DE102007055711B4 - Material based on SiAlONs - Google Patents

Material based on SiAlONs Download PDF

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Publication number
DE102007055711B4
DE102007055711B4 DE102007055711.8A DE102007055711A DE102007055711B4 DE 102007055711 B4 DE102007055711 B4 DE 102007055711B4 DE 102007055711 A DE102007055711 A DE 102007055711A DE 102007055711 B4 DE102007055711 B4 DE 102007055711B4
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mass
volume
sialon
microns
cation
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DE102007055711A1 (en
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Dr. Bitterlich Bernd
Dr. Friederich Kilian
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Ceramtec GmbH
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Ceramtec GmbH
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    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

Werkstoff auf der Basis von SiAlONen, enthaltend einen α/β-SiAlON-Werkstoff mit 5 bis 50% Masse%, bevorzugt 5 bis 30% Masse% α/(α+β) RE-α-SiAlON, wobei RE für mindestens ein Kation aus Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Mg oder Ca, bevorzugt mindestens ein Kation aus Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb und zusätzlich mindestens ein Kation aus Mg oder Ca steht, sowie 95 bis 50 Masse% , bevorzugt 95 bis 70 Masse% β/(α+β) β-SiAION und einer Hf-haltigen amorphen oder teil-kristallinen Korngrenzenphase mit einem Anteil am Gesamtwerkstoff von unter 10 Vol%, wobei der Hf-Gehalt des gesinterten Werkstoffs 0,4 bis 0,6 Masse% beträgt und einer Dispersionsphase, bestehend aus globularen Partikeln mit mittleren Partikelgrößen von 0,2 bis 15 µm, bevorzugt 0,4 bis 10 µm aus mindestens einem Hartstoff aus SiC, TiN, TiC, Ti(C,N), Carbide und/oder Nitride der Elemente der Gruppen IVb, Vb und Vlb des Periodensystems (PSE) sowie Scandiumcarbid und/oder Scandiumoxicarbid oder Mischungen aus den aufgeführten Hartstoffen, die in einem Anteil von 5 bis 30 Vol%, bevorzugt 7,5 bis 20 Vol%, besonders bevorzugt 10 bis 15 Vol% im Sinterkörper enthalten sind.SiAlON-based material containing an α / β-SiAlON material having 5 to 50% mass%, preferably 5 to 30% mass% α / (α + β) RE-α-SiAlON, where RE is at least one cation from Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Mg or Ca, preferably at least one cation of Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and additionally at least one cation of Mg or Ca, and 95 to 50 mass%, preferably 95 to 70 mass % β / (α + β) β-SiAION and an Hf-containing amorphous or partially crystalline grain boundary phase with a total material content of less than 10% by volume, the Hf content of the sintered material being from 0.4 to 0.6% by mass is and a dispersion phase consisting of globular particles having average particle sizes of 0.2 to 15 microns, preferably 0.4 to 10 microns of at least one hard material of SiC, TiN, TiC, Ti (C, N), carbides and / or nitrides the elements of groups IVb, Vb and Vlb of the periodic table (PSE) sow ie Scandiumcarbid and / or Scandiumoxicarbid or mixtures of the listed hard materials, which are contained in a proportion of 5 to 30% by volume, preferably 7.5 to 20% by volume, particularly preferably 10 to 15% by volume in the sintered body.

Description

SiAlON-Werkstoffe eignen sich aufgrund ihrer hohen Verschleißbeständigkeit zum Zerspanen metallischer Werkstoffe, vorzugsweise Gusseisen. Insbesondere alpha/beta-SiAlONe besitzen eine günstige Kombination aus Härte und Zähigkeit. Neben den mechanischen Eigenschaften bei Raumtemperatur sind für die Anwendung als keramischer Schneidwerkstoff auch die Eigenschaften bei Temperaturen um 800°C bis 1000°C entscheidend. Eine wirtschaftliche Herstellung von SiAlONen ist allerdings nur durch Verwendung von Sinterhilfsmitteln möglich. Diese vereinfachen zwar die Verdichtung des Werkstoffs, bleiben nach dem Abkühlen jedoch als überwiegend glasartige Korngrenzenphase im Produkt zurück. Das Erweichen dieser Korngrenzphase bestimmt die mechanischen und chemischen Eigenschaften des Werkstoffs bei erhöhten Temperaturen. Beim Zerspanen von metallischen Werkstoffen wird der Verschleiß vorwiegend durch mechanische Abrasion und zusätzlich durch chemische Reaktionen verursacht. Eine hohe Verschleißfestigkeit kann also nur erzielt werden, wenn Härte, Zähigkeit und chemische Beständigkeit auch bei den Anwendungs-Temperaturen hoch bleiben. Die Menge und Zusammensetzung der glasartigen Korngrenzenphase besitzt deshalb eine Schlüsselfunktion hinsichtlich des Verschleißes.Due to their high wear resistance, SiAlON materials are suitable for machining metallic materials, preferably cast iron. In particular, alpha / beta SiAlONs have a favorable combination of hardness and toughness. In addition to the mechanical properties at room temperature, the properties at temperatures around 800 ° C to 1000 ° C are crucial for use as a ceramic cutting material. An economical production of SiAlONs is only possible by using sintering aids. Although these simplify the compaction of the material, they remain as a predominantly vitreous grain boundary phase in the product after cooling. The softening of this grain boundary phase determines the mechanical and chemical properties of the material at elevated temperatures. When machining metallic materials, wear is mainly caused by mechanical abrasion and also by chemical reactions. High wear resistance can only be achieved if hardness, toughness and chemical resistance remain high even at the application temperatures. The amount and composition of the vitreous grain boundary phase therefore has a key function in terms of wear.

Verbesserte Hochtemperatur-Eigenschaften können prinzipiell durch Verwenden einer geringeren Menge an Sinteradditiven erreicht werden. Dies führt zu weniger Korngrenzenphase im Produkt, wodurch bei ihrer Erweichung bei hohen Temperaturen der Einfluss auf die Werkstoffeigenschaften geringer ist. Da herkömmliche Schneidwerkstoffe bereits sehr geringe Additivmengen besitzen, ist eine weitere Reduzierung wegen der sich dann verschlechternden Sintereigenschaften kaum möglich, wenn insbesondere das wirtschaftliche Gasdrucksintern angewandt werden soll.Improved high temperature properties can in principle be achieved by using a smaller amount of sintering additives. This results in less grain boundary phase in the product which, when softened at high temperatures, reduces the influence on the material properties. Since conventional cutting materials already have very small amounts of additive, a further reduction due to the then deteriorating sintering properties is hardly possible if in particular the economic gas pressure sintering is to be applied.

Die Härte von SiAlON-Werkstoffen bei höheren Temperaturen kann auch durch die Zugabe von Hartstoffpartikel wie z.B. SiC gesteigert werden, wie aus der WO 2005/016847 A1 bekannt ist. WO 2005/016847 A1 zeigt somit die Kombination aus einem alpha/beta SiAlON und einem Hartstoff. Die WO 97/48659 A1 zeigt ebenfalls einen SiAlON-Werkstoff aus einem alpha/beta-SiAlOn und Hartstoffen.The hardness of SiAlON materials at higher temperatures can also be increased by the addition of hard particles such as SiC, such as from the WO 2005/016847 A1 is known. WO 2005/016847 A1 thus shows the combination of an alpha / beta SiAlON and a hard material. The WO 97/48659 A1 also shows a SiAlON material made of an alpha / beta-SiAlOn and hard materials.

In der EP 0 479 485 A1 wird beschrieben, wie ein SiC-verstärkter beta-SiAlON-Werkstoff durch die Zugabe von 1 bis 60 Masse% HfO2 leichter verdichtet werden kann, ohne dass der zusätzliche HfO2-Zusatz die Hochtemperatur-Eigenschaften negativ beeinflusst. Das HfO2 bildet beim Sintern eine flüssige Phase, die die Verdichtung fördert, nach dem Sinterprozess aber als „disperse Phase“ vorliegt.In the EP 0 479 485 A1 describes how a SiC-reinforced beta-SiAlON material can be more easily compacted by the addition of 1 to 60% by mass HfO 2 , without the additional HfO 2 addition adversely affecting the high-temperature properties. The HfO 2 forms a liquid phase during sintering, which promotes the compression, but after the sintering process is present as a "disperse phase".

In der US 5,200,374 A wird beschrieben, dass sich bei Zugabe von HfO2 nach dem Sintern eine Hf-Oxid-Phase mit Defekt-Fluorit-Struktur bildet, in der dreiwertige Ionen, wie z.B. Seltenerde-Elemente, eingelagert sind.In the US 5,200,374 A It is described that upon addition of HfO 2 after sintering, a Hf oxide phase having a defect fluorite structure is formed, in which trivalent ions such as rare earth elements are incorporated.

Auch in anderen Veröffentlichungen wie in der EP 0 227 471 A2 und der EP 0 792 854 A2 wird beschrieben, wie HfO2 oder ein ähnlicher Zusatz beigegeben werden kann, um bei einem schwer zu verdichtenden Werkstoff eine ausreichende Enddichte zu erreichen. In jedem Fall wird jedoch, wie insbesondere aus der EP 0 479 485 A2 bekannt, eine Mindestmenge von 1 Masse% HfO2 als notwendig angesehen, um eine merkbare Verbesserung des Verdichtungsverhaltens zu erzielen.Also in other publications as in the EP 0 227 471 A2 and the EP 0 792 854 A2 describes how HfO 2 or a similar additive can be added to achieve a sufficient final density in a difficult to compact material. In any case, however, as in particular from the EP 0 479 485 A2 a minimum quantity of 1% by mass of HfO 2 is considered necessary in order to achieve a noticeable improvement in the compaction behavior.

Aufgabe der vorliegenden Erfindung ist es, einen verschleißfesten SiAlON-Werkstoff bereitzustellen, der trotz niedriger Anteile an Sinterhilfsmitteln, insbesondere Hf, anstelle des aufwändigen Heißpressens (HP) oder heißisostatischen Pressens (HIP) auch durch das wirtschaftlichere Gasdrucksintern verdichtet werden kann.The object of the present invention is to provide a wear-resistant SiAlON material which, in spite of low levels of sintering aids, in particular Hf, can also be compacted by the more economical gas pressure sintering instead of expensive hot pressing (HP) or hot isostatic pressing (HIP).

Beim erfindungsgemäßen Werkstoff auf der Basis von SiAlONen reicht bereits ein geringerer Hf-Zusatz als bei herkömmlichen SiAlON-Werkstoffen aus, um gute Sintereigenschaften und verbesserte Verschleißbeständigkeit beim Zerspanen zu erreichen. Der erfindungsgemäße Werkstoff wird bei Temperaturen von 1750 bis 2000°C gesintert. Er kann durch Gasdrucksintern auf >99% theoretische Dichte verdichtet werden.In the case of the material according to the invention based on SiAlONs, a lower Hf addition is already sufficient than with conventional SiAlON materials in order to achieve good sintering properties and improved wear resistance during machining. The material according to the invention is sintered at temperatures of 1750 to 2000 ° C. It can be compressed by gas pressure sintering to> 99% theoretical density.

Der erfindungsgemäße α/β-SiAlON-Werkstoff enthält 5 bis 50 Masse%, bevorzugt 5 bis 30% Masse% α/(α+β) RE-α-SiAlON, wobei RE für mindestens ein Kation aus Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Mg oder Ca, bevorzugt mindestens ein Kation aus Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb und zusätzlich mindestens ein Kation aus Mg oder Ca steht, sowie 95 bis 50 Masse%, bevorzugt 95 bis 70 Masse% β/(α+β) β-SiAlON und einer Hf-haltigen amorphen oder teil-kristallinen Korngrenzenphase mit einem Anteil am Gesamtwerkstoff von unter 10 Vol%. Der Hf-Gehalt des gesinterten Werkstoffs beträgt 0,4 bis 0,6 Masse%. Die Dispersionsphase enthält globulare Partikeln mit mittleren Partikelgrößen von 0,2 bis 15 µm, bevorzugt 0,4 bis 10 µm aus mindestens einem Hartstoff aus SiC, TiN, TiC, Ti(C,N), Carbide und/oder Nitride der Elemente der Gruppen IVb, Vb und VIb des Periodensystems (PSE) sowie Scandiumcarbid und/oder Scandiumoxicarbid oder Mischungen aus den aufgeführten Hartstoffen, die in einem Anteil von 5 bis 30 Vol%, bevorzugt 7,5 bis 20 Vol%, besonders bevorzugt 10 bis 15% Vol% im Sinterkörper enthalten sind.The α / β-SiAlON material according to the invention contains 5 to 50% by mass, preferably 5 to 30% by mass% α / (α + β) RE-α-SiAlON, where RE is at least one cation from Y, Sc, Lu, La , Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Mg or Ca, preferably at least one cation of Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and additionally at least one cation of Mg or Ca, and 95 to 50% by mass, preferably 95 to 70% by mass β / (α + β) β-SiAlON and an Hf-containing amorphous or partially crystalline grain boundary phase with a share of the total material of less than 10% by volume. The Hf content of the sintered material is 0.4 to 0.6 mass%. The dispersion phase contains medium-particle globular particles Particle sizes of 0.2 to 15 .mu.m, preferably 0.4 to 10 .mu.m of at least one hard material of SiC, TiN, TiC, Ti (C, N), carbides and / or nitrides of the elements of groups IVb, Vb and VIb of the Periodic Table (PSE) and scandium carbide and / or Scandiumoxicarbid or mixtures of the listed hard materials, which are contained in a proportion of 5 to 30% by volume, preferably 7.5 to 20% by volume, particularly preferably 10 to 15% by volume in the sintered body.

Die Rohstoffmischung des α/β-SiAlON-SiC-Werkstoffs enthält die Komponenten Si3N4, Al2O3, AlN, MgO, Y2O3, HfO2 und SiC, wobei der Anteil an SiC 5 bis 30 Vol%, bevorzugt 7,5 bis 20 Vol%, besonders bevorzugt 10 bis 15 Vol%, der Anteil an HfO2 0,2 bis 1,0 Masse%, bevorzugt 0,3 bis 0,9 Masse%, besonders bevorzugt 0,4 bis 0,8 Masse%, der Gesamt-Additiv-Anteil 6,0 bis 10,0, bevorzugt 6,5 bis 9,0, besonders bevorzugt 7,0 bis 8,5 und das Atom%-Verhältnis von Y zu Mg 7,0 bis 10,0, bevorzugt 7,5 bis 9,0, besonders bevorzugt 8,0 bis 8,5 beträgt.The raw material mixture of the α / β-SiAlON-SiC material contains the components Si 3 N 4 , Al 2 O 3 , AlN, MgO, Y 2 O 3 , HfO 2 and SiC, the proportion of SiC being 5 to 30% by volume, preferably 7.5 to 20% by volume, particularly preferably 10 to 15% by volume, the proportion of HfO 2 is 0.2 to 1.0% by mass, preferably 0.3 to 0.9% by mass, particularly preferably 0.4 to 0 , 8 mass%, the total additive content 6.0 to 10.0, preferably 6.5 to 9.0, particularly preferably 7.0 to 8.5 and the atomic% ratio of Y to Mg 7.0 to 10.0, preferably 7.5 to 9.0, particularly preferably 8.0 to 8.5.

HfO2 besitzt in der Schmelzphase der sonstigen Sinteradditive eine geringe Löslichkeit, die von der Zusammensetzung der Ausgangsmischung abhängt. Beim Abkühlen scheidet sich das gelöste Hf teilweise als eine fein verteilte kristalline Hf-Phase in der Korngrenzenphase aus. Der Zusatz einer geringen Menge an Hf-Oxid erhöht also die Menge an Schmelzphase während des Sintervorgangs, führt aber nicht zu mehr glasartiger Korngrenzenphase im Produkt. Damit besteht eine Möglichkeit, die Menge der sonstigen Sinteradditive zu verringern, ohne die Sinterfähigkeit zu verschlechtern. Überschüssiges HfO2, was sich nicht in der Flüssigphase lösen kann, kann beim Sintern durch eine N2-reiche Atmosphäre in dispers verteilte Hf-Nitride umgewandelt werden.HfO 2 has a low solubility in the melt phase of the other sintering additives, which depends on the composition of the starting mixture. Upon cooling, the dissolved Hf partially precipitates as a finely divided crystalline Hf phase in the grain boundary phase. The addition of a small amount of Hf oxide thus increases the amount of melt phase during the sintering process, but does not lead to more glassy grain boundary phase in the product. Thus, there is a possibility to reduce the amount of other sintering additives without deteriorating the sinterability. Excess HfO 2 , which can not dissolve in the liquid phase, can be converted by sintering through a N 2 -rich atmosphere into dispersed Hf nitrides.

Nur durch die Zugabe von HfO2 bei gleichzeitig leicht verringerter Menge an sonstigen Additiven kann eine merkliche Verbesserung im Verschleißverhalten festgestellt werden, wie an Hand von Ausführungsbeispielen (siehe Tabelle 2) bewiesen wird. Ein Zusatz von mehr als 1 Masse% HfO2 verschlechtert dagegen die Werkstoffeigenschaften, wie anhand von Beispielen gezeigt wird. Die gleichzeitige Verwendung von Sinteradditiven mit unterschiedlichen Kationen, wie beispielsweise Y und Mg der Ausführungsbeispiele, beeinflusst, zusätzlich zum Hf-Zusatz, das Sinterverhalten positiv. Es wird jedoch vermutet, dass auch bei Rohstoffmischungen mit nur einem Kation ein zusätzlicher Hf-Zusatz die beschriebenen Vorteile bewirkt.Only by the addition of HfO 2 at the same time slightly reduced amount of other additives, a significant improvement in the wear behavior can be found, as demonstrated by means of embodiments (see Table 2). In contrast, addition of more than 1% by mass of HfO 2 deteriorates the material properties, as shown by examples. The simultaneous use of sintering additives with different cations, such as Y and Mg of the embodiments, in addition to the Hf additive, the sintering behavior positively. However, it is believed that even with raw material blends with only one cation, an additional Hf addition causes the benefits described.

Das Hf kann statt als Oxid auch in anderer Form als organische oder inorganische Verbindung eingebracht werden. Wird das Hf als pulverförmige Verbindung, z.B. als HfO2, eingebracht, sollte die Größe der Pulverteilchen nur wenige µm betragen. Sind die Pulverteilchen zu grob, lösen sie sich während des Sinterns nur langsam auf und tragen damit kaum zur Erhöhung der Flüssigphase bei, was keine Verbesserung der Sintereigenschaften bewirkt.Instead of being an oxide, the Hf can also be introduced in other forms as an organic or inorganic compound. If the Hf is introduced as a pulverulent compound, for example as HfO 2 , the size of the powder particles should be only a few μm. If the powder particles are too coarse, they dissolve only slowly during sintering and thus hardly contribute to increasing the liquid phase, which does not improve the sintering properties.

Nach dem Sintern können mit herkömmlichen röntgenographischen Analyseverfahren, beispielsweise XRD, keine oder nur sehr schwache Anzeichen für das Vorhandensein einer kristallinen Hf-Oxid-Phase detektiert werden, da deren Gehalte zu gering sind, d.h. kleiner als etwa 1 Masse%. Je nach Sinterbedingungen können jedoch geringe Mengen an Hf-Oxinitrid- oder Hf-Nitrid-Phasen nachgewiesen werden, die bei hohen Hf-Gehalten sogar im REM als disperse Teilchen mit etwa 0,5 µm Durchmesser sichtbar sind.After sintering, no or very faint signs of the presence of a crystalline Hf oxide phase can be detected by conventional X-ray analysis methods, such as XRD, because their contents are too low, i.e., less than 90%. less than about 1 mass%. Depending on the sintering conditions, however, small amounts of Hf-oxynitride or Hf-nitride phases can be detected, which are visible even at high Hf levels even in the SEM as disperse particles with about 0.5 microns in diameter.

Außer SiC sind auch alle anderen Hartstoffpartikel möglich, die mit den anderen Komponenten des erfindungsgemäßen Werkstoffs keine Reaktionen eingehen. Allerdings ist die Größe der beigegebenen Hartstoffpartikel zu beachten. Wenn diese zu klein sind, unter 0,2 µm, wird wegen der großen Pulver-Oberfläche viel Glasphase zur Benetzung benötigt, die beim Sintern fehlt. Sind die Hartstoffpartikel zu grob, etwa im Bereich von über 15 µm, erfolgt eine Sinterbehinderung.Apart from SiC, all other hard material particles are possible which do not react with the other components of the material according to the invention. However, the size of the added hard particles is to be observed. If these are too small, below 0.2 μm, a large amount of glass phase is required for wetting due to the large powder surface, which is missing during sintering. If the hard material particles are too coarse, for example in the range of more than 15 μm, there is a sintering obstruction.

Anhand von Ausführungsbeispielen wird die Erfindung näher erläutert. Es wurden drei Werkstoffgruppen gebildet, die in den nachfolgenden Tabellen 1 und 2 aufgeführt sind. Aus den jeweiligen Werkstoffen wurden Sinterkörper in der Form von Schneidwerkzeugen hergestellt. Es wurde die Auswirkung der Zugabe von HfO2 zu Y-Mg-alpha/beta-SiAlON-Werkstoffen unterschiedlicher Zusammensetzung auf das Sinterverhalten und den Verschleiß beim Zerspanen verglichen.Reference to exemplary embodiments, the invention is explained in detail. Three groups of materials were formed, which are listed in Tables 1 and 2 below. From the respective materials sintered bodies were produced in the form of cutting tools. The effect of adding HfO 2 to Y-Mg-alpha / beta-SiAlON materials of different composition on sintering behavior and wear during cutting was compared.

Zur Herstellung eines erfindungsgemäßen SiAlON-Werkstoffs der Ausführungsbeispiele wurde feines bzw. fein gemahlenes Si3N4-Pulver mit einer Korngröße von D50 ≤ 1 µm und mit einer spezifischen Oberfläche ≥ 10 m2/g sowie SiC als Hartstoffpartikel mit einer Korngröße von D50 etwa 0,6 µm unter Zusatz der übrigen pulverförmigen Rohstoffe und bekannter Bindemittel gemischt und axial gepresst.To produce a SiAlON material according to the invention of the embodiments, fine or finely ground Si 3 N 4 powder with a particle size of D50 ≤ 1 microns and with a specific surface ≥ 10 m 2 / g and SiC as a hard material particles with a particle size of D50 about 0.6 microns with the addition of the other powdery raw materials and known binder mixed and pressed axially.

Nach dem Entbindern erfolgte das Sintern. Die Ausführungsbeispiele wurden alle mittels Gasdrucksintern bei 1930°C und einem Gasdruck von 100 bar hergestellt. Die Haltezeit betrug drei Stunden. After debinding, the sintering took place. The embodiments were all prepared by gas pressure sintering at 1930 ° C and a gas pressure of 100 bar. The holding time was three hours.

Aus dem Werkstoff wurden Schneidwerkzeuge hergestellt, mit denen an Bremsscheiben aus dem Werkstoff GG15 Zerspantests durchgeführt wurden. Dabei wurden die Bremsscheiben mit einer Schnittgeschwindigkeit von vc = 1000 m/min, einem Vorschub von f = 0,50 mm/U, einer Schnitttiefe von ap = 2,0 mm und einem Einstellwinkel von a = 85° abgedreht. Tabelle 1: Ausführungsbeispiele: Daten der Rohstoffmischung Rohstoffmischung Gruppe Nr: Si3N4 [Masse-%] AIN [Masse%] Atom%-Verhältnis Y: Mg Gesamt-Additiv-Gehalt [Masse-%] (1) Hf [Masse-%] SiC [Vol.-%] A 1 (Ref.) 89,5 5,00 7,5 10,5 - - A 2 88,5 5,00 7,5 11,5 0,85 - A 3 85,5 5,00 7,5 14,5 3,39 - B 4 (Ref.) 66,0 4,14 9,0 9,3 - 25 B 5 65,0 4,14 9,0 10,3 0,85 25 B 6 65,3 4,14 9,0 10,0 0,42 25 C 7 (Ref.) 80,8 4,14 9,0 9,3 - 10 C 8 81,1 4,14 8,5 9,0 0,85 10 C 9 81,3 4,14 8,3 8,8 0,76 10 C 10 81,7 4,14 8,3 8,4 0,69 10 C 11 82,4 4,14 8,2 7,7 0,58 10 C 12 83,2 4,14 9,2 6,9 0,46 10 (1) Entspricht der Menge von AlN+Al2O3+MgO+Y2O3+HfO2, den Stoffen, die beim Sintern die flüssige Phase bilden (Oxid-Verunreinigung des Si3N4 oder AIN bleiben unberücksichtigt). Das Masse%-Verhältnis zwischen Al2O3 und MgO beträgt stets 2,53. Tabelle 2: Ausführungsbeispiele: Eigenschaften Eigenschaften Werkstoff Gruppe Nr: Dichte [% th.] Alpha-SiAlON [Masse-%] (2) Härte [HV10] Zähigkeit KIC [MPam1/2] Verschleiß bzgl. Referenz A 1 (Ref.) 99,8 42 1782 6,3 1 A 2 99,8 38 1697 5,9 - *) A 3 99,7 19 1582 6,3 - *) B 4 (Ref.) 99,8 25 2053 6,3 1 B 5 99,8 33 1897 5,8 1,06 B 6 99,8 41 1893 6,1 1,03 C 7 (Ref.) >99,8 30 1746 6,3 1 C 8 >99,8 17 1707 5,8 0,96 C 9 >99,8 20 1758 6,0 0,94 C 10 >99,8 20 -*) -*) -*) C 11 >99,8 18 1744 5,8 0,81 C 12 88 -*) -*) -*) -*) *) nicht bestimmt (2) Im gesinterten Bauteil; Anteil von alpha-SiAlON, bezogen auf die Gesamtmenge von alpha- und beta-SiAION, d.h. α/(α+β) in Masse%. The material was used to produce cutting tools with which Zerspantests were carried out on brake discs made of the material GG15. The brake disks were turned off at a cutting speed of vc = 1000 m / min, a feed of f = 0.50 mm / rev, a cutting depth of ap = 2.0 mm and a setting angle of a = 85 °. Table 1: Exemplary embodiments: data of the raw material mixture raw material mixture group No: Si 3 N 4 [mass%] AIN [mass%] Atom% ratio Y: Mg Total additive content [% by mass] (1) Hf [mass%] SiC [vol.%] A 1 (Ref.) 89.5 5.00 7.5 10.5 - - A 2 88.5 5.00 7.5 11.5 0.85 - A 3 85.5 5.00 7.5 14.5 3.39 - B 4 (Ref.) 66.0 4.14 9.0 9.3 - 25 B 5 65.0 4.14 9.0 10.3 0.85 25 B 6 65.3 4.14 9.0 10.0 0.42 25 C 7 (Ref.) 80.8 4.14 9.0 9.3 - 10 C 8th 81.1 4.14 8.5 9.0 0.85 10 C 9 81.3 4.14 8.3 8.8 0.76 10 C 10 81.7 4.14 8.3 8.4 0.69 10 C 11 82.4 4.14 8.2 7.7 0.58 10 C 12 83.2 4.14 9.2 6.9 0.46 10 (1) Corresponds to the amount of AlN + Al 2 O 3 + Y 2 O 3 + MgO + HfO 2, the substances which form the liquid phase during sintering (Me oxide contamination of the Si 3 N 4 or AIN disregarded). The mass% ratio between Al 2 O 3 and MgO is always 2.53. Table 2: Exemplary embodiments: Properties Properties Material group No: Density [% th.] Alpha-SiAlON [% by mass] (2) Hardness [HV10] Toughness K IC [MPam 1/2 ] Wear with reference A 1 (Ref.) 99.8 42 1782 6.3 1 A 2 99.8 38 1697 5.9 - *) A 3 99.7 19 1582 6.3 - *) B 4 (Ref.) 99.8 25 2053 6.3 1 B 5 99.8 33 1897 5.8 1.06 B 6 99.8 41 1893 6.1 1.03 C 7 (Ref.) > 99.8 30 1746 6.3 1 C 8th > 99.8 17 1707 5.8 0.96 C 9 > 99.8 20 1758 6.0 0.94 C 10 > 99.8 20 - *) - *) - *) C 11 > 99.8 18 1744 5.8 0.81 C 12 88 - *) - *) - *) - *) *) not determined (2) In the sintered component; Amount of alpha-SiAlON, based on the total amount of alpha- and beta-SiAION, ie α / (α + β) in mass%.

Gruppe A (Nr.1 bis 3):Group A (Nos. 1 to 3):

Der Einfluss der Zugabe von HfO2 zu einer α/β-SiAlON-Zusammensetzung: Die Härte sinkt, die Zähigkeit wird nicht signifikant verändert. Zerspantests wurden wegen der niedrigen Härte nicht durchgeführt. Eine zusätzliche Hf-Zugabe zu einer herkömmlichen SiAION-Zusammensetzung verschlechtert also die Härte, was sich unmittelbar auf einen höheren Verschleiß beim Zerspanen auswirken würde.Influence of adding HfO 2 to an α / β-SiAlON composition: The hardness decreases, the toughness is not significantly changed. Zerspantests were not performed because of the low hardness. Additional Hf addition to a conventional SiAION composition thus worsens the hardness, which would directly affect a higher wear during machining.

Gruppe B (Nr.4 bis 6):Group B (Nos. 4 to 6):

Der Einfluss der Zugabe von HfO2 zu einem SiC-haltigen α/β-SiAlON: Hier sinkt trotz des hohen SiC-Anteils die Härte ebenfalls merklich ab. Der Verschleiß gegenüber der Hf-freien Zusammensetzung ist erhöht. Die Sinterfähigkeit des hoch hartstoff-haltigen SiAlONs wird durch den geringen Hf-Zusatz nicht merklich verbessert.The influence of the addition of HfO 2 to a SiC-containing α / β-SiAlON: Here, despite the high SiC content, the hardness also drops markedly. The wear on the Hf-free composition is increased. The sinterability of the highly hard-containing SiAlONs is not significantly improved by the low Hf addition.

Gruppe C (Nr.7 bis 12):Group C (Nos. 7 to 12):

Der Einfluss der Zugabe von HfO2 zu einem SiC-haltigen SiAlON, bei dem der Gesamtadditivgehalt, d.h. die Summe aller eine Schmelze bildenden Zusätze der Rohstoffmischung, trotz zusätzlicher HfO2-Zugabe nicht erhöht wird: Die herkömmliche Sinteradditivmenge wird reduziert und als Ausgleich HfO2 zugegeben, das, wie oben beschrieben, beim Sintern die Menge an der Flüssigphase erhöht, beim Abkühlen jedoch kristallisiert und eine hochtemperatur-stabile KorngrenzenPhase bewirkt. Die Ausgleichsmenge an HfO2 kann sogar geringer sein als die reduzierte Menge der übrigen Sinteradditive. Die Härte wird nicht merklich beeinflusst, der Verschleiß jedoch erniedrigt. Das bessere Verschleißverhalten wird in diesem Fall verursacht durch den niedrigeren Gehalt an amorpher KorngrenzenPhase, was eine bessere Warmhärte und geringere chemische Reaktionen mit dem Werkstoff des Werkstücks bewirkt.The influence of the addition of HfO 2 to a SiC-containing SiAlON, in which the total additive, ie the sum of all melt-forming additives of the raw material mixture, despite additional HfO 2 addition is not increased: The conventional Sinteradditiv amount is reduced and in compensation HfO 2 is added, which, as described above, increases the amount of the liquid phase during sintering, but crystallizes on cooling and causes a high-temperature stable grain boundary phase. The compensation amount of HfO 2 may even be lower than the reduced amount of the remaining sintering additives. The hardness is not significantly affected, but the wear is reduced. The better wear behavior is in this case caused by the lower content of amorphous grain boundary phase, which causes a better hot hardness and lower chemical reactions with the material of the workpiece.

Claims (9)

Werkstoff auf der Basis von SiAlONen, enthaltend einen α/β-SiAlON-Werkstoff mit 5 bis 50% Masse%, bevorzugt 5 bis 30% Masse% α/(α+β) RE-α-SiAlON, wobei RE für mindestens ein Kation aus Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Mg oder Ca, bevorzugt mindestens ein Kation aus Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb und zusätzlich mindestens ein Kation aus Mg oder Ca steht, sowie 95 bis 50 Masse% , bevorzugt 95 bis 70 Masse% β/(α+β) β-SiAION und einer Hf-haltigen amorphen oder teil-kristallinen Korngrenzenphase mit einem Anteil am Gesamtwerkstoff von unter 10 Vol%, wobei der Hf-Gehalt des gesinterten Werkstoffs 0,4 bis 0,6 Masse% beträgt und einer Dispersionsphase, bestehend aus globularen Partikeln mit mittleren Partikelgrößen von 0,2 bis 15 µm, bevorzugt 0,4 bis 10 µm aus mindestens einem Hartstoff aus SiC, TiN, TiC, Ti(C,N), Carbide und/oder Nitride der Elemente der Gruppen IVb, Vb und Vlb des Periodensystems (PSE) sowie Scandiumcarbid und/oder Scandiumoxicarbid oder Mischungen aus den aufgeführten Hartstoffen, die in einem Anteil von 5 bis 30 Vol%, bevorzugt 7,5 bis 20 Vol%, besonders bevorzugt 10 bis 15 Vol% im Sinterkörper enthalten sind.SiAlON-based material containing an α / β-SiAlON material having 5 to 50% mass%, preferably 5 to 30% mass% α / (α + β) RE-α-SiAlON, where RE is at least one cation from Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Mg or Ca, preferably at least one cation of Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and additionally at least one cation of Mg or Ca, and 95 to 50 mass%, preferably 95 to 70 mass % β / (α + β) β-SiAION and an Hf-containing amorphous or partially crystalline grain boundary phase with a total material content of less than 10% by volume, the Hf content of the sintered material being from 0.4 to 0.6% by mass is and a dispersion phase consisting of globular particles having average particle sizes of 0.2 to 15 microns, preferably 0.4 to 10 microns of at least one hard material of SiC, TiN, TiC, Ti (C, N), carbides and / or nitrides the elements of groups IVb, Vb and Vlb of the periodic table (PSE) sow Scandium carbide and / or Scandiumoxicarbid or mixtures of the listed hard materials which are contained in a proportion of 5 to 30% by volume, preferably 7.5 to 20% by volume, particularly preferably 10 to 15% by volume in the sintered body. Werkstoff nach Anspruch 1, dadurch gekennzeichnet, dass das Si3N4-Pulver eine spezifische Oberfläche von ≥ 10 m2/g aufweist.Material after Claim 1 , characterized in that the Si 3 N 4 powder has a specific surface area of ≥ 10 m 2 / g. Werkstoff nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Hartstoffpartikel eine Korngröße zwischen 0,2 µm und 15 µm aufweisen.Material after Claim 1 or 2 , characterized in that the hard material particles have a particle size between 0.2 microns and 15 microns. Werkstoff nach Anspruch 3, dadurch gekennzeichnet, dass die Korngröße von zugegebenem SiC bei 0,6 µm liegt.Material after Claim 3 , characterized in that the grain size of added SiC is 0.6 microns. Werkstoff nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass die theoretische Dichte größer als 99 % ist.Material according to one of Claims 1 to 4 , characterized in that the theoretical density is greater than 99%. Sinterkörper, hergestellt aus einem Werkstoff nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass er ein Schneidwerkzeug ist.Sintered body made of a material according to one of Claims 1 to 5 , characterized in that it is a cutting tool. Verfahren zur Herstellung eines Werkstoff auf der Basis von SiAlONen, enthaltend einen α/β-SiAlON-Werkstoff mit 5 bis 50% Masse%, bevorzugt 5 bis 30% Masse% α/(α+β) RE-α-SiAION, wobei RE für mindestens ein Kation aus Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Mg oder Ca, bevorzugt mindestens ein Kation aus Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb und zusätzlich mindestens ein Kation aus Mg oder Ca steht, sowie 95 bis 50% Masse%, bevorzugt 95 bis 70 Masse% α/(α+β) β-SiAlON und einer Hf-haltigen amorphen oder teil-kristallinen Korngrenzenphase mit einem Anteil am Gesamtwerkstoff von unter 10 Vol%, wobei der Hf-Gehalt des gesinterten Werkstoffs 0,2 bis 1,0 Masse%, bevorzugt 0,3 bis 0,8 Masse%, besonders bevorzugt 0,4 bis 0,6 Masse% beträgt und einer Dispersionsphase, bestehend aus globularen Partikeln mit mittleren Partikelgrößen von 0,2 bis 15 µm, bevorzugt 0,4 bis 10 µm aus mindestens einem Hartstoff aus SiC, TiN, TiC, Ti(C,N), Carbide und/oder Nitride der Elemente der Gruppen IVb, Vb und VIb des Periodensystems (PSE) sowie Scandiumcarbid und/oder Scandiumoxicarbid oder Mischungen aus den aufgeführten Hartstoffen, die in einem Anteil von 5 bis 30 Vol%, bevorzugt 7,5 bis 20 Vol%, besonders bevorzugt 10 bis 15 Vol% im Sinterkörper enthalten sind, durch Axialpressen eines binderhaltigen Pressgranulats bei 140 bis 200 MPa, Entbindern bei auf den Binder abgestimmten Temperaturen und anschließendem Sintern, gegebenenfalls Drucksintern oder HIP, bei Temperaturen zwischen 1750 °C und 2000 °C.A method of producing a material based on SiAlONs, comprising an α / β-SiAlON material having 5 to 50% by mass, preferably 5 to 30% by mass% α / (α + β) RE-α-SiAION, where RE for at least one cation of Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Mg or Ca, preferably at least one cation of Y, Sc, Lu, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and additionally at least one cation of Mg or Ca, and 95 to 50% mass%, preferably 95 to 70 mass% α / (α + β) β-SiAlON and a Hf-containing amorphous or partially crystalline grain boundary phase with a total material content of less than 10% by volume, wherein the Hf content of the sintered material 0.2 to 1.0% by mass, preferably 0.3 to 0.8% by mass, particularly preferably 0.4 to 0.6% by mass, and a dispersion phase consisting of globular particles having average particle sizes of 0.2 to 15 μm, preferably 0 , 4 to 10 microns of at least one hard material of SiC, TiN, TiC, Ti (C, N), carbides and / or nitrides of the elements of groups IVb, Vb and VIb of the Periodic Table (PSE) as well as scandium carbide and / or scandium oxycarbide or mixtures of the listed hard materials, in an amount of 5 to 30% by volume 7.5 to 20% by volume, more preferably 10 to 15% by volume in the sintered body, by axial pressing of a binder-containing granules at 140 to 200 MPa, debindering at temperatures matched to the binder and subsequent sintering, optionally pressure sintering or HIP, at temperatures between 1750 ° C and 2000 ° C. Verfahren nach Anspruch 7, dadurch gekennzeichnet, dass eine Rohstoffmischung des α/β-SiAlON-SiC-Werkstoffs der Zusammensetzung α/β-SiAlON und α/(α+β) RE-α-SiAION aus den Komponenten Si3N4, Al2O3, AlN, MgO, Y2O3, HfO2 und Hartstoffpartikeln von SiC, TiN, TiC, Ti(C,N), Carbide und/oder Nitride der Elemente der Gruppen IVb, Vb und VIb des Periodensystems (PSE) sowie Scandiumcarbid und/oder Scandiumoxicarbid oder Mischungen aus den aufgeführten Hartstoffen in einer Korngröße von 0,2 µm bis 15 µm mit einem Anteil von 5 bis 30 Vol%, bevorzugt 7,5 bis 20 Vol%, besonders bevorzugt 10 bis 15 Vol% und einem Anteil an HfO2 von 0,2 bis 1,0 Masse%, bevorzugt 0,3 bis 0,9 Masse%, besonders bevorzugt 0,4 bis 0,8 Masse%, hergestellt wird, wobei der Gesamt-Additiv-Anteil 6,0 bis 10,0, bevorzugt 6,5 bis 9,0, besonders bevorzugt 7,0 bis 8,5 und das Atom%-Verhältnis von Y zu Mg 7,0 bis 10,0, bevorzugt 7,5 bis 9,0, besonders bevorzugt 8,0 bis 8,5 beträgt und das Si3N4-Pulver eine Korngröße von D50 ≤ 1 µm und eine spezifische Oberfläche ≥ 10 m2/g hat.Method according to Claim 7 , characterized in that a raw material mixture of the α / β-SiAlON-SiC material of the composition α / β-SiAlON and α / (α + β) RE-α-SiAION from the components Si 3 N 4 , Al 2 O 3 , AlN, MgO, Y 2 O 3 , HfO 2 and hard material particles of SiC, TiN, TiC, Ti (C, N), carbides and / or nitrides of the elements of groups IVb, Vb and VIb of the Periodic Table (PSE) as well as scandium carbide and / or Scandiumoxicarbid or mixtures of the listed hard materials in a particle size of 0.2 microns to 15 microns with a proportion of 5 to 30% by volume, preferably 7.5 to 20% by volume, particularly preferably 10 to 15% by volume and a proportion of HfO 2 from 0.2 to 1.0% by weight, preferably 0.3 to 0.9% by weight, more preferably 0.4 to 0.8% by weight, wherein the total additive content is 6.0 to 10 , 0, preferably 6.5 to 9.0, particularly preferably 7.0 to 8.5 and the atomic% ratio of Y to Mg 7.0 to 10.0, preferably 7.5 to 9.0, particularly preferably 8.0 to 8.5, and the Si 3 N 4 powder has a grain size of D 50 ≤ 1 μm and a specific surface ≥ 10 m 2 / g. Verfahren nach Anspruch 7 oder 8, dadurch gekennzeichnet, dass das Gasdrucksintern bei 1930 °C und 100 bar Gasdruck in einer Haltezeit von 3 Stunden erfolgt.Method according to Claim 7 or 8th , characterized in that the gas pressure sintering takes place at 1930 ° C and 100 bar gas pressure in a holding time of 3 hours.
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