WO2018145900A1 - Schlicker, prepreg, sowie daraus aufgebautes laminat daraus hergestellter grünkörper und cmc-turbinenkomponente - Google Patents

Schlicker, prepreg, sowie daraus aufgebautes laminat daraus hergestellter grünkörper und cmc-turbinenkomponente Download PDF

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Publication number
WO2018145900A1
WO2018145900A1 PCT/EP2018/051692 EP2018051692W WO2018145900A1 WO 2018145900 A1 WO2018145900 A1 WO 2018145900A1 EP 2018051692 W EP2018051692 W EP 2018051692W WO 2018145900 A1 WO2018145900 A1 WO 2018145900A1
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Prior art keywords
slip
ceramic powder
mineral
prepreg
polyol
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PCT/EP2018/051692
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English (en)
French (fr)
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Gia Khanh Pham
Steffen Walter
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Siemens Aktiengesellschaft
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Publication of WO2018145900A1 publication Critical patent/WO2018145900A1/de

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Definitions

  • the invention relates to a slip, a prepreg, a laminate, a green body and a product made therefrom
  • Ceramic Matrix Composites are increasingly being used to produce highly stressed components, in particular high-temperature components such as turbine components.
  • CMCs are fiber-reinforced CMCs, Continuous Fiber Reinforced Ceramic Matrix Composites (CFCC) and given ⁇ possibly also with short fibers combined Ceramic Fiber
  • Entspre ⁇ sponding CFCC prepregs are usually on the impregnation tion of fibers, fiber fabrics and / or fiber composites - prepared with slip - in each case matching the component to be manufactured.
  • glycerol used in the starting materials for CMC turbine components is from Kemr M., Mizuhara H., San Mateo
  • WO 2016/016388 Al a method for producing a slip for a CMC material, in particular a ⁇ sondere for forming a CMC prepreg laminate ⁇ be known.
  • the method known from WO 2016016388 has the disadvantage that at least an amount of 10 to 20% by weight, based on the total weight of ceramic powder, of glycerol in the slip is used.
  • a disadvantage of a high content of glycerol is that the drying of the prepreg, the lamination of the prepregs and finally the production of the turbine component take a longer time.
  • the object of the present invention is to provide a slip in which the proportion of glycerol in the slip, based on the ceramic powder, is reduced. This object is achieved by the subject matter of the present ⁇ invention as disclosed in the specification and the claims.
  • the subject matter of the present invention is a slip, that is to say a mineral-water mixture, comprising the following components:
  • the invention relates to a prepreg Kera ⁇ mix fibers in the form of fibers, continuous fibers, fiber tissue and / or fiber composites comprising impregnated with a slurry having the above composition comprising.
  • the subject matter of the invention is a laminate comprising several prepregs laminated together with the abovementioned composition.
  • a green body which can be produced by drying said laminate in the drying oven or by drying, curing and compression, is the subject of the present invention.
  • a turbine component obtainable by sintering the green body described above is still the subject of the present invention.
  • the ceramic powder used here is present in the slip, in the prepreg, in the green body and in the finished CMC component.
  • all ceramic powders can be used, but it is particularly preferred that the material of the ceramic powder is compatible with that of the reinforcing fibers, that is to say it can be mixed indefinitely. This is for example the case if the powder and the fiber are two different Modifikatio ⁇ NEN a chemical compound.
  • the ceramic powder of amorphous material and the fiber of crystalline or semi-crystalline material may be the same or a similar chemical compound.
  • fibers and ceramic powder may also be made of different compounds.
  • the ceramic powder of Al 2 O 3, insbeson ⁇ particular alpha-AI2O3, S1O2, ZrO 2, Y2O3 and / or Zr0 2 stabilized by Y 2 O 3, yttrium-aluminum-garnet, an aluminosilicate, such as mullite, silicon carbide, and / or carbon and / or any mixtures of two or more of these compounds.
  • the polyol is in the slip in an amount of 0.5 wt% to 10 wt%, preferably 3 wt% to 7 wt%, more preferably 4 wt% to 6 wt% based on the total weight of the mineral see and / or ceramic powder , in front.
  • the polyol may be in the form of a mixture of different polyols.
  • the polyols which can be used here are preferably alditols, ie noncyclic polyols of the general formula
  • glycerol 1, 2-propanediol, sorbitol, and similarity ⁇ Liche.
  • the employable herein continuous fibers are selected for example from fibers on the following material basis: Al 2 O 3, and in particular alpha-AI2O3, S1O2, ZrO 2, Y2O3 and / or ZrO 2 stabili ⁇ Siert by Y 2 O 3, yttrium-aluminum garnet, a Alumosilicate, so for example mullite, silicon carbide, and / or carbon fibers and / or any mixtures thereof.
  • the mixtures can be present as true blends as mixed compounds and / or as bundles, fabrics, composites and / or rovings of fibers of different compounds.
  • the proportion of ceramic compound, as specified above, in a fiber should be more than 90% by weight, better still more than 95% by weight of the total weight of the fiber.
  • a precursor structure for a CMC ceramic body is referred to.
  • the prepreg derived from "pre-impregnated” includes reinforcing fibers, so in particular ⁇ sondere ceramic fibers, which are contained in the produced CMC body as a structural reinforcement. These reinforcing fibers in the prepreg with a slurry, ie a mineral-water mixture impregnated.
  • the green bodies can be produced by drying in the drying cabinet or by drying, curing and compression.
  • the prepregs are dried so that the water content is reduced.
  • the glycerin and the polyol are still close in the green body unchanged, since the boiling temperatures of glycerine and polyols are much higher than that of water.
  • the reinforcing fibers in the CMC can be used as continuous fibers, short fibers, as fiber bundles, so-called rovings, for example in bundles of 100 or more fibers.
  • the ceramic powder before the prepreg is still a certain amount of a
  • the level of polyol increases the mobility of the reinforcing fibers, reinforcing fiber fabrics and / or composites during impregnation and / or drapability of the fabric
  • Prepreg in the laminate as particularly highly filled slurry are ⁇ adjustable ago.
  • the polyols are added to the ceramic powder alone and / or in admixture with the glycerine.
  • Glycerin in the slurry to produce easily processable prepregs can be used as additions for the preparation of the slip.
  • additives known to the person skilled in the art such as dispersants, surface-active substances, or surfactants, can be used as additions for the preparation of the slip.
  • the prepreg Due to the high proportion of powder, a highly viscous slicer is produced, which can be easily processed into prepreg.
  • the prepreg has good tackiness, which favors the production of the laminate, while at the same time the content of glycerol is no longer so high that the drying and / or sintering unnecessarily lengthens.
  • the resulting laminate can be easily processed by drying to green body.
  • the invention is the first time a glycerol-containing compound
  • Schlicker provided for the production of a CMC component whose content of mineral and / or ceramic powder 40% by volume or more, based on the total volume of the slurry, and / or its content of glycerol is below 10% by weight - based on the Total weight of the ceramic Pul ⁇ vers in the slip - is.

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Abstract

Die Erfindung betrifft einen Schlicker, ein Prepreg, ein Laminat, einen Grünkörper sowie eine daraus hergestellte Ceramic Matrix Composite Turbinenkomponente. Durch die Erfindung wird erstmals ein Glycerin-haltiger Schlicker zur Herstellung einer CMC-Komponente zur Verfügung gestellt, dessen Gehalt an mineralischem und/oder keramischem Pulver 40 Vol% oder mehr, bezogen auf das gesamte Volumen des Schlickers, beträgt und/oder dessen Gehalt an Glycerin unter 10 Gew% - bezogen auf das Gesamtgewicht des keramischen Pulvers im Schlicker – liegt.

Description

Beschreibung
Schlicker, Prepreg, sowie daraus aufgebautes Laminat daraus hergestellter Grünkörper und CMC-Turbinenkomponente
Die Erfindung betrifft einen Schlicker, ein Prepreg, ein Laminat, einen Grünkörper sowie eine daraus hergestellte
Ceramic Matrix Composite Turbinenkomponente. Bei der neuen Generation von Turbinenkomponenten, insbesondere von Turbinenschaufeln und/oder Turbinenblättern von Heißdampfturbinen wird zunächst ein Schlicker hergestellt, der zur Herstellung eines Prepregs, das gegebenenfalls nach er¬ folgter Laminierung, in einem Trocknungs- und folgendem Sin- terschritt zur fertigen Turbinenkomponente sinterbar ist.
Ceramic Matrix Composites, kurz CMCs, werden verstärkt zur Herstellung stark belasteter, insbesondere hochtemperatur- belasteter Bauteile wie Turbinenkomponenten eingesetzt. Dabei kommen in der Regel faserverstärkte CMCs, Continuous-Fiber- Reinforced-Ceramic-Matrix-Composites (CFCC) und gegebenen¬ falls auch mit Kurzfasern kombinierte Ceramic Fiber
Reinforced Composite (CFRC) Materialien zum Einsatz. Entspre¬ chende CFCC-Prepregs werden in der Regel über die Imprägnie- rung von Fasern, Fasergeweben und/oder Faserverbunden - jeweils passend zum herzustellenden Bauteil - mit Schlicker hergestellt .
Der Einsatz von Glycerin in den Ausgangsmaterialien für CMC- Turbinenkomponenten ist aus Kemr M., Mizuhara H., San Mateo
S: Flexible ceramic tape and method of making same US 4329271 (1982) bekannt.
Davon ausgehend ist aus der WO 2016/016388 AI ein Verfahren zur Herstellung eines Schlickers für ein CMC-Material, insbe¬ sondere eines zur Ausbildung eines CMC-Prepreg-Laminats be¬ kannt . Das aus der WO 2016016388 bekannte Verfahren hat jedoch den Nachteil, dass zumindest eine Menge von 10 bis 20 Gewichts%, bezogen auf das Gesamtgewicht an keramischem Pulver, an Gly- cerin im Schlicker eingesetzt wird.
Nachteilig an einem hohen Gehalt an Glycerin ist jedoch, dass die Trocknung des Prepregs, das Laminieren der Prepregs und schließlich auch die Herstellung der Turbinenkomponente längere Zeit brauchen.
Aufgabe der vorliegenden Erfindung ist es, einen Schlicker zu schaffen, bei dem der Anteil an Glycerin im Schlicker bezogen auf das keramische Pulver, vermindert ist. Diese Aufgabe wird durch den Gegenstand der vorliegenden Er¬ findung, wie er in der Beschreibung und den Ansprüchen offenbart ist, gelöst.
Dementsprechend ist Gegenstand der vorliegenden Erfindung ein Schlicker, also ein Mineral-Wasser-Gemisch, folgende Komponenten umfassend:
40 Vol% oder mehr, bezogen auf das gesamte Volumen des Schlickers, an mineralischem und/oder keramischem Pulver;
4 Gew% bis 8 Gew%, bezogen auf das Gesamtgewicht des minera- lischen und/oder keramischen Pulvers, an Glycerin;
0 Gew& bis 2 Gew%, bezogen auf das Gesamtgewicht des minera¬ lischen und/oder keramischen Pulvers, an organischem Binder; 0,5 Gew% bis 10 Gew%, bezogen auf das Gesamtgewicht des mine¬ ralischen und/oder keramischen Pulvers, zumindest eines
Polyols,
sowie Wasser.
Des Weiteren ist Gegenstand der Erfindung ein Prepreg, kera¬ mische Fasern in Form von Fasern, Endlosfasern, Fasergewebe und/oder Faserverbunden umfassend, die mit einem Schlicker mit der oben genannten Zusammensetzung imprägniert sind, aufweisend . Schließlich ist Gegenstand der Erfindung ein Laminat, mehrere Prepregs mit der oben genannten Zusammensetzung zusammen laminiert aufweisend. Zudem ist noch ein Grünkörper, der durch Trocknung des genannten Laminatsim Trockenschrank oder durch Trocknung, Aushärtung und Verdichtung herstellbar ist, Gegenstand der vorliegenden Erfindung. Schließlich ist eine Turbinenkomponente, erhältlich durch Sinterung des oben beschriebenen Grünkörpers, noch Gegenstand der vorliegenden Erfindung .
Das hier einsetzbare keramische Pulver liegt im Schlicker, im Prepreg, im Grünkörper und in der fertigen CMC-Komponente vor. Grundsätzlich sind alle keramischen Pulver einsetzbar, jedoch ist besonders bevorzugt, dass das Material des kerami- sehen Pulvers mit dem der Verstärkungsfasern kompatibel, also unbegrenzt mischbar ist. Dies ist beispielsweise der Fall, wenn das Pulver und die Faser zwei verschiedene Modifikatio¬ nen einer chemischen Verbindung sind. So können - wiederum beispielsweise - das keramische Pulver aus amorphem Material und die Faser aus kristallinem oder teilkristallinem Material einer gleichen oder einer ähnlichen chemischen Verbindung sein. Selbstverständlich können Fasern und keramisches Pulver auch aus verschiedenen Verbindungen gemacht sein. Beispielsweise ist das keramische Pulver aus AI2O3, insbeson¬ dere alpha- AI2O3, S1O2, ZrÜ2, Y2O3 und/oder Zr02 stabilisiert durch Y2O3, Yttrium-Aluminium-Granat, ein Alumosilikat wie beispielsweise Mullit, Siliziumcarbid, und/oder Kohlenstoff und/oder beliebige Mischungen von zwei oder mehr dieser Ver- bindungen.
Das Polyol liegt im Schlicker in einer Menge von 0,5 Gew% bis 10 Gew%, bevorzugt 3 Gew% bis 7 Gew%, insbesondere bevorzugt 4 Gew% bis 6 Gew% bezogen auf das Gesamtgewicht des minerali- sehen und/oder keramischen Pulvers, vor. Das Polyol kann als in Form einer Mischung verschiedener Polyole vorliegen. Die hier einsetzbaren Polyole sind bevorzugt Alditole, also nichtzyklische Polyole der allgemeinen Formel
CH2OH (CHOH) nCH2OH mit n=3 bis 30, insbesondere 3 bis 24, be¬ sonders bevorzugt n = 3 bis 18,
beispielsweise, Glycerol, 1, 2-propandiol, Sorbitol, und ähn¬ liche .
Die hier einsetzbaren Endlosfasern sind beispielsweise ausgewählt aus Fasern auf folgender Materialbasis: AI2O3, insbe- sondere alpha- AI2O3, S1O2, ZrÜ2, Y2O3 und/oder ZrÜ2 stabili¬ siert durch Y2O3, Yttrium-Aluminium-Granat, einem Alumosi- likat, also beispielsweise Mullit, Siliziumcarbid, und/oder Kohlenstofffasern und/oder beliebige Mischungen davon. Die Mischungen können dabei als echte Blends vorliegen als Misch- Verbindungen sein und/oder als Bündel, Gewebe, Verbünde und/oder Rovings von Fasern aus unterschiedlichen Verbindungen. Der Anteil an keramischer Verbindung, wie oben präzisiert, in einer Faser sollte dabei bei über 90 Gew%, besser noch bei über 95 Gew% des Gesamtgewichts der Faser liegen.
Als Prepreg wird vorliegend eine Vorläufer-Struktur für einen CMC-keramischen Körper bezeichnet. Das Prepreg, abgeleitet von „pre-impregnated" umfasst Verstärkungsfasern, also insbe¬ sondere keramische Fasern, die in dem herzustellenden CMC- Körper als Struktur-Verstärkung enthalten sind. Diese Verstärkungsfasern sind im Prepreg mit einem Schlicker, also einem Mineralstoff-Wasser-Gemisch imprägniert.
Aus einem Laminat von Prepregs kann beispielsweise durch Ab- legen der Prepregs auf einer Stützstruktur und/oder alternative Wege zur Bildung eines Laminats der Grünkörper durch Trocknung im Trockenschrank oder durch Trocknung, Aushärtung und Verdichtung hergestellt werden. Bei der Bildung des Laminats werden die Prepregs getrocknet, so dass sich der Wasser- gehalt verringert. In der Regel sind im Grünkörper zwar noch wasserhaltig, aber nicht mehr so stark wie die Prepregs. Das Glycerin und das Polyol sind jedoch im Grünkörper noch nahezu unverändert vorhanden, da die Siedetemperaturen des Glycerins und der Polyole weitaus höher als der des Wassers sind.
Die Verstärkungsfasern im CMC können als Endlosfasern, Kurz- fasern, als Faserbündel, so genannte Rovings, beispielsweise in Bündeln zu 100 oder mehr Fasern.
Gemäß der vorliegenden Erfindung wird dem keramischen Pulver vor der Prepregbildung noch eine gewisse Menge an einem
Polyol und nicht mehr als 8 Gew% Glycerin zugesetzt, damit die Trocknung/Sinterung der CMC-Komponente schneller erfolgt.
Zusätzlich erhöht der Anteil an Polyol die Beweglichkeit der Verstärkungsfasern, Verstärkungsfasergewebe und/oder Verbünde während der Imprägnierung und/oder die Drapierfähigkeit des
Prepregs im Laminat, da besonders hochgefüllte Schlicker her¬ stellbar sind.
Die Polyole werden allein und/oder in Mischung mit dem Glyce- rin zum keramischen Pulver zugegeben.
Durch die Zugabe der Polyole ist Schlicker mit hohem Anteil an keramischem Pulver herstellbar. Beispielsweise konnte ein Schlicker mit einem Anteil von über 40 Vol%, insbesondere von über 45Vol% an keramischem Pulver hergestellt werden. Durch die Zugabe an Polyolen reicht ein geringer Wasser- und
Glycerinanteil im Schlicker um gut verarbeitbare Prepregs herzustellen . Dabei können zusätzlich dem Fachmann bekannte Additive wie Dispergatoren, Oberflächenaktive Substanzen, oder Tenside alsZugaben zur Herstellung des Schlickers eingesetzt werden.
Durch den hohen Pulveranteil entsteht ein hochviskoser Schli- cker, der gut zum Prepreg verarbeitbar ist. Durch die Polyole und das Glycerin hat das Prepreg eine gute Klebrigkeit, die die Herstellung des Laminats begünstigt, wobei gleichzeitig der Gehalt an Glycerin eben nicht mehr so hoch ist, dass sich die Trocknung und/oder die Sinterung unnötig in die Länge zieht .
Das entstandene Laminat lässt sich leicht durch Trocknen zum Grünkörper verarbeiten.
Durch die Erfindung wird erstmals ein Glycerin-haltiger
Schlicker zur Herstellung einer CMC-Komponente zur Verfügung gestellt, dessen Gehalt an mineralischem und/oder keramischem Pulver 40 Vol% oder mehr, bezogen auf das gesamte Volumen des Schlickers, beträgt und/oder dessen Gehalt an Glycerin unter 10 Gew% - bezogen auf das Gesamtgewicht des keramischen Pul¬ vers im Schlicker - liegt.

Claims

Patentansprüche
1. Schlicker, also ein Mineral-Wasser-Gemisch, folgende Komponenten umfassend:
40 Vol% oder mehr, bezogen auf das gesamte Volumen des Schlickers, an mineralischem und/oder keramischem Pulver;
4 Gew% bis 8 Gew%, bezogen auf das Gesamtgewicht des minera- lischen und/oder keramischen Pulvers, an Glycerin;
0 Gew& bis 2 Gew%, bezogen auf das Gesamtgewicht des minera¬ lischen und/oder keramischen Pulvers, an organischem Binder; 0,5 Gew% bis 10 Gew%, bezogen auf das Gesamtgewicht des mine¬ ralischen und/oder keramischen Pulvers, zumindest eines
Polyols,
sowie Wasser.
2. Schlicker nach Anspruch 1, wobei der Anteil an Polyol zwischen 4 Gew% und 6 Gew%, bezogen auf das Gesamtgewicht des mineralischen und/oder keramischen Pulvers, liegt.
3. Schlicker nach einem der Ansprüche 1 oder 2, wobei das Polyol als geradkettiges Polyol vorliegt.
4. Schlicker nach einem der vorhergehenden Ansprüche, wobei das Polyol oder die Mischung der Polyole ausgewählt ist aus den Polyolen der chemischen Formel CH2OH (CHOH) nCH2OH mit n=3 bis 30.
5. Schlicker nach einem der vorhergehenden Ansprüche, wobei der Schlicker 45 Vol% oder mehr, bezogen auf das gesamte Volumen des Schlickers, an mineralischem und/oder keramischem Pulver umfasst.
6. Prepreg, herstellbar aus einem Schlicker nach einem der Ansprüche 1 bis 5 zusammen mit Verstärkungsfasern, die in Form von Faserbündeln, Fasergeweben und/oder Faserverbunden vorliegen .
7. Prepreg nach Anspruch 6, wobei die Verstärkungsfasern zumindest teilweise ausgewählt sind aus der Gruppe folgender Verbindungen AI2O3, insbesondere alpha- AI2O3, S1O2, ZrÜ2, Y2O3 und/oder ZrÜ2 stabilisiert durch Y2O3, Yttrium-Aluminium- Granat, einem Alumosilikat , also beispielsweise Mullit,
Siliziumcarbid, und/oder Kohlenstofffasern und/oder beliebige Mischungen davon.
8. Laminat, herstellbar aus zumindest einem Prepreg gemäß ei- nem der Ansprüche 6 oder 7.
9. Grünkörper, erhältlich durch Trocknen eines Laminats im Trockenschrank oder durch Trocknung, Aushärtung undVerdich- tung nach Anspruch 8.
10. Turbinenkomponente aus CMC-Material, herstellbar aus ei¬ nem Grünkörper nach Anspruch 9.
PCT/EP2018/051692 2017-02-13 2018-01-24 Schlicker, prepreg, sowie daraus aufgebautes laminat daraus hergestellter grünkörper und cmc-turbinenkomponente WO2018145900A1 (de)

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WO2019185246A1 (de) * 2018-03-26 2019-10-03 Siemens Aktiengesellschaft Formteil aus oxidischer faserverbundkeramik, sowie verfahren zur herstellung eines formteils und vorrichtung zur durchführung des verfahrens dazu

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DE102018200853A1 (de) 2018-01-19 2019-07-25 Siemens Aktiengesellschaft Schlicker für keramisches faserverstärktes Matrixmaterial
DE102019116844A1 (de) 2019-06-21 2020-12-24 Schunk Kohlenstofftechnik Gmbh Einrichtung zur Entnahme und Abgabe einer Schmelze sowie Verfahren zum Herstellen der Einrichtung

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US4329271A (en) 1980-12-15 1982-05-11 Gte Products Corporation Flexible ceramic tape and method of making same
EP0661247A1 (de) * 1993-12-20 1995-07-05 General Motors Corporation Vorform und Verfahren zur Herstellung eines verstärkten Verbundwerkstoffs
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EP0661247A1 (de) * 1993-12-20 1995-07-05 General Motors Corporation Vorform und Verfahren zur Herstellung eines verstärkten Verbundwerkstoffs
DE19928918A1 (de) * 1999-06-24 2000-12-28 Bosch Gmbh Robert Keramischer Schlicker und Verfahren zur Herstellung keramischer Grünkörper mit dem Schlicker
US20140200130A1 (en) * 2013-01-14 2014-07-17 Coi Ceramics, Inc. Methods of forming ceramic matrix composite structures, and related systems, apparatuses, and ceramic matrix composite structures
WO2016016388A1 (en) 2014-07-30 2016-02-04 Universität Bayreuth Ceramic matrix composites and processes for their production
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