as delivered was examined.
  • a semi-cylindrical body 55 mm in diameter and 220 mm in length was made from the above material with 0.045% by weight of boron worked out.
  • the workpiece was subjected to a zone annealing process to produce a single crystal.
  • the invention is not restricted to the exemplary embodiments.
  • the new method relates to the expansion of the temperature range of the secondary recrystallization of an oxide-dispersion-hardened nickel-based superalloy during the coarse-grain annealing of a workpiece and during annealing to produce a single crystal of large dimensions with a cross section of at least 10 cm2, the oxide-dispersion-hardened nickel-based superalloy with a boron content of more is doped as 0.011% by weight.
  • the doping is preferably 0.026 to 0.3% by weight of boron or 0.026 to 0.1% by weight of boron.
  • the advantages of the claimed alloys and the new process lie in that created by expanding the temperature range of the secondary recrystallization greater freedom of the annealing process, especially the zone annealing process. This enables the complete, flawless recrystallization to coarse, longitudinally oriented stem crystals in the case of large workpiece cross sections to be treated. This applies even more to the annealing of a workpiece for the production of a single crystal of large dimensions.
  • the new process made it possible to manufacture single-section turbine blades with a large cross-section, as required for modern high-performance industrial gas turbines.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Turbine Rotor Nozzle Sealing (AREA)
  • Powder Metallurgy (AREA)

Abstract

Oxide dispersion hardened superalloy based on nickel, which is composed of the following main components… … Cr             5 - 13.95% by wt. or =                14.05 - 22% by wt. Al =                2.5 - 7% by wt. Mo =                  0 - 2% by wt. W =                  0 - 15% by wt. Ta =                  0 - 7% by wt. Hf =                  0 - 1% by wt. Ti =                  0 - 3% by wt. Zr =             0.02 - 0.2% by wt. Co =                 0 - 10% by wt. C =                 0 - 0.2% by wt. Y2O3 =                1 - 2% by wt. Ni =                      remainder … and which additionally contains 0.026 to 0.3% by weight of boron. …<??>Process for extending the temperature range of the secondary recrystallisation of an oxide dispersion hardened nickel-based superalloy of the above composition during coarse annealing and in the production of a single crystal having a cross-section of at least 5 cm<2> by doping with a boron content of at least 0.011% by weight. …<IMAGE>…

Description

TECHNISCHES GEBIETTECHNICAL AREA

Oxyddispersionsgehärtete Superlegierungen auf der Basis von Nickel, welche dank ihrer hervorragenden mechanischen Eigen­schaften bei hohen Temperaturen beim Bau thermisch und mecha­nisch hochbeanspruchter thermischer Maschinen Verwendung finden. Bevorzugte Verwendung als Schaufelwerkstoffe für Gasturbinen.Oxide dispersion-hardened superalloys based on nickel, which thanks to their excellent mechanical properties are used at high temperatures in the construction of thermally and mechanically highly stressed thermal machines. Preferred use as blade materials for gas turbines.

Die Erfindung bezieht sich auf die Weiterentwicklung von oxyd­dispersionsgehärteten Nickelbasis-Superlegierungen mit insge­samt optimalen Eigenschaften insbesondere bezüglich Verhalten bei der sekundären Rekristallisation zur Erzielung grobkörnigen Gefüges und zur Herstellung von Einkristallen grosser Abemssun­gen.The invention relates to the further development of oxide-dispersion-hardened nickel-based superalloys with overall optimal properties, in particular with regard to behavior during secondary recrystallization, in order to achieve coarse-grained structure and for the production of single crystals of large dimensions.

Insbesondere betrifft sie eine oxyddispersionsgehärtete Super­legierung auf der Basis von Nickel, welche aus folgenden Haupt­bestandteilen zusammengesetzt ist: Cr = 5 - 13,95 Gew.-% oder 14,05 - 22 Gew.-% Al = 2,5 - 7 Gew.-% Mo = 0 - 2 Gew.-% W = 0 - 15 Gew.-% Ta = 0 - 7 Gew.-% Hf = 0 - 1 Gew.-% Ti = 0 - 3 Gew.-% Zr = 0,02 - 0,2 Gew.-% Co = 0 - 10 Gew.-% C = 0 - 0,2 Gew.-% Y₂O₃ = 1 - 2 Gew.-% Ni = Rest. In particular, it relates to an oxide dispersion-hardened superalloy based on nickel, which is composed of the following main components: Cr = 5 - 13.95% by weight or 14.05 - 22% by weight Al = 2.5 - 7% by weight Mo = 0-2% by weight W = 0 - 15% by weight Ta = 0 - 7% by weight Hf = 0-1% by weight Ti = 0 - 3% by weight Zr = 0.02 - 0.2% by weight Co = 0 - 10% by weight C = 0 - 0.2% by weight Y₂O₃ = 1 - 2% by weight Ni = Rest.

Sie betrifft ferner ein Verfahren zur Erweiterung des Tempera­turbereiches der sekundären Rekristallisation einer oxyddis­persionsgehärteten Nickelbasis-Superlegierung beim Grobkorn­glühen eines Werkstücks und beim Glühen zur Herstellung eines Einkristalls grosser Abmessungen mit einem Querschnitt von mindestens 5 cm².It also relates to a method for expanding the temperature range of the secondary recrystallization of an oxide-dispersion-hardened nickel-based superalloy during the coarse grain annealing of a workpiece and during annealing to produce a single crystal of large dimensions with a cross section of at least 5 cm 2.

STAND DER TECHNIKSTATE OF THE ART

Zum allgemeinen Stand der Technik wird folgende Literatur zitiert:
- G.H. Gessinger, Powder Metallurgy of Superalloys, Butter­worths, London, 1984
- R.F. Singer and E. Arzt, Conf. Proc. "High Temperature Mate­rials for Gas Turbines", Liège, Belgium, Oktober 1986
- J.S. Benjamin, Metall. Trans., 1970, 1, 2943 - 2951.The following literature is cited on the general state of the art:
- GH Gessinger, Powder Metallurgy of Superalloys, Butterworths, London, 1984
- RF Singer and E. Doctor, Conf. Proc. "High Temperature Materials for Gas Turbines", Liège, Belgium, October 1986
- JS Benjamin, metal. Trans., 1970, 1, 2943-2951.

Im Verlauf der vergangenen Jahre ist eine neue Klasse von hochwarmfesten Superlegierungen, insbesondere für Bauteile thermischer Maschinen (Gasturbinenschaufeln) entwickelt worden. Es handelt sich um Nickelbasislegierungen, welche fein verteilte Dispersoide in Form von Oxyden enthalten. Meistens handelt es sich bei letzteren um Y₂O₃-Partikel. Die Legierungen werden im Zustand grobkörniger, in der Längsachse des Bauteils ausge­richteter Stengelkristalle eingesetzt. Je gröber die Kristalle, desto besser die mechanischen Hochtemperatureigenscshaften (Widerstand gegen Kriechen und Ermüdungsfestigkeit bei ver­gleichsweise niedriger Lastwechselzahl etc.). Der angestrebte Gefügezustand wird durch einen Glühprozess des geschmiede­ten, heissgepressten oder meist stranggepressten, feinkörni­gen Halbzeugs zu verwirklichen versucht, wobei das "zonen­glühen" eine dominierende Rolle spielt. Dabei wird das Werkstück zonenweise kurzzeitig über die Rekristallisationstemperatur erhitzt, wobei ein möglichst hoher Temperatur/Weg-Gradient beim Aufheizen verwirklicht werden muss. Dies gilt für den ganzen Werkstückquerschnitt. Bei grossen Querschnitten stösst diese Forderung wegen des dafür notwendigen transversalen Wärmeflusses auf Schwierigkeiten. Es steht nämlich nur der Temperaturbereich zwischen Rekristallisations- und Solidus­temperatur (Auftreten der ersten flüssigen Phase) als "Fenster" für die Durchführung des Glühprozesses zur Verfügung. Dieser Bereich ist bei den herkömmlichen, handelsüblichen oxyddis­persionsgehärteten Nickelbasis-Superlegierungen verhältnismässig schmal und reicht nicht aus, um Werkstücke grossen Querschnitts erfolgreich in grobes Korn und im Idealfall in einen Einkristall überzuführen.Over the past few years, a new class of high-temperature super alloys has been developed, particularly for components of thermal machines (gas turbine blades). These are nickel-based alloys that contain finely divided dispersoids in the form of oxides. Most often, the latter are Y₂O₃ particles. The alloys are used in the state of coarse-grained stem crystals aligned in the longitudinal axis of the component. The coarser the crystals, the better the mechanical high-temperature properties (resistance to creep and fatigue strength with a comparatively low number of load cycles, etc.). The desired structural state is attempted by means of an annealing process of the forged, hot-pressed or mostly extruded, fine-grained semi-finished product, with "zone annealing" playing a dominant role. The workpiece is briefly heated in zones above the recrystallization temperature, the highest possible temperature / displacement gradient having to be achieved during the heating. This applies to the entire workpiece cross section. In the case of large cross sections, this requirement encounters difficulties because of the transverse heat flow required for this. Only the temperature range between recrystallization and solidus temperature (occurrence of the first liquid phase) is available as a "window" for carrying out the annealing process. This area is relatively narrow in the case of the conventional, commercially available oxide-dispersion-hardened nickel-based superalloys and is not sufficient to successfully convert large-diameter workpieces into coarse grains and, ideally, into a single crystal.

Es besteht daher ein ausgesprochenes Bedürfnis nach Verbesse­rung der Rekristallisationsbedingungen oxyddispersionsgehärte­ter Superlegierungen, insbesondere nach grösserer Freiheit in der Wahl der Betriebsparameter beim Grobkornglühen und beim Glühen zur Herstellung von Einkristallen grosser Abmessun­gen.There is therefore a pronounced need for improving the recrystallization conditions of oxide-dispersion-hardened superalloys, in particular for greater freedom in the choice of operating parameters for coarse-grain annealing and annealing for the production of single crystals of large dimensions.

Als Stand der Technik und Beispiel einer bekannten herkömmlichen ausscheidungshärtbaren, oxyddispersionsverfestigten Nickel­basis-Superlegierung wird die Legierung mit der Handelsbe­zeichnung MA6000 von INCO genannt (vergl. DE-A-23 53 971). Es sind ferner entsprechende Legierungen mit vergleichsweise niedrigem Chromgehalt bekannt (vergl. K.Mino und K.Asakawa, "An oxide dispersion strengthened nickel-base superalloy with excellent high temperature strength", Transactions of the Iron and Steel Institute of Japan, Vol. 27, p. 823-829, Tokyo 1987).The alloy with the trade name MA6000 from INCO is cited as prior art and an example of a known conventional precipitation-hardenable, oxide-dispersion-strengthened nickel-base superalloy (cf. DE-A-23 53 971). Corresponding alloys with a comparatively low chromium content are also known (see K.Mino and K.Asakawa, "An oxide dispersion strengthened nickel-base superalloy with excellent high temperature strength", Transactions of the Iron and Steel Institute of Japan, Vol. 27 , p. 823-829, Tokyo 1987).

Es ist schon vorgeschlagen worden, bei herkömmlichen, nichtoxyd­dispersionsgehärteten Nickelbasis-Superlegierungen die mechani­schen und thermischen Eigenschaften bei mittleren und hohen Temperaturen, insbesondere die Duktilität und den Widerstand gegen thermische Ermüdung (Ermüdung bei vergleichsweise niedrigen Lastwechselzahlen) durch Zusätze von Bor und Kohlenstoff zu verbessern (vergl. DE-A-24 63 066; M.A. Burke, J. Greggi, G.A. Whitlow, The effect of boron and carbon on the microstruc­tural chemistries of two wrought nickel base superalloys, Scripta metallurgica, Vol. 18, p. 91-94, Pergamon 1984). Es finden sich indessen keinerlei Hinweise auf oxyddispersionsge­härtete Superlegierungen. Ausserdem ist der Mechanismus der Rekristallisation bei letzteren (sog. sekundäre Rekristallisa­tion) dank dem Vorhandensein inkohärenter oxydischer Disper­soide ein völlig anderer als derjenige von herkömmlichen Legie­rungen.It has already been proposed to improve the mechanical and thermal properties at medium and high temperatures, in particular the ductility and the resistance to thermal fatigue (fatigue at comparatively low number of load cycles) in conventional, non-oxide dispersion hardened nickel-base superalloys by adding boron and carbon (cf. DE-A-24 63 066; MA Burke, J. Greggi, GA Whitlow, The effect of boron and carbon on the microstructural chemistries of two wrought nickel base superalloys, Scripta metallurgica, Vol. 18, p. 91-94, Pergamon 1984). However, there is no evidence of oxide dispersion-hardened superalloys. In addition, the mechanism of recrystallization in the latter (so-called secondary recrystallization) is completely different from that of conventional alloys thanks to the presence of incoherent oxidic dispersoids.

DARSTELLUNG DER ERFINDUNGPRESENTATION OF THE INVENTION

Der Erfindung liegt die Aufgabe zugrunde, oxyddispersionsge­härtete Superlegierungen auf der Basis von Nickel anzugeben, welche einen gegenüber bekannten Legierungen erweiterten Bereich der Temperaturgrenzen für die Durchführung der zur Erzeugung von Grobkorn notwendigen Glühung (sekundäre Rektristallisation) aufweisen. Die Aufgabe besteht insbesondere darin, ein Verfahren zur Erweiterung des Temperaturbereiches der sekundären Rekri­stallisation anzugeben, welches gestattet, durch geeignete Glühprozesse (z.B. "Zonenglühen") selbst Einkristalle grosser Abmessungen (Querschnitt mindestens 5 cm²) herzustellen.The invention is based on the object of specifying oxide-dispersion-hardened nickel-based superalloys which have a wider range of temperature limits than known alloys for carrying out the annealing required for producing coarse grains (secondary recrystallization). The task consists in particular in specifying a method for expanding the temperature range of the secondary recrystallization, which allows suitable methods Annealing processes (eg "zone annealing") to produce even single crystals of large dimensions (cross section at least 5 cm²).

Diese Aufgabe wird dadurch gelöst, dass die eingangs erwähnte Superlegierung auf der Basis von Nickel zusätzlich Bor in einem Gehalt von 0,026 bis 0,3 Gew.-% enthält.This object is achieved in that the above-mentioned superalloy based on nickel additionally contains boron in a content of 0.026 to 0.3% by weight.

Diese Aufgabe wird ferner dadurch gelöst, dass im eingangs erwähnten Verfahren die oxyddispersionsgehärtete Nickelbasis-­Superlegierung mit einem Borgehalt von mehr als 0,011 Gew.-% dotiert wird.This object is further achieved in that the oxide-dispersion-hardened nickel-base superalloy is doped with a boron content of more than 0.011% by weight in the process mentioned at the outset.

WEG ZUR AUSFÜHRUNG DER ERFINDUNGWAY OF CARRYING OUT THE INVENTION

Die Erfindung wird anhand der nachfolgenden, durch Figuren näher erläuterten Ausführungsbeispiele beschrieben. Dabei zeigt:

  • Fig. 1 ein Diagramm des Verlaufs der Rekristallisationstempe­ratur und der Solidustemperatur in Funktion des Bor-­Gehaltes einer oxyddispersionsgehärteten Nickelbasis-­Superlegierung mit 15 Gew.-% Chrom,
  • Fig. 2 ein Diagramm des Verlaufs der Rekristallisationstempe­ratur und der Solidustemperatur in Funktion des Bor-­Gehaltes einer oxyddispersionsgehärteten Nickelbasis-­Superlegierung mit 20 Gew.-% Chrom,
  • Fig. 3 ein Diagramm des Verlaufs der Rekristallisationstempe­ratur und der Solidustemperatur in Funktion des Bor-­Gehaltes einer oxyddispersionsgehärteten Nickelbasis-­Superlegierung mit 17 Gew.-% Chrom,
  • Fig. 4 ein Diagramm des Verlaufs der Rekristallisationstempe­ratur und der Solidustemperatur in Funktion des Bor-­Gehaltes einer oxyddispersionsgehärteten Nickelbasis-­Superlegierung mit niedrigem Chromgehalt.
The invention is described on the basis of the following exemplary embodiments which are explained in more detail by means of figures. It shows:
  • 1 shows a diagram of the course of the recrystallization temperature and the solidus temperature as a function of the boron content of an oxide-dispersion-hardened nickel-base superalloy with 15% by weight of chromium,
  • 2 shows a diagram of the course of the recrystallization temperature and the solidus temperature as a function of the boron content of an oxide-dispersion-hardened nickel-base superalloy with 20% by weight of chromium,
  • 3 shows a diagram of the course of the recrystallization temperature and the solidus temperature as a function of the boron content of an oxide-dispersion-hardened nickel-base superalloy with 17% by weight of chromium,
  • 4 shows a diagram of the course of the recrystallization temperature and the solidus temperature as a function of the boron content of an oxide-dispersion-hardened nickel-base superalloy with a low chromium content.

In Fig. 1 ist ein Diagramm des Verlaufs der Rekristallisations­temperatur und der Solidustemperatur in Funktion des Bor-Gehal­tes einer oxyddispersionsgehärteten Nickelbasis-Superlegierung mit 15 Gew.-% Chrom dargestellt. 1 ist die Kurve für den Verlauf der Rekristallisationstemperatur, 2 die Kurve für den Verlauf der Solidustemperatur. ΔT ist der maximal zur Verfügung ste­hende Temperaturbereich für die sekundäre Rekristallisation. Unterhalb der Kurve 1 findet keine Rekristallisation statt und ein Glühen mit dem Ziel, grobes Korn oder gar einen Ein­kristall zu züchten, ist zwecklos. Oberhalb der Kurve 2 treten flüssige Phasen auf und der Kristallverband wird zerstört. Die Dispersoide agglomerieren und werden als Härtungsfaktor unwirksam. Gemäss Kurve 2 nimmt zwar die Solidustemperatur mit steigendem Bor-Gehalt geringfügig ab, die Rekristallisa­tionstemperatur gemäss Kurve 1 jedoch bedeutend stärker, wodurch ΔT erweitert wird.1 shows a diagram of the course of the recrystallization temperature and the solidus temperature as a function of the boron content of an oxide-dispersion-hardened nickel-base superalloy with 15% by weight of chromium. 1 is the curve for the course of the recrystallization temperature, 2 the curve for the course of the solidus temperature. ΔT is the maximum temperature range available for secondary recrystallization. No recrystallization takes place below curve 1 and annealing with the aim of growing coarse grain or even a single crystal is pointless. Liquid phases appear above curve 2 and the crystal structure is destroyed. The dispersoids agglomerate and become ineffective as a hardening factor. According to curve 2, the solidus temperature decreases slightly with increasing boron content, but the recrystallization temperature according to curve 1 increases significantly, which increases ΔT.

Fig. 2 zeigt ein Diagramm des Verlaufs der Rekristallisations­temperatur und der Solidustemperatur in Funktion des Bor-­Gehaltes einer oxyddispersionsgehärteten Nickelbasis-Superle­gierung mit 20 Gew.-% Chrom. 3 ist die mit zunehmendem Bor-Ge­halt relativ steil abfallende Kurve für die Rekristallisations­temperatur, 4 die wesentlich flacher verlaufende für die Solidus­temperatur. Bei einem Bor-Gehalt von 0,03 Gew.-% beträgt der Temperaturbereich ΔT bereits ca. 150 °C.2 shows a diagram of the course of the recrystallization temperature and the solidus temperature as a function of the boron content of an oxide-dispersion-hardened nickel-base superalloy with 20% by weight of chromium. 3 is the curve for the recrystallization temperature that drops relatively steeply with increasing boron content, 4 the significantly flatter curve for the solidus temperature. With a boron content of 0.03% by weight, the temperature range ΔT is already approx. 150 ° C.

Fig. 3 bezieht sich auf ein Diagramm des Verlaufs der Rekri­stallisationstemperatur und der Solidustemperatur in Funktion des Bor-Gehaltes einer oxyddispersionsgehärteten Nickelbasis-­Superlegierung mit 17 Gew.-% Chrom. 5 ist die Kurve für den Verlauf der Rekristallisationstemperatur, 6 diejenige für den Verlauf der Solidustemperatur. Bei einem Bor-Gehalt von 0,035 Gew.-% beträgt der Temperaturbereich ΔT ca. 145 °C.3 relates to a diagram of the course of the recrystallization temperature and the solidus temperature as a function of the boron content of an oxide-dispersion-hardened nickel-base superalloy with 17% by weight of chromium. 5 is the curve for the course of the recrystallization temperature, 6 that for the course of the solidus temperature. With a boron content of 0.035% by weight, the temperature range ΔT is approx. 145 ° C.

In Fig. 4 ist ein Diagramm des Verlaufs der Rekristallisations­temperatur und der Solidustemperatur in Funktion des Bor-Ge­ haltes einer oxyddispersionsgehärteten Nickelbasis-Superlegie­rung mit niedrigem Chromgehalt dargestellt. Im vorliegenden Fall betrug letzterer ca. 6 Gew.-%. 7 ist die Kurve für den Verlauf der Rekristallisationstemperatur, 8 die Kurve für den Verlauf der Solidustemperatur. Bei einem Bor-Gehalt von 0,04 Gew.-% beträgt der Temperaturbereich ΔT ca. 140 °C.4 is a diagram of the course of the recrystallization temperature and the solidus temperature as a function of the boron Ge of an oxide dispersion hardened nickel-base superalloy with a low chromium content. In the present case, the latter was approximately 6% by weight. 7 is the curve for the course of the recrystallization temperature, 8 is the curve for the course of the solidus temperature. With a boron content of 0.04% by weight, the temperature range ΔT is approx. 140 ° C.

Es konnte beobachtet werden, dass bei allen untersuchten oxyd­dispersionsgehärteten Nickelbasis-Superlegierungen die Tempera­tur der sekundären Rekristallisation mit steigendem Bor-Gehalt herabgesetzt wird. Die Grösse der Wirkung des Bor-Zusatzes ist unterschiedlich und hängt von der Zusammensetzung der Legierung ab. Offenbar spielt dabei der Chromgehalt eine wichtige Rolle. Bei Legierungen mit hohem Chromgehalt konnte eine Er­niedrigung der Rekristallisationstemperatur von bis zu 50 °C pro 0,01 Gew.-% Bor-Zusatz festgestellt werden.It was observed that the temperature of the secondary recrystallization is reduced with increasing boron content in all investigated oxide dispersion hardened nickel-base superalloys. The magnitude of the effect of the boron addition varies and depends on the composition of the alloy. The chromium content obviously plays an important role in this. In the case of alloys with a high chromium content, a reduction in the recrystallization temperature of up to 50 ° C. per 0.01 wt.

AUSFÜHRUNGSBEISPIELEEXAMPLES AUSFÜHRUNGSBEISPIEL 1:EMBODIMENT 1: Siehe Fig. 1 !See Fig. 1!

Es wurde eine im Anlieferungszustand stranggepresste feinkörni­ge oxyddispersionsgehärtete Nickelbasis-Superlegierung unter­sucht. Die borfreie Legierung hatte die nachfolgende Grund-­Zusammensetzung: Cr = 15 Gew.-% W = 4,0 Gew.-% Mo = 2,0 Gew.-% Al = 4,5 Gew.-% Ti = 2,5 Gew.-% Ta = 2,0 Gew.-% C = 0,05 Gew.-% Zr = 0,15 Gew.-% Y₂O₃ = 1,1 Gew.-% Ni = Rest. A fine-grained oxide dispersion-hardened nickel-base superalloy extruded in the delivered condition was examined. The basic composition of the boron-free alloy was as follows: Cr = 15% by weight W = 4.0% by weight Mo = 2.0% by weight Al = 4.5% by weight Ti = 2.5% by weight Ta = 2.0% by weight C = 0.05% by weight Zr = 0.15% by weight Y₂O₃ = 1.1% by weight Ni = Rest.

Es wurden Proben mit verschiedenen Bor-Zusätzen hergestellt, wobei der gesamte Bor-Gehalt zwischen 0 und ca. 0,05 Gew.-% variiert wurde. Die Rekristallisationstemperatur und die Solidus­temperatur wurden nach herkömmlichen Methoden bestimmt. Die Ergebnisse sind in Fig. 1 graphisch dargestellt.Samples with various boron additives were produced, the total boron content being varied between 0 and approximately 0.05% by weight. The recrystallization temperature and the solidus temperature were determined by conventional methods. The results are shown graphically in FIG. 1.

Aus obigem Werkstoff mit 0,04 Gew.-% Bor wurde ein prismatischer Körper von 20 mm Dicke, 50 mm Breite und 180 mm Länge einem Zonenglühprozess unterworfen. Es konnten längsgerichtete Sten­gelkristalle von durchschnittlich 25 mm Breite, 8 mm Dicke und 60 mm Länge erzielt werden.A prismatic body 20 mm thick, 50 mm wide and 180 mm long was subjected to a zone annealing process from the above material with 0.04% by weight boron. Longitudinal stem crystals with an average of 25 mm wide, 8 mm thick and 60 mm long could be obtained.

AUSFÜHRUNGSBEISPIEL 2:EMBODIMENT 2: Siehe Fig. 2 !See Fig. 2!

Die Untersuchung bezog sich auf eine im Anlieferungszustand stranggepresste feinkörnige oxyddispersionsgehärtete Nickel­basis-Superlegierung. Die borfreie Legierung wies die nachfol­gende Grund-Zusammensetzung auf: Cr = 20,0 Gew.-% Al = 6,0 Gew.-% Mo = 2,0 Gew.-% W = 3,5 Gew.-% Zr = 0,19 Gew.-% C = 0,01 Gew.-% Y₂O₃ = 1,1 Gew.-% Ni = Rest. The investigation referred to a fine-grained oxide dispersion hardened nickel-base superalloy as delivered. The boron-free alloy had the following basic composition: Cr = 20.0% by weight Al = 6.0% by weight Mo = 2.0% by weight W = 3.5% by weight Zr = 0.19% by weight C = 0.01% by weight Y₂O₃ = 1.1% by weight Ni = Rest.

Es wurden Prüfkörper mit systematisch steigenden Bor-Gehalten hergestellt, wobei die Bor-Werte zwischen 0 und ca. 0,045 Gew.-% variiert wurden. Sowohl die Rekristallisationstemperatur wie die Solidustemperatur wurden nach herkömmlichen Methoden bestimmt. Fig. 2 zeigt die dabei erzielten Ergebnisse.Test specimens with systematically increasing boron contents were produced, the boron values being varied between 0 and approximately 0.045% by weight. Both the recrystallization temperature and the solidus temperature were determined using conventional methods. Fig. 2 shows the results achieved.

Aus obigem Werkstoff mit 0,03 Gew.-% Bor wurde ein Tragflügel­profil mit folgenden Abmessungen herausgearbeitet: Breite = 92 mm Grösste Dicke = 22 mm Profilhöhe = 26 mm Länge = 240 mm Das Werkstück wurde einem Zonenglühprozess unterworfen, wobei ein Einkristall erzeugt wurde.A wing profile with the following dimensions was worked out from the above material with 0.03% by weight boron: Width = 92 mm Greatest thickness = 22 mm Profile height = 26 mm Length = 240 mm The workpiece was subjected to a zone annealing process to produce a single crystal.

AUSFÜHRUNGSBEISPIEL 3:EMBODIMENT 3: Siehe Fig. 3 !See Fig. 3!

Es wurde eine im Anlieferungszustand stranggepresste feinkörnige oxyddispersionsgehärtete Nickelbasis-Superlegierung der Prüfung unterzogen. Die borfreie Legierung hatte die nachfolgende Grund-Zusammensetzung: Cr = 17,0 Gew.-% Al = 6,0 Gew.-% Mo = 2,0 Gew.-% W = 3,5 Gew.-% Ta = 2,0 Gew.-% Zr = 0,15 Gew.-% C = 0,05 Gew.-% Y₂O₃ = 1,1 Gew.-% Ni = Rest. A fine-grained oxide dispersion-hardened nickel-base superalloy extruded in the delivered condition was subjected to the test. The basic composition of the boron-free alloy was as follows: Cr = 17.0% by weight Al = 6.0% by weight Mo = 2.0% by weight W = 3.5% by weight Ta = 2.0% by weight Zr = 0.15% by weight C = 0.05% by weight Y₂O₃ = 1.1% by weight Ni = Rest.

Es wurden Proben mit verschiedenen Bor-Zusätzen hergestellt, wobei der gesamte Bor-Gehalt zwischen 0,005 und 0,05 Gew.-% variiert wurde. Die Solidustemperatur und die Rekristallisa­tionstemperatur wurde jeweils nach üblichen bekannten Methoden bestimmt. Die Ergebnisse sind in Fig. 3 dargestellt.Samples with various boron additives were produced, the total boron content being varied between 0.005 and 0.05% by weight. The solidus temperature and the recrystallization temperature were determined in each case by customary known methods. The results are shown in FIG. 3.

Aus obigem Werkstoff mit 0,035 Gew.-% Bor wurde ein zylindri­scher Körper von 40 mm Durchmesser und 200 mm Länge herausge­arbeitet und einem Zonenglühprozess unterworfen. Das rekri­stallisierte Gefüge bestand aus längsgerichteten Stengelkri­stallen von durchschnittlich 10 mm allseitiger Dicke und 130 mm Länge.A cylindrical body 40 mm in diameter and 200 mm in length was worked out from the above material with 0.035% by weight of boron and subjected to a zone annealing process. The recrystallized structure consisted of longitudinal stem crystals with an average thickness of 10 mm on all sides and 130 mm in length.

AUSFÜHRUNGSBEISPIEL 4:EMBODIMENT 4: Siehe Fig. 4 !See Fig. 4!

Es wurde eine im Anlieferungszustand warmgeknetete feinkörnige oxyddispersionsgehärtete Nickelbasis-Superlegierung mit Zeilen­struktur untersucht. Die Legierung hatte die nachfolgende Grund-Zusammensetzung: Co = 9,7 Gew.-% Cr = 5,9 Gew.-% Al = 4,2 Gew.-% Mo = 2,0 Gew.-% W = 12,4 Gew.-% Ta = 4,7 Gew.-% Ti = 0,8 Gew.-% Zr = 0,05 Gew.-% C = 0,05 Gew.-% Y₂O₃ = 1,1 Gew.-% Ni = Rest. A fine-grained oxide dispersion-hardened nickel-base superalloy with a row structure that was hot-kneaded as delivered was examined. The alloy had the following basic composition: Co = 9.7% by weight Cr = 5.9% by weight Al = 4.2% by weight Mo = 2.0% by weight W = 12.4% by weight Ta = 4.7% by weight Ti = 0.8% by weight Zr = 0.05% by weight C = 0.05% by weight Y₂O₃ = 1.1% by weight Ni = Rest.

Der Legierung der Grund-Zusammensetzung wurden jeweils verschie­dene Gehalte an Bor zulegiert, deren Werte sich zwischen 0,001 und 0,06 Gew.-% bewegten. Sowohl die Solidustemperatur wie die Rekristallisationstemperatur wurde nach den üblichen, herkömmlichen Methoden bestimmt. Die Resultate sind in Fig. 4 graphisch dargestellt.Different amounts of boron were added to the alloy of the basic composition, the values of which ranged between 0.001 and 0.06% by weight. Both the solidus temperature and the recrystallization temperature were determined using the customary, conventional methods. The results are shown graphically in FIG. 4.

Aus obigem Werkstoff mit 0,045 Gew.-% Bor wurde ein halbzy­lindrischer Körper von 55 mm Durchmesser und 220 mm Länge herausgearbeitet. Das Werkstück wurde einem Zonenglühprozess unterworfen, wobei ein Einkristall erzeugt wurde.A semi-cylindrical body 55 mm in diameter and 220 mm in length was made from the above material with 0.045% by weight of boron worked out. The workpiece was subjected to a zone annealing process to produce a single crystal.

Die Erfindung ist nicht auf die Ausführungsbeispiele beschränkt.The invention is not restricted to the exemplary embodiments.

Die Zusammensetzung der oxyddispersionsgehärteten Superlegie­rungen stellt sich wie folgt: Cr = 5 - 13,95 Gew.-% Al = 2,5 - 7 Gew.-% Mo = 0 - 2 Gew.-% W = 0 - 15 Gew.-% Ta = 0 - 7 Gew.-% Hf = 0 - 1 Gew.-% Ti = 0 - 3 Gew.-% Zr = 0,02 - 0,2 Gew.-% Co = 0 - 10 Gew.-% C = 0 - 0,2 Gew.-% Y₂O₃ = 1 - 2 Gew.-% Ni = Rest, sowie 0,026 bis 0,3 Gew.-% Bor oder 0,026 bis 0,1 Gew.-% Bor.The composition of the oxide dispersion hardened superalloys is as follows: Cr = 5 - 13.95% by weight Al = 2.5 - 7% by weight Mo = 0-2% by weight W = 0 - 15% by weight Ta = 0 - 7% by weight Hf = 0-1% by weight Ti = 0 - 3% by weight Zr = 0.02 - 0.2% by weight Co = 0 - 10% by weight C = 0 - 0.2% by weight Y₂O₃ = 1 - 2% by weight Ni = Rest, and 0.026 to 0.3% by weight boron or 0.026 to 0.1% by weight boron.

Ferner: Cr = 14,05 - 22 Gew.-% Al = 2,5 - 7 Gew.-% Mo = 0 - 2 Gew.-% W = 0 - 15 Gew.-% Ta = 0 - 7 Gew.-% Hf = 0 - 1 Gew.-% Ti = 0 - 3 Gew.-% Zr = 0,02 - 0,2 Gew.-% Co = 0 - 10 Gew.-% C = 0 - 0,2 Gew.-% Y₂O₃ = 1 - 2 Gew.-% Ni = Rest, sowie 0,026 bis 0,3 Gew.-% Bor oder 0,026 bis 0,1 Gew.-% Bor.Further: Cr = 14.05 - 22% by weight Al = 2.5 - 7% by weight Mo = 0-2% by weight W = 0 - 15% by weight Ta = 0 - 7% by weight Hf = 0-1% by weight Ti = 0 - 3% by weight Zr = 0.02 - 0.2% by weight Co = 0 - 10% by weight C = 0 - 0.2% by weight Y₂O₃ = 1 - 2% by weight Ni = Rest, and 0.026 to 0.3% by weight boron or 0.026 to 0.1% by weight boron.

Es fällt ferner folgende Legierung unter die beanspruchte Zusammensetzung: Cr = 18 - 22 Gew.-% Al = 5 - 7 Gew.-% Mo = 0 - 4 Gew.-% W = 2 - 5 Gew.-% Zr = 0,1 - 0,2 Gew.-% C = 0 - 0,2 Gew.-% Y₂O₃ = 1 - 2 Gew.-% Ni = Rest, sowie 0,011 bis 0,3 Gew.-% Bor oder 0,011 bis 0,1 Gew.-% Bor.The following alloy also falls under the claimed composition: Cr = 18-22% by weight Al = 5 - 7% by weight Mo = 0 - 4% by weight W = 2 - 5% by weight Zr = 0.1 - 0.2% by weight C = 0 - 0.2% by weight Y₂O₃ = 1 - 2% by weight Ni = Rest, and 0.011 to 0.3% by weight boron or 0.011 to 0.1% by weight boron.

Eine weitere Legierungsklasse hat die nachfolgende Zusammenset­zung: Cr = 16 - 18 Gew.-% Al = 6 - 7 Gew.-% Mo = 2 - 2,5 Gew.-% W = 3 - 3,5 Gew.-% Ta = 2 - 2,5 Gew.-% Hf = 0 - 1,5 Gew.-% Zr < 0,2 Gew.-% C < 0,1 Gew.-% Y₂O₃ = 1 - 1,5 Gew.-% Ni = Rest, sowie 0,02 bis 0,3 Gew.-% Bor oder 0,02 bis 0,1 Gew.-% Bor.Another alloy class has the following composition: Cr = 16-18% by weight Al = 6 - 7% by weight Mo = 2 - 2.5% by weight W = 3 - 3.5% by weight Ta = 2 - 2.5% by weight Hf = 0 - 1.5% by weight Zr < 0.2% by weight C < 0.1% by weight Y₂O₃ = 1 - 1.5% by weight Ni = Rest, and 0.02 to 0.3% by weight boron or 0.02 to 0.1% by weight boron.

Ferner wird der folgende Legierungstyp beansprucht: Cr = 16 - 18 Gew.-% Al = 6 - 7 Gew.-% Co = 8 - 10 Gew.-% Ta = 5 - 7 Gew.-% Zr < 0,2 Gew.-% C < 0,1 Gew.-% Y₂O₃ = 1 - 1,5 Gew.-% Ni = Rest, sowie 0,02 bis 0,3 Gew.-% Bor oder 0,02 bis 0,1 Gew.-% Bor.The following alloy type is also claimed: Cr = 16-18% by weight Al = 6 - 7% by weight Co = 8-10% by weight Ta = 5 - 7% by weight Zr < 0.2% by weight C < 0.1% by weight Y₂O₃ = 1 - 1.5% by weight Ni = Rest, and 0.02 to 0.3% by weight boron or 0.02 to 0.1% by weight boron.

Unter den Legierungen mit niedrigerem Chromgehalt werden die nachfolgenden beansprucht: Co = 0 - 10 Gew.-% Cr = 5 - 17 Gew.-% Al = 2,5 - 7 Gew.-% Mo = 0 - 2 Gew.-% W = 2,5 - 13 Gew.-% Ta = 0 - 7 Gew.-% Ti = 0,5 - 1,9 Gew.-% Zr = 0,02 - 0,1 Gew.-% C = 0 - 0,2 Gew.-% Y₂O₃ = 1 - 2 Gew.-% Ni = Rest, sowie 0,011 bis 0,3 Gew.-% Bor oder 0,011 bis 0,1 Gew.-% Bor.Among the alloys with a lower chromium content, the following are claimed: Co = 0 - 10% by weight Cr = 5 - 17% by weight Al = 2.5 - 7% by weight Mo = 0-2% by weight W = 2.5 - 13% by weight Ta = 0 - 7% by weight Ti = 0.5 - 1.9% by weight Zr = 0.02 - 0.1% by weight C = 0 - 0.2% by weight Y₂O₃ = 1 - 2% by weight Ni = Rest, and 0.011 to 0.3% by weight boron or 0.011 to 0.1% by weight boron.

Vorzugsweise hat die erwähnte Legierung die nachfolgende Zusammensetzung: Cr = 13 - 17 Gew.-% Al = 2,5 - 7 Gew.-% Mo = 1 - 1,7 Gew.-% W = 2,5 - 3,4 Gew.-% Ta = 0 - 5 Gew.-% Ti = 1 - 1,9 Gew.-% Zr = 0,02 - 0,1 Gew.-% C = 0 - 0,2 Gew.-% Y₂O₃ = 1 - 2 Gew.-% Ni = Rest, sowie 0,011 bis 0,3 Gew.-% Bor oder 0,011 bis 0,1 Gew.-% Bor.The alloy mentioned preferably has the following composition: Cr = 13 - 17% by weight Al = 2.5 - 7% by weight Mo = 1 - 1.7% by weight W = 2.5 - 3.4% by weight Ta = 0 - 5% by weight Ti = 1 - 1.9% by weight Zr = 0.02 - 0.1% by weight C = 0 - 0.2% by weight Y₂O₃ = 1 - 2% by weight Ni = Rest, and 0.011 to 0.3% by weight boron or 0.011 to 0.1% by weight boron.

Eine spezielle, vorteilhafte Auswahl stellt die nachfolgende Zusammensetzung dar: Cr = 15 Gew.-% Al = 5 Gew.-% Mo = 1,7 Gew.-% W = 3,4 Gew.-% Ta = 4,5 Gew.-% Ti = 1,9 Gew.-% Zr = 0,1 Gew.-% C = 0,05 Gew.-% Y₂O₃ = 1,1 Gew.-% Ni = Rest, sowie 0,011 bis 0,3 Gew.-% Bor oder 0,011 bis 0,1 Gew.-% Bor.The following composition represents a special, advantageous selection: Cr = 15% by weight Al = 5% by weight Mo = 1.7% by weight W = 3.4% by weight Ta = 4.5% by weight Ti = 1.9% by weight Zr = 0.1% by weight C = 0.05% by weight Y₂O₃ = 1.1% by weight Ni = Rest, and 0.011 to 0.3% by weight boron or 0.011 to 0.1% by weight boron.

Das neue Verfahren bezieht sich auf die Erweiterung des Tempera­turbereiches der sekundären Rekristallisation einer oxyddisper­sionsgehärteten Nickelbasis-Superlegierung beim Grobkornglühen eines Werkstücks und beim Glühen zur Herstellung eines Ein­kristalls grosser Abmessungen mit einem Querschnitt von minde­stens 10 cm², wobei die oxyddisperionsgehärtete Nickelbasis-­Superlegierung mit einem Borgehalt von mehr als 0,011 Gew.-% dotiert wird. Die Dotierung beträgt vorzugsweise 0,026 bis 0,3 Gew.-% Bor oder 0,026 bis 0,1 Gew.-% Bor.The new method relates to the expansion of the temperature range of the secondary recrystallization of an oxide-dispersion-hardened nickel-based superalloy during the coarse-grain annealing of a workpiece and during annealing to produce a single crystal of large dimensions with a cross section of at least 10 cm², the oxide-dispersion-hardened nickel-based superalloy with a boron content of more is doped as 0.011% by weight. The doping is preferably 0.026 to 0.3% by weight of boron or 0.026 to 0.1% by weight of boron.

Die Vorteile der beanspruchten Legierungen und des neuen Verfahrens liegen in der durch die Erweiterung des Tempera­turbereichs der sekundären Rekristallisation geschaffenen grösseren Freiheit des Glühprozesses, insbesondere des Zonen­glühprozesses. Dadurch wird die vollständige, einwandfreie Rekristallisation zu groben, längsgerichteten Stengelkri­stallen bei grossen, zu behandelnden Werkstückquerschnitten überhaupt erst ermöglicht. Dies gilt noch mehr für das Glühen eines Werkstücks zur Herstellung eines Einkristalls grosser Abmessungen. Mit dem neuen Verfahren wurde die Möglichkeit geschaffen, aus einem Einkristall bestehende Turbinenschaufeln grossen Querschnitts herzustellen, wie sie für neuzeitliche industrielle Gasturbinen hoher Leistung gefordert werden.The advantages of the claimed alloys and the new process lie in that created by expanding the temperature range of the secondary recrystallization greater freedom of the annealing process, especially the zone annealing process. This enables the complete, flawless recrystallization to coarse, longitudinally oriented stem crystals in the case of large workpiece cross sections to be treated. This applies even more to the annealing of a workpiece for the production of a single crystal of large dimensions. The new process made it possible to manufacture single-section turbine blades with a large cross-section, as required for modern high-performance industrial gas turbines.

Claims (19)

1. Oxyddispersionsgehärtete Superlegierung auf der Basis von Nickel, welche aus folgenden Hauptbestandteilen zusammen­gesetzt ist: Cr = 5 - 13,95 Gew.-% Al = 2,5 - 7 Gew.-% Mo = 0 - 2 Gew.-% W = 0 - 15 Gew.-% Ta = 0 - 7 Gew.-% Hf = 0 - 1 Gew.-% Ti = 0 - 3 Gew.-% Zr = 0,02 - 0,2 Gew.-% Co = 0 - 10 Gew.-% C = 0 - 0,2 Gew.-% Y₂O₃ = 1 - 2 Gew.-% Ni = Rest,
dadurch gekennzeichnet, dass sie zusätzlich Bor in einem Gehalt von 0,026 bis 0,3 Gew.-% enthält.1. Oxide dispersion hardened superalloy based on nickel, which is composed of the following main components: Cr = 5 - 13.95% by weight Al = 2.5 - 7% by weight Mo = 0-2% by weight W = 0 - 15% by weight Ta = 0 - 7% by weight Hf = 0-1% by weight Ti = 0 - 3% by weight Zr = 0.02 - 0.2% by weight Co = 0 - 10% by weight C = 0 - 0.2% by weight Y₂O₃ = 1 - 2% by weight Ni = Rest,
characterized in that it additionally contains boron in a content of 0.026 to 0.3% by weight. 2. Oxyddispersionsgehärtete Superlegierung nach Anspruch 1, dadurch gekennzeichnet, dass die Bor in einem Gehalt von 0,026 bis 0,1 Gew.-% enthält.2. Oxide dispersion hardened superalloy according to claim 1, characterized in that the boron contains in a content of 0.026 to 0.1 wt .-%. 3. Oxyddispersionsgehärtete Superlegierung auf der Basis von Nickel, welche aus folgenden Hauptbestandteilen zusammen­gesetzt ist: Cr = 14,05 - 22 Gew.-% Al = 2,5 - 7 Gew.-% Mo = 0 - 2 Gew.-% W = 0 - 15 Gew.-% Ta = 0 - 7 Gew.-% Hf = 0 - 1 Gew.-% Ti = 0 - 3 Gew.-% Zr = 0,02 - 0,2 Gew.-% Co = 0 - 10 Gew.-% C = 0 - 0,2 Gew.-% Y₂O₃ = 1 - 2 Gew.-% Ni = Rest,
dadurch gekennzeichnet, dass sie zusätzlich Bor in einem Gehalt von 0,026 bis 0,3 Gew.-% enthält.3. Oxide dispersion-hardened superalloy based on nickel, which is composed of the following main components: Cr = 14.05 - 22% by weight Al = 2.5 - 7% by weight Mo = 0-2% by weight W = 0 - 15% by weight Ta = 0 - 7% by weight Hf = 0-1% by weight Ti = 0 - 3% by weight Zr = 0.02 - 0.2% by weight Co = 0 - 10% by weight C = 0 - 0.2% by weight Y₂O₃ = 1 - 2% by weight Ni = Rest,
characterized in that it additionally contains boron in a content of 0.026 to 0.3% by weight. 4. Oxyddispersionsgehärtete Superlegierung nach Anspruch 3, dadurch gekennzeichnet, dass sie Bor in einem Gehalt von 0,026 bis 0,1 Gew.-% enthält.4. Oxide dispersion hardened superalloy according to claim 3, characterized in that it contains boron in a content of 0.026 to 0.1 wt .-%. 5. Oxyddispersionsgehärtete Superlegierung auf der Basis von Nickel, dadurch gekennzeichnet, dass sie die nachfolgende Zusammensetzung aufweist: Cr = 18 - 22 Gew.-% Al = 5 - 7 Gew.-% Mo = 0 - 4 Gew.-% W = 2 - 5 Gew.-% Zr = 0,1 - 0,2 Gew.-% B = 0,011 - 0,3 Gew.-% C = 0 - 0,2 Gew.-% Y₂O₃ = 1 - 2 Gew.-% Ni = Rest.
5. Oxide dispersion hardened superalloy based on nickel, characterized in that it has the following composition: Cr = 18-22% by weight Al = 5 - 7% by weight Mo = 0 - 4% by weight W = 2 - 5% by weight Zr = 0.1 - 0.2% by weight B = 0.011 - 0.3% by weight C = 0 - 0.2% by weight Y₂O₃ = 1 - 2% by weight Ni = Rest.
6. Oxyddispersionsgehärtete Superlegierung nach Anspruch 5, dadurch gekennzeichnet, dass sie Bor in einem Gehalt von 0,011 bis 0,1 Gew.-% enthält.6. Oxide dispersion hardened superalloy according to claim 5, characterized in that it contains boron in a content of 0.011 to 0.1 wt .-%. 7. Oxyddispersionsgehärtete Superlegierung auf der Basis von Nickel, dadurch gekennzeichnet, dass sie die nachfolgende Zusammensetzung aufweist: Cr = 16 - 18 Gew.-% Al = 6 - 7 Gew.-% Mo = 2 - 2,5 Gew.-% W = 3 - 3,5 Gew.-% Ta = 2 - 2,5 Gew.-% Hf = 0 - 1,5 Gew.-% Zr < 0,2 Gew.-% B = 0,02 - 0,3 Gew.-% C < 0,1 Gew.-% Y₂O₃ = 1 - 1,5 Gew.-% Ni = Rest.
7. Oxide dispersion-hardened superalloy based on nickel, characterized in that it has the following composition: Cr = 16-18% by weight Al = 6 - 7% by weight Mo = 2 - 2.5% by weight W = 3 - 3.5% by weight Ta = 2 - 2.5% by weight Hf = 0 - 1.5% by weight Zr < 0.2% by weight B = 0.02 - 0.3% by weight C < 0.1% by weight Y₂O₃ = 1 - 1.5% by weight Ni = Rest.
8. Oxyddispersionsgehärtete Superlegierung nach Anspruch 7, dadurch gekennzeichnet, dass sie Bor in einem Gehalt von 0,02 bis 0,1 Gew.-% enthält.8. Oxide dispersion hardened superalloy according to claim 7, characterized in that it contains boron in a content of 0.02 to 0.1 wt .-%. 9. Oxyddispersionsgehärtete Superlegierung auf der Basis von Nickel, dadurch gekennzeichnet, dass sie die nachfolgende Zusammensetzung aufweist: Cr = 16 - 18 Gew.-% Al = 6 - 7 Gew.-% Co = 8 - 10 Gew.-% Ta = 5 - 7 Gew.-% Zr < 0,2 Gew.-% B = 0,02 - 0,3 Gew.-% C < 0,1 Gew.-% Y₂O₃ = 1 - 1,5 Gew.-% Ni = Rest.
9. Oxide dispersion-hardened superalloy based on nickel, characterized in that it has the following composition: Cr = 16-18% by weight Al = 6 - 7% by weight Co = 8-10% by weight Ta = 5 - 7% by weight Zr < 0.2% by weight B = 0.02 - 0.3% by weight C < 0.1% by weight Y₂O₃ = 1 - 1.5% by weight Ni = Rest.
10. Oxyddispersionsgehärtete Superlegierung nach Anspruch 9, dadurch gekennzeichnet, dass sie Bor in einem Gehalt von 0,02 bis 0,1 Gew.-% enthält.10. Oxide dispersion hardened superalloy according to claim 9, characterized in that it contains boron in a content of 0.02 to 0.1 wt .-%. 11. Oxyddispersionsgehärtete Superlegierung auf der Basis von Nickel, dadurch gekennzeichnet, dass sie die nachfolgende Zusammensetzung aufweist: Co = 0 - 10 Gew.-% Cr = 5 - 17 Gew.-% Al = 2,5 - 7 Gew.-% Mo = 0 - 2 Gew.-% W = 2,5 - 13 Gew.-% Ta = 0 - 7 Gew.-% Ti = 0,5 - 1,9 Gew.-% Zr = 0,02 - 0,1 Gew.-% C = 0 - 0,2 Gew.-% B = 0,011- 0,3 Gew.-% Y₂O₃ = 1 - 2 Gew.-% Ni = Rest.
11. Oxide dispersion-hardened superalloy based on nickel, characterized in that it has the following composition: Co = 0 - 10% by weight Cr = 5 - 17% by weight Al = 2.5 - 7% by weight Mo = 0-2% by weight W = 2.5 - 13% by weight Ta = 0 - 7% by weight Ti = 0.5 - 1.9% by weight Zr = 0.02 - 0.1% by weight C = 0 - 0.2% by weight B = 0.011-0.3% by weight Y₂O₃ = 1 - 2% by weight Ni = Rest.
12. Oxyddispersionsgehärtete Superlegierung nach Anspruch 11, dadurch gekennzeichnet, dass sie Bor in einem Gehalt von 0,011 bis 0,1 Gew.-% enthält.12. Oxide dispersion hardened superalloy according to claim 11, characterized in that it contains boron in a content of 0.011 to 0.1 wt .-%. 13. Oxyddispersionsgehärtete Superlegierung nach Anspruch 11, dadurch gekennzeichnet, dass sie die nachfolgende Zusammen­setzung aufweist: Cr = 13 - 17 Gew.-% Al = 2,5 - 7 Gew.-% Mo = 1 - 1,7 Gew.-% W = 2,5 - 3,4 Gew.-% Ta = 0 - 5 Gew.-% Ti = 1 - 1,9 Gew.-% Zr = 0,02 - 0,1 Gew.-% C = 0 - 0,2 Gew.-% B = 0,011- 0,3 Gew.-% Y₂O₃ = 1 - 2 Gew.-% Ni = Rest.
13. Oxide dispersion hardened superalloy according to claim 11, characterized in that it has the following composition: Cr = 13 - 17% by weight Al = 2.5 - 7% by weight Mo = 1 - 1.7% by weight W = 2.5 - 3.4% by weight Ta = 0 - 5% by weight Ti = 1 - 1.9% by weight Zr = 0.02 - 0.1% by weight C = 0 - 0.2% by weight B = 0.011-0.3% by weight Y₂O₃ = 1 - 2% by weight Ni = Rest.
14. Oxyddispersionsgehärtete Superlegierung nach Anspruch 13, dadurch gekennzeichnet, dass sie Bor in einem Gehalt von 0,011 bis 0,1 Gew.-% enthält.14. Oxide dispersion hardened superalloy according to claim 13, characterized in that it contains boron in a content of 0.011 to 0.1 wt .-%. 15. Oxyddispersionsgehärtete Superlegierung nach Anspruch 13, dadurch gekennzeichnet, dass sie die nachfolgende Zusammen­setzung aufweist: Cr = 15 Gew.-% Al = 5 Gew.-% Mo = 1,7 Gew.-% W = 3,4 Gew.-% Ta = 4,5 Gew.-% Ti = 1,9 Gew.-% Zr = 0,1 Gew.-% C = 0,05 Gew.-% B = 0,011 - 0,3 Gew.-% Y₂O₃ = 1,1 Gew.-% Ni = Rest.
15. Oxide dispersion hardened superalloy according to claim 13, characterized in that it has the following composition: Cr = 15% by weight Al = 5% by weight Mo = 1.7% by weight W = 3.4% by weight Ta = 4.5% by weight Ti = 1.9% by weight Zr = 0.1% by weight C = 0.05% by weight B = 0.011 - 0.3% by weight Y₂O₃ = 1.1% by weight Ni = Rest.
16. Oxyddispersionsgehärtete Superlegierung nach Anspruch 15, dadurch gekennzeichnet, dass sie Bor in einem Gehalt von 0,011 bis 0,1 Gew.-% enthält.16. Oxide dispersion hardened superalloy according to claim 15, characterized in that it contains boron in a content of 0.011 to 0.1 wt .-%. 17. Verfahren zur Erweiterung des Temperaturbereiches der sekun­dären Rekristallisation einer oxyddispersionsgehärteten Nickelbasis-Superlegierung beim Grobkornglühen eines Werk­stücks und beim Glühen zur Herstellung eines Einkristalls grosser Abmessungen mit einem Querschnitt von mindestens 5 cm², dadurch gekennzeichnet, dass die oxyddisperionsge­härtete Nickelbasis Superlegierung mit einem Borgehalt von mehr als 0,011 Gew.-% dotiert wird.17. A method for expanding the temperature range of the secondary recrystallization of an oxide-dispersion-hardened nickel-based superalloy during the coarse grain annealing of a workpiece and during annealing to produce a single crystal of large dimensions with a cross section of at least 5 cm², characterized in that the oxide-dispersion-hardened nickel-based superalloy with a boron content of more than 0.011 wt .-% is doped. 18. Verfahren nach Anspruch 17, dadurch gekennzeichnet, dass die oxyddispersionsgehärtete Nickelbasis-Superlegierung mit einem Borgehalt von 0,026 bis 0,3 Gew.-% dotiert wird.18. The method according to claim 17, characterized in that the oxide dispersion hardened nickel-based superalloy is doped with a boron content of 0.026 to 0.3 wt .-%. 19. Verfahren nach Anspruch 18, dadurch gekennzeichnet, dass die oxyddispersionsgehärtete Nickelbasis-Superlegierung mit einem Borgehalt von 0,026 bis 0,1 Gew.-% dotiert wird.19. The method according to claim 18, characterized in that the oxide dispersion hardened nickel-base superalloy is doped with a boron content of 0.026 to 0.1% by weight.
EP88121056A 1988-01-18 1988-12-16 Work piece made of a nickel base superalloy hardened by dispersion of oxides Ceased EP0325760A1 (en)

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WO1992013179A1 (en) * 1991-01-23 1992-08-06 Man B&W Diesel A/S Valve with hard-facing
EP0525816A1 (en) * 1991-08-02 1993-02-03 Isover Saint-Gobain Method and apparatus for manufacturing mineral wool, and mineral wool produced thereby
EP0583791A1 (en) * 1992-08-20 1994-02-23 Isover Saint-Gobain Method for producing mineral wool, and mineral wool produced thereby
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CN111379028A (en) * 2020-04-08 2020-07-07 中国科学院金属研究所 Ni-Al binary single crystal alloy, Ni-Al binary model single crystal alloy and preparation method thereof

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US5180451A (en) * 1990-03-20 1993-01-19 Asea Brown Boveri Ltd. Process for the production of longitudinally-directed coarse-grained columnar crystals in a workpiece consisting of an oxide-dispersion-hardened nickel-based superalloy
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EP0525816A1 (en) * 1991-08-02 1993-02-03 Isover Saint-Gobain Method and apparatus for manufacturing mineral wool, and mineral wool produced thereby
WO1993002977A1 (en) * 1991-08-02 1993-02-18 Isover Saint-Gobain Method and apparatus for manufacturing mineral wood, and mineral wool produced thereby
US6158249A (en) * 1991-08-02 2000-12-12 Isover Saint-Gobain Apparatus for manufacturing mineral wool
WO1994004468A1 (en) * 1992-08-20 1994-03-03 Isover Saint-Gobain Method for producing mineral wool, and mineral wool produced thereby
EP0583791A1 (en) * 1992-08-20 1994-02-23 Isover Saint-Gobain Method for producing mineral wool, and mineral wool produced thereby
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US7824606B2 (en) 2006-09-21 2010-11-02 Honeywell International Inc. Nickel-based alloys and articles made therefrom
EP2431489A1 (en) * 2010-09-20 2012-03-21 Siemens Aktiengesellschaft Nickel-base superalloy
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WO2012038166A3 (en) * 2010-09-20 2012-09-07 Siemens Aktiengesellschaft Nickel-base superalloy
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CN111379028A (en) * 2020-04-08 2020-07-07 中国科学院金属研究所 Ni-Al binary single crystal alloy, Ni-Al binary model single crystal alloy and preparation method thereof

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