DE4301396C2 - Process for the production of porous fiber components - Google Patents

Process for the production of porous fiber components

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Publication number
DE4301396C2
DE4301396C2 DE4301396A DE4301396A DE4301396C2 DE 4301396 C2 DE4301396 C2 DE 4301396C2 DE 4301396 A DE4301396 A DE 4301396A DE 4301396 A DE4301396 A DE 4301396A DE 4301396 C2 DE4301396 C2 DE 4301396C2
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Germany
Prior art keywords
fiber
fibers
fixing material
fixing
production
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Expired - Fee Related
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DE4301396A
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German (de)
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DE4301396A1 (en
Inventor
Hartmut Dr Greulich
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Individual
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Individual
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Priority to DE4301396A priority Critical patent/DE4301396C2/en
Publication of DE4301396A1 publication Critical patent/DE4301396A1/en
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Publication of DE4301396C2 publication Critical patent/DE4301396C2/en
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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4209—Inorganic fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2055—Carbonaceous material
    • B01D39/2065—Carbonaceous material the material being fibrous
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2068—Other inorganic materials, e.g. ceramics
    • B01D39/2082—Other inorganic materials, e.g. ceramics the material being filamentary or fibrous
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2068—Other inorganic materials, e.g. ceramics
    • B01D39/2082—Other inorganic materials, e.g. ceramics the material being filamentary or fibrous
    • B01D39/2089—Other inorganic materials, e.g. ceramics the material being filamentary or fibrous otherwise bonded, e.g. by resins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
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    • C04B30/00—Compositions for artificial stone, not containing binders
    • C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • C04B35/589—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained from Si-containing polymer precursors or organosilicon monomers
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83—Carbon fibres in a carbon matrix
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    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4209—Inorganic fibres
    • D04H1/4242—Carbon fibres
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    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4374—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece using different kinds of webs, e.g. by layering webs
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
    • D04H1/60—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives the bonding agent being applied in dry state, e.g. thermo-activatable agents in solid or molten state, and heat being applied subsequently
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
    • B01D2239/065—More than one layer present in the filtering material
    • B01D2239/0668—The layers being joined by heat or melt-bonding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
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    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
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    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
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    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
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    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5252—Fibers having a specific pre-form
    • C04B2235/5256—Two-dimensional, e.g. woven structures
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    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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  • Chemical & Material Sciences (AREA)
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  • Ceramic Engineering (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Composite Materials (AREA)
  • Laminated Bodies (AREA)
  • Woven Fabrics (AREA)

Description

Die Erfindung bezieht sich auf ein Verfahren zur Herstellung von porösen Faserbau­ teilen, bei dem die Fasern mit einem Fixierungsmaterial in Kontakt gebracht werden.The invention relates to a method for producing porous fiber construction share in which the fibers are brought into contact with a fixing material.

Bei der Herstellung von Faserverbundkeramiken beispielsweise, wird ein poröses fasriges Zwischenprodukt hergestellt, das anschließend durch eine Gasphasen- oder Flüssigphaseninfiltration mit einer keramischen Matrix verdichtet wird. Das fas­ rige Zwischenprodukt muß eine hohe Porosität und gleichzeitig eine zur Handha­ bung und weiteren Bearbeitung ausreichende Festigkeit besitzen.For example, in the manufacture of fiber composite ceramics, a porous one fibrous intermediate product, which is then through a gas phase or liquid phase infiltration is compacted with a ceramic matrix. That almost Intermediate product must have a high porosity and at the same time one to hand exercise and further processing have sufficient strength.

Aus der EP 223 022 A2 ist ein Verfahren der eingangs genannten Art bekannt, bei dem eine aus losen Fasern bestehende Matte oder ähnliches Faserwerkstück im CVD-Verfahren oder durch Abscheidung amorpher Produkte aus flüssiger Phase beschichtet wird derart, daß die Fasern sich an ihren Kreuzpunkten miteinander verbinden. Ein derartiges Bauteil hat eine selbsttragende Struktur. Es konnte jedoch festgestellt werden, daß das flüssige Fixierungsmaterial in die Faserbündel ein­ dringt, was für manche Anwendungsfälle nachteilig ist.A method of the type mentioned at the outset is known from EP 223 022 A2 a mat made of loose fibers or a similar fiber workpiece in the CVD process or by separating amorphous products from the liquid phase is coated in such a way that the fibers meet at their cross points connect. Such a component has a self-supporting structure. However, it could be found that the liquid fixing material into the fiber bundle penetrates, which is disadvantageous for some applications.

Ein Verfahren zur Herstellung faserverstärkter Keramik mit Hilfe fester Ausgangssubstanzen (Silazane) ist in DE 41 14 218 A1 beschrieben. Die Substanzen (Keramikpulver, Kurzfasern und Silazanbindemittel) werden gemischt und bei hohen Temperaturen miteinander versintert. Es entsteht ein Bauteil mit geringer Porosität. Es werden in diesem Verfahren Kurzfasern eingesetzt und die Fasern werden direkt mit dem Fixierungsmittel vermischt. Der mit diesem Verfahren erzeugte Werkstoff hat eine kleine Porosität. Das Verfahren ist nicht geeignet zur Erzeugung von hochporösen Fasergelegen zur nachfolgenden Gasphasen- oder Flüssigphaseninfiltration.A method of manufacturing fiber-reinforced ceramics using solid Starting substances (silazanes) are described in DE 41 14 218 A1. The Substances (ceramic powder, short fibers and silazane binders) are mixed and sintered together at high temperatures. A component is created with low porosity. Short fibers are used in this process and the Fibers are mixed directly with the fixative. The one with this procedure generated material has a small porosity. The method is not suitable for Generation of highly porous fiber fabrics for subsequent gas phase or Liquid phase infiltration.

Die Herstellung von Formlingen aus keramischen oder metallischen Fasern ist in DE 39 35 276 A1 beschrieben. Hier werden die Fasern mit dem Bindemittel vermischt und danach die gewünschte Werkstückgeometrie durch Strangpressen oder Spritzgießen erzeugt. Auch hier wurden mit Bindemitteln imprägnierte Kurzfasern eingesetzt. The production of moldings from ceramic or metallic fibers is in DE 39 35 276 A1 described. Here the fibers are mixed with the binder and then the desired workpiece geometry by extrusion or Injection molding creates. Here too, short fibers were impregnated with binders used.  

Die Verwendung von Langfasergelegen zur Herstellung faserverstärkter Keramik wird in DE 36 16 265 C2 beschrieben. Als Matrix wird eine Suspension von Keramikpartikeln in Wasser oder Alkohol, also in flüssiger Form verwendet. Es entsteht nach der Wärmebehandlung eine Glaskeramik hoher Dichte und sehr geringer Porosität.The use of long fiber fabrics for the production of fiber-reinforced ceramics is described in DE 36 16 265 C2. A suspension of Ceramic particles in water or alcohol, i.e. used in liquid form. It after the heat treatment, a glass ceramic of high density and very low porosity.

Eine Methode zur Herstellung poröser Keramikstrukturen wird in DE 35 41 444 A1 beschrieben. Durch Infiltrieren von Polyuretanschäumen mit Keramikschlickern, die auch Kurzfasern enthalten können und anschließendem Herausbrennen des Polyuretanschaums entsteht eine sehr poröse Keramikstruktur. Aber auch hier wird mit Kurzfasern gearbeitet, die zudem vor der Formgebung mit dem Bindemittel in Verbindung gebracht wurden.A method for producing porous ceramic structures is described in DE 35 41 444 A1 described. By infiltrating polyurethane foams with ceramic slurries can also contain short fibers and then burning out the Polyurethane foam creates a very porous ceramic structure. But here too worked with short fibers, which are also in Have been connected.

Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren der eingangs genannten Art zu schaffen, bei dem das Eindringen von Fixierungsmaterial in die Faserbündel vermindert werden kann.The invention has for its object a method of the aforementioned To create a way in which the penetration of fixation material into the fiber bundle can be reduced.

Die Aufgabe ist erfindungsgemäß durch die Merkmale des Anspruches 1 gelöst.The object is achieved by the features of claim 1.

Durch die Konsistenz des Materials als Feststoff wird erreicht, daß das Material nur wenig in die Faserbündel eindringt und nur die Verbindung zwischen den Faserbün­ deln bzw. den Gewebelagen bewerkstelligt. Es ist daher möglich, mit erheblich weniger Fixierungsmaterial (bis zu 1/50tel) vorfixierte Fasergelege zu erzeugen als bei Verwendung flüssigen Fixierungsmaterials. Dieses führt außerdem zu einer er­ höhten Porosität des Faserbauteiles. Dies ist insbesondere bei der Gasphasen- oder Flüssigphaseninfiltration vorteilhaft, indem das Matrixmaterial besser infiltrier­ bar ist. Die erhöhte Porosität läßt die Gase oder die Flüssigkeit, aus der die Kera­ mikmatrix abgeleitet wird, besser in das Innere von Bauteilelementen eindringen, die eine höhere Wanddicke aufweisen. Ein weiterer Vorteil ist, daß es möglich ist, eine höhere Menge an Keramikmatrix in das Fasergelege einzubringen, denn die mechanischen Eigenschaften einer faserverstärkten Keramik werden hauptsächlich durch die Keramikmatrix bestimmt, wogegen das eingebrachte Fixierungsmaterial eher schwächend wirkt.The consistency of the material as a solid means that the material only little penetrates into the fiber bundle and only the connection between the fiber bundle the fabric layers. It is therefore possible with considerable to produce less fixation material (up to 1 / 50th) of pre-fixed fiber fabrics than when using liquid fixation material. This also leads to a he increased porosity of the fiber component. This is particularly the case with gas phase or liquid phase infiltration advantageous in that the matrix material infiltrates better is cash. The increased porosity leaves the gases or the liquid from which the Kera mikmatrix is derived, better penetrate into the interior of component elements, which have a higher wall thickness. Another advantage is that it is possible to bring a higher amount of ceramic matrix into the fiber fabric, because the mechanical properties of a fiber-reinforced ceramic are mainly determined by the ceramic matrix, whereas the introduced fixation material rather debilitating.

Poröse Bauteile dieser Art eignen sich für diverse Anwendungszwecke, wie z. B. für die Herstellung von Partikelfiltern, oder als Grundbauteil zur Herstellung von faserverstärkter Keramik oder Metallen. Porous components of this type are suitable for various applications, such as. B. for the production of particle filters, or as a basic component for the production of fiber reinforced ceramics or metals.  

Es sind zwar Verfahren bekannt (DE 32 46 755 A1, DE 39 33 039 A1, DE 38 38 153 A1), in denen langfaserverstärkte Werkstücke hergestellt werden, jedoch unter Verwendung von Prepregs (harzgetränkte Gewebelagen oder unidirektional gelegte Fasern). In DE 38 38 153 A1 wird zusätzlich ein Verfahren beschrieben, diese Prepregs auch mit thermoplastischer Matrix herzustellen. Keine der genannten Anmeldungen beschreibt jedoch den Aufbau einer Faserstruktur aus mehreren Lagen nicht vorimprägnierten Endlosfasermaterials (UD oder Gewebe). In DE 32 46 755 A1 wird zusätzlich ein Verfahren genannt, in dem Wabenschichten mit Endlosfasergelegen durch Verschmelzen mit Thermoplastfolien verbunden werden. Auch hier werden vorimprägnierte Endlosfasergelege (Prepregs) verwendet und die Wabenschichten enthalten nur Kurzfasern (Papier). Ein solches Verfahren ist sehr gut dazu geeignet, leichte und dennoch feste Strukturbauteile zu fertigen, nicht aber zur Herstellung einer faserverstärkten Keramik durch nachträgliche Infiltration eines langfaserverstärkten Vorkörpers.Methods are known (DE 32 46 755 A1, DE 39 33 039 A1, DE 38 38 153 A1), in which long fiber reinforced workpieces are produced, but under Use of prepregs (resin-impregnated fabric layers or unidirectional ones) Fibers). DE 38 38 153 A1 also describes a method, this Prepregs can also be produced with a thermoplastic matrix. None of the above However, applications describe the construction of a fiber structure from several Layers of non-pre-impregnated continuous fiber material (UD or fabric). In DE 32 46 755 A1 a method is additionally mentioned in which honeycomb layers with Continuous fiber laid together by fusing with thermoplastic films. Pre-impregnated continuous fiber fabrics (prepregs) are also used here and the Honeycomb layers only contain short fibers (paper). Such a procedure is very well suited for producing light yet strong structural components, but not for the production of a fiber-reinforced ceramic by subsequent infiltration of a long fiber reinforced body.

Für temperaturbeständige Materialien wie eine Faserverbundkeramik eignen sich insbesondere organische Verbindungen, wie z. B. Siliziumverbindungen für die Fixierung der Fasern. Nach dem Aufstreuen auf die Fasergelege haben die Kleber­ partikel noch keine oder nur eine geringe Haftung auf den Fasern. Dies kann da­ durch erreicht werden, daß die Fasern mit einem Lösungsmittel behandelt werden, die den festen Kleber anlösen und dadurch eine Haftung zustande bringen oder daß die Fasern allein oder zusammen mit dem Kleber einer Temperaturbehandlung unterzogen werden, die den Kleber anschmelzen läßt. Dadurch wird eine intensive Verbindung zwischen den Faserlagen und dem Kleber geschaffen, ohne daß der Kleber vollständig in die Faserbündel eindringt. Er wirkt nur als Verbindungsglied zwischen den einzelnen Faserlagen.Suitable for temperature-resistant materials such as fiber composite ceramics especially organic compounds, such as. B. silicon compounds for the Fixation of the fibers. After sprinkling on the fiber fabric, the glue has particles have no or only slight adhesion to the fibers. This can happen by treating the fibers with a solvent, which loosen the solid adhesive and thereby bring about a liability or that the fibers alone or together with the adhesive of a heat treatment be subjected to melting of the adhesive. This will make an intense Connection between the fiber layers and the adhesive created without the Glue penetrates completely into the fiber bundle. It only acts as a link between the individual fiber layers.

Die in die Fasergelege eingebrachten organischen Verbindungen werden schließlich bei 100° bis 300°C unter Verwendung von Stützformen einer Temperaturbehandlung unterzogen. Dies kann eine Härtung von organischen bzw. siliziumorganischen Harzen sein oder auch ein kurzes Anschmelzen von thermoplastischen Matrixparti­ keln. Gleichzeitig kann durch die Anwendung von Formen das Fasergelege noch etwas verdichtet werden, so daß auch ein für die weiteren Prozeßschritte optimaler Faservolumengehalt eingestellt werden kann. Damit sind die Fasergelege vorfixiert und können als Ganzes für weitere Behandlungen gehandhabt werden.The organic compounds introduced into the fiber fabric eventually become at 100 ° to 300 ° C using support forms of a temperature treatment subjected. This can harden organic or organosilicon Resin or a short melting of thermoplastic matrix parts keln. At the same time, the fiber structure can still be used by using shapes somewhat compacted so that it is also optimal for the further process steps Fiber volume content can be adjusted. The fiber fabrics are pre-fixed and can be used as a whole for further treatments.

Vor einer Gasphasen- oder Flüssigphaseninfiltration von Matrixmaterial wird das Fixierungsmaterial vorzugsweise noch einer Pyrolyse unterzogen. Dieser Prozeß­ schritt wird vorgenommen, damit Pyrolyseprodukte das eigentliche Einbringen der keramischen Matrix nicht stören. Dabei werden die organischen Substanzen in Kohlenstoff und siliziumorganische Verbindung in eine Keramiksubstanz mit einem hohen Silizium-Anteil überführt.Before a gas phase or liquid phase infiltration of matrix material Fixing material preferably subjected to pyrolysis. This process step is carried out so that pyrolysis products actually introduce the  ceramic matrix. The organic substances in Carbon and organosilicon compound in a ceramic substance with a transferred high silicon content.

Die festen Fixierungsmaterialien können sowohl in der Form einer Folie, wie in der Form von Pulver auf die Fasergewebe aufgetragen werden.The solid fixing materials can be in the form of a film as well as in the Form of powder to be applied to the fiber tissue.

Die Erfindung wird an Hand von in der Zeichnung dargestellten Ausführungsbei­ spielen näher beschrieben.The invention is illustrated by the embodiment shown in the drawing play described in more detail.

In Fig. 1 wird ein erstes Fasergelege 10 aus C, SiC, Al₂O₃ oder andern Fasern ge­ zeigt, auf das ein pulveriges Fixierungsmaterial 11, beispielsweise ein Polyamid, ein Polysilazan oder ein bereits mit Härter vermischtes Epoxid, aufgestreut wird. Darauf wird ein zweites Fasergelege 12 gelegt und ebenfalls mit dem Fixierungspul­ ver 11 bestreut und mit einem dritten Fasergelege, das nicht gezeigt ist, abgedeckt. Die Zahl der übereinandergeschichteten Fasergelege richtet sich nach der ge­ wünschten Bauteildicke.In Fig. 1, a first fiber fabric 10 made of C, SiC, Al₂O₃ or other fibers is shown, on which a powdery fixing material 11 , for example a polyamide, a polysilazane or an epoxy already mixed with hardener, is sprinkled. Then a second fiber fabric 12 is placed and also sprinkled with the fixing powder 11 and covered with a third fiber fabric, which is not shown. The number of layered fiber fabrics depends on the desired component thickness.

Anstelle von pulverigem Fixierungsmaterial 11 kann gemäß Fig. 2 in Folien 13 ver­ arbeitetes Fixierungsmaterial verwendet werden, das ebenfalls zwischen Fasergele­ gen 14, 15, 16 usw. gelegt wird.Instead of powdery fixing material 11 can be used according to FIG. 2 in foils 13 processed fixation material, which is also placed between fiber gels 14 , 15 , 16 , etc.

Diese Faserpackungen 10, 12 bzw. 13 bis 15 werden dann in einem Ofen tempera­ turbehandelt, wobei sich die Behandlungstemperatur nach dem jeweilig verwendeten Fixierungsmaterial 11 bzw. 13 richtet. Wird thermoplastisches Material wie z. B. Polyethylen verwendet, wird das Fasergelege bei ca. 130°C temperaturbehandelt, ein kalthärtendes Epoxidharz benötigt eine Temperatur von ca. 50°C, ein Phenol­ harz bis zu 200°C. Üblich ist eine Aufheizrate von 5°C/Minute und eine Haltezeit von 1 Stunde bei der Maximaltemperatur. Nach dieser Temperaturbehandlung sind die Fasergelege selbsttragend.These fiber packs 10 , 12 or 13 to 15 are then temperature-treated in an oven, the treatment temperature depending on the fixing material 11 or 13 used in each case. Is thermoplastic material such. B. polyethylene is used, the fiber fabric is heat treated at about 130 ° C, a cold-curing epoxy resin needs a temperature of about 50 ° C, a phenolic resin up to 200 ° C. A heating rate of 5 ° C / minute and a holding time of 1 hour at the maximum temperature are common. After this temperature treatment, the fiber fabrics are self-supporting.

Vor der Einbringung der keramischen oder metallischen Matrix wird das fixierte Fasergelege unter Schutzgas (z. B. N₂ oder Argon) auf eine Temperatur gebracht, die oberhalb der Zersetzungstemperatur des eingebrachten Fixierungsmittels ist. Am besten bewähren sich dabei Temperaturen oberhalb 600°C. Ein gebräuchliches Temperaturprogramm ist eine Aufheizrate von 1°C/Minute auf die Maximaltempera­ tur und eine Haltezeit von 2 Stunden bei dieser Temperatur. Es können aber auch Haltezeiten und langsame Aufheizraten in Temperaturbereichen, in denen das Fixie­ rungsmaterial sich chemisch sehr stark verändert, vorteilhaft sein. This is fixed before the ceramic or metallic matrix is introduced Fiber fabric is brought to a temperature under protective gas (e.g. N₂ or argon), which is above the decomposition temperature of the introduced fixative. Temperatures above 600 ° C work best. A common one The temperature program is a heating rate of 1 ° C / minute to the maximum temperature tur and a holding time of 2 hours at this temperature. But it can also Holding times and slow heating rates in temperature ranges in which the fixie material changes chemically very much, be advantageous.  

Diese zweite Temperaturbehandlung führt zu einer chemischen Umwandlung der Fixierungsmatrix in eine temperaturbeständige Substanz. Ist die Ausgangssubstanz z. B. ein organisches Harz, so wird dieses in Kohlenstoff überführt. Diese zweite Temperaturbehandlung kann auch durchgeführt werden, während das Fasergelege auf die zur Infiltration der keramischen Matrix aufgeheizt wird, die entstehenden Pyrolysegase können dabei aber die Infiltrationsapparaturen verunreinigen, so daß zu Erzielung optimaler Materialeigenschaften der faserverstärkten Keramik ein separater Schritt vorzuziehen ist.This second temperature treatment leads to a chemical transformation of the Fixation matrix in a temperature-resistant substance. Is the starting substance e.g. B. an organic resin, this is converted into carbon. This second Temperature treatment can also be done during the scrim to which the ceramic matrix is heated for infiltration, the resulting Pyrolysis gases can contaminate the infiltration equipment, so that to achieve optimal material properties of the fiber-reinforced ceramic separate step is preferable.

Nach der Pyrolyse des Fasergeleges als zweiter Temperaturbehandlung kann das fixierte Fasergelege nun weiteren Verfahrensschritten unterzogen werden, welche die Infiltration der eigentlichen Matrix bewirken und so zu dem herzustellenden Bauteil führt.After pyrolysis of the fiber fabric as a second temperature treatment, this can be done fixed fiber fabrics are now subjected to further process steps, which effect the infiltration of the actual matrix and thus to the one to be produced Component leads.

Claims (7)

1. Verfahren zur Herstellung von porösen Faserbauteilen, bei dem die Fasern mit einem bei Raumtemperatur festen Fixierungsmaterial in Kontakt gebracht und anschließend temperaturbehandelt werden, dadurch gekennzeichnet, daß Fasergelege (10) aus Endlosfasern (20) hergestellt und ohne Imprägnierung in mindestens zwei Lagen (10) aufeinandergelegt wurden, wobei auf jeder Lage Fixierungsmaterial (11, 15) in Form von Pulver oder Folie zur Fixierung der Lagen aufgebracht wird.1. A process for the production of porous fiber components, in which the fibers are brought into contact with a fixing material which is solid at room temperature and are subsequently heat-treated, characterized in that fiber fabrics ( 10 ) are made from continuous fibers ( 20 ) and are impregnated in at least two layers ( 10 ) were placed one on top of the other, fixing material ( 11 , 15 ) in the form of powder or film for fixing the layers being applied to each layer. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß für Bauteile aus kera­ mischen- oder C-Fasern (20, 21) als Fixierungsmaterial (11, 13) organische Polymere oder deren Vorstufen, z. B. Siliziumverbindungen, Pulver oder Folien mit den Fasern kontaktiert und anschließend durch Temperaturbehandlung gehärtet werden.2. The method according to claim 1, characterized in that for components made of kera mix or C fibers ( 20 , 21 ) as the fixing material ( 11, 13 ) organic polymers or their precursors, eg. B. silicon compounds, powder or films are contacted with the fibers and then cured by heat treatment. 3. Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet, daß das Fixierungs­ material durch eine Temperaturbehandlung zum Kleben mit den Fasern gebracht wird.3. The method according to claim 1 and 2, characterized in that the fixing material is glued to the fibers by a heat treatment becomes. 4. Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet, daß das Fixierungs­ material durch die Anwendung von Lösungsmitteln zum Kleben mit den Fasern ge­ bracht wird.4. The method according to claim 1 and 2, characterized in that the fixing material by the use of solvents for gluing with the fibers is brought. 5. Verfahren nach Anspruch 1 bis 4, dadurch gekennzeichnet, daß bei der Tempera­ turbehandlung des Fixierungsmaterials Stützformen zum Einsatz gebracht werden.5. The method according to claim 1 to 4, characterized in that in the tempera The treatment of the fixation material supporting molds can be used. 6. Verfahren nach Anspruch 1 bis 4, dadurch gekennzeichnet, daß bei der Tempera­ turbehandlung des Fixierungsmaterials die Fasergelege durch Anlegen eines äußeren Drucks verdichtet werden.6. The method according to claim 1 to 4, characterized in that in the tempera Treatment of the fixation material by laying a fiber external pressure can be compressed. 7. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß das Fixierungsmaterial (11, 13) nach dem Härtevorgang pyrolysiert wird.7. The method according to claim 2, characterized in that the fixing material ( 11 , 13 ) is pyrolyzed after the hardening process.
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US5780126A (en) * 1996-07-17 1998-07-14 Minnesota Mining & Manufacturing Filter material
US5849375A (en) * 1996-07-17 1998-12-15 Minnesota Mining & Manufacturing Company Candle filter

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DE3246755A1 (en) * 1982-12-17 1984-06-20 Richard 4937 Lage Pott METHOD FOR PRODUCING A MOLDED BODY FROM COMPOSITE MATERIAL AND MOLDED BODY PRODUCED BY THIS METHOD
DE3623786A1 (en) * 1985-11-13 1987-05-14 Man Technologie Gmbh METHOD FOR PRODUCING SOOT FILTERS
DE3541444A1 (en) * 1985-11-23 1987-05-27 Man Technologie Gmbh POROESER, TEMPERATURE-RESISTANT BODY AND METHOD FOR THE PRODUCTION THEREOF
DE3838153A1 (en) * 1988-11-10 1990-05-31 Schuetz Werke Gmbh Co Kg LIGHTWEIGHT MATERIAL AND METHOD AND SYSTEM FOR PRODUCING HONEYCOMB STRUCTURES FROM THE LIGHTWEIGHT MATERIAL
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