EP0489637B1 - Verfahren zur Fabrikation einer faserigen Rohrform gebildet aus feuerfesten Fasern zur Herstellung eines Verbundwerkstoffes - Google Patents

Verfahren zur Fabrikation einer faserigen Rohrform gebildet aus feuerfesten Fasern zur Herstellung eines Verbundwerkstoffes Download PDF

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Publication number
EP0489637B1
EP0489637B1 EP91403260A EP91403260A EP0489637B1 EP 0489637 B1 EP0489637 B1 EP 0489637B1 EP 91403260 A EP91403260 A EP 91403260A EP 91403260 A EP91403260 A EP 91403260A EP 0489637 B1 EP0489637 B1 EP 0489637B1
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EP
European Patent Office
Prior art keywords
yarn
fibers
preform
covering
precursor
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP91403260A
Other languages
English (en)
French (fr)
Other versions
EP0489637A1 (de
Inventor
Pierre Olry
Dominique Coupe
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Societe Europeenne de Propulsion SEP SA
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Societe Europeenne de Propulsion SEP SA
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Filing date
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Application filed by Societe Europeenne de Propulsion SEP SA filed Critical Societe Europeenne de Propulsion SEP SA
Publication of EP0489637A1 publication Critical patent/EP0489637A1/de
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Anticipated expiration legal-status Critical
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Classifications

    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D02G3/16—Yarns or threads made from mineral substances
    • D02G3/18—Yarns or threads made from mineral substances from glass or the like

Definitions

  • the present invention relates to the manufacture of fibrous preforms formed of refractory fibers for the production of parts of composite material according to the preamble of claim 1.
  • the invention also relates to a composite yarn suitable for the manufacture of such preforms according to the preamble of claim 8.
  • refractory fibers is meant here essentially carbon fibers and ceramic fibers.
  • precursors of refractory fibers is meant here fibers in a state preceding the refractory state, the transition to the latter being most often effected by heat treatment.
  • a carbon precursor is the preoxidized polyacrylonitrile (PAN), or a pitch
  • a precursor of the silicon carbon is polycarbosilane (PCS).
  • a particular field of application of the invention is the manufacture of parts made of composite material consisting of a refractory fibrous preform densified by a matrix. Densification consists in the deposition or infiltration of the matrix material in the porosity of the preform, throughout the volume of the latter.
  • a conventional method consists of superimposing strata of a two-dimensional fibrous texture, in particular a fabric, and, optionally, of binding the strata together, for example by needling.
  • Document FR-A-2 608 641 describes the production of a fibrous preform from yarn formed of staple fibers of refractory material using conventional spinning equipment.
  • Document JP-A-2 210 036 discloses a reinforcing thread comprising a plurality of threads, in particular of refractory material, ligated by means of one or more covering threads. These can be of a soluble or easily carbonizable material, or still in a material which, after heat treatment, behaves like a matrix.
  • a difficulty encountered with known refractory fiber yarns consists in their poor ability to undergo textile operations, such as weaving, especially for ceramic fiber yarns, and, above all, needling.
  • One way of overcoming this difficulty consists in carrying out the necessary textile operations on yarns, the constituent fibers of which are in the precursor state, better able to undergo these operations. The transformation of the precursor into refractory material is then carried out after the textile operations have been carried out.
  • Another way of overcoming this difficulty for the needling of superimposed layers of carbon fiber fabric is to interpose layers of felt between the layers.
  • the attack of the threads by the needles has the effect of breaking the fibers more than detaching the fibers to implant them through the strata.
  • the interposition of layers of felt makes it possible to provide the fibers likely to be entrained by the needles.
  • Another problem encountered during the production of parts made of composite material is that of the accessibility of the internal porosity of the preform during densification.
  • the liquid method consists of impregnating the preform with a precursor liquid of the material constituting the matrix and then transforming the precursor, generally by heat treatment.
  • the gas process (chemical vapor infiltration) consists of placing the preform in an enclosure where a gas flow is introduced under determined temperature and pressure conditions to form the matrix material in contact with the fibers of the preform by decomposition of one or more constituents of the gas flow or by reaction between constituents thereof.
  • the object of the present invention is to provide a method for manufacturing a fibrous preform made of refractory fibers, the manufacturing process possibly comprising textile operations, including needling.
  • Another object of the invention is to provide a process allowing the manufacture of fibrous preforms having practically no "dead” volumes, therefore capable of being easily densified.
  • the covering yarn has a low denier compared to that of the assembled staple fibers, so as not to leave too large voids within the preform after elimination of the covering yarn.
  • the denier of the covering yarn is preferably less than a tenth of that of the assembled staple fibers.
  • fugitive material which constitutes the covering yarn, is meant here any material capable of being eliminated without leaving a residue on the yarn and without alteration of the refractory fibers.
  • the fugitive material is a soluble polymer, such as a PVA (polyvinyl alcohol), or a polymer capable of being completely removed by heat treatment, such as polyvinyl acetate or polyethylene.
  • the supply of the wire comprises a step of obtaining staple fibers, preferably long staple fibers, parallel to each other, in refractory material or in a precursor thereof. This is achieved for example by controlled stretching and cracking of a multifilament cable, as described in particular in document FR-A-2 608 641.
  • the fibers are left parallel to each other, and not twisted, the integrity of the thread being made up by covering with the thread of fugitive material.
  • the covering is carried out by means of a known covering machine, for example the "Parafil” machine from the German company Spindelfabrik Suessen.
  • the covering gives the yarn the necessary resistance to undergo textile operations, in particular weaving.
  • the method according to the present invention can be implemented for all applications requiring the execution of textile operations on the yarn, such as weaving and needling.
  • the method according to the invention provides an additional advantage in that it allows the elimination of dead volumes which are not completely densifiable.
  • the preform has been produced and the covering yarn eliminated, the released fibers tend to occupy the volumes available under the effect of the "swelling" of the yarn. This makes it possible to obtain a preform whose porosity is more easily and more uniformly accessible to the material constituting the matrix. This results in more complete densification and less inhomogeneity of the material.
  • the transformation of the precursor into refractory material is carried out after manufacture of the preform and after elimination of the covering wire.
  • the covering thread is made of a removable material by heat, this elimination can be carried out during a temperature rise carried out with a view to the transformation of the precursor by heat treatment.
  • Example 1 Manufacture of a carbon fiber preform.
  • a two-dimensional texture (2D) is formed by weaving a yarn of non-twisted fibers in PAN (polyacrylonitrile) preoxidized gimped with a yarn of PVA (polyvinyl alcohol).
  • the characteristics of the 2D fabric are as follows: - title of the pre-oxidized PAN wire Nm2 - PVA covering wire 45 dtex - weaving weave satin 8 - number of warp threads 10 / cm - number of threads in the weft 10 / cm - surface mass 1050 g / m2
  • the fabric After weaving, the fabric is washed in a water bath at 80 ° C for 10 minutes, then wrung and dried.
  • the PVA covering yarn is completely dissolved and the fibers of the preoxidized PAN yarns expand within the fabric allowing direct needling thereof, without adding a layer of felt.
  • the carbon fiber preform can then be densified by a material constituting a matrix, for example carbon or a ceramic, in order to obtain the composite material. desired carbon fiber reinforcement. Densification is carried out by liquid means or by chemical vapor infiltration. The proliferation of fibers within the fibrous texture, resulting from the loosening of the untwisted fibers after elimination of the covering yarn, avoids the formation of dead volumes within the preform and consequently promotes a more complete and more homogeneous densification.
  • a material constituting a matrix for example carbon or a ceramic
  • Example 2 Manufacture of a ceramic fiber preform.
  • a texture is formed by multilayer weaving of a thread of non-twisted silicon carbide (SiC) fibers wrapped in a PVA thread.
  • the characteristics of the fabric are as follows: - title of the SiC thread Nm 3 - PVA covering wire 45 dtex - weaving weave Interlock - number of layers 5 - number of warp threads 40 / cm - number of threads in the weft 30 / cm - fabric thickness 3 mm
  • the texture is soaked in a water bath at 80 ° C for 15 minutes then wrung and dried. It is noted that the PVA yarn is dissolved and that the SiC fibers expand within the texture.
  • the volume content of fibers in the woven texture as indicated above is approximately 30%.
  • the texture obtained is particularly suitable for subsequent densification by the liquid or gaseous route.
  • a carbon fiber preform can be made directly from carbon fibers, including high strength fibers.

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Woven Fabrics (AREA)
  • Nonwoven Fabrics (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Inorganic Fibers (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Claims (11)

  1. Verfahren zur Herstellung eines faserigen Vorformlings zur Bildung eines Verbundwerkstoffteiles, bestehend aus den folgenden Stufen:
    - es wird ein im wesentlichen aus diskontinuierlichen Fasern aus einem hitzebeständigen Material oder einem Zwischenprodukt davon bestehender Faden zugeführt, und
    - es wird ein faseriger Vorformling aus dem im wesentlichen aus diskontinuierlichen Fasern bestehenden Fasern gebildet,
    dadurch gekennzeichnet, daß
       der Faden aus im wesentlichen diskontinuierlichen Fasern zusammengesetzt wird, die parallel zueinander und im ungezwirnten Zustand angeordnet werden, und die Integrität des Fadens durch einen Umspinnungsfaden aus einem unbeständigen Material sichergestellt wird, und
       nach der Bildung des faserigen Vorformlings der Umspinnungsfaden entfernt wird, damit sich die diskontinuierlichen Fasern im gesamten Volumen des Vorformlings freisetzen können.
  2. Verfahren nach Anspruch 1,
    dadurch gekennzeichnet, daß
    der Umspinnungsfaden ein Denier weniger als ein Zehntel desjenigen der zusammengestzten diskontinuierlichen Fasern hat.
  3. Verfahren nach Anspruch 1 oder 2,
    dadurch gekennzeichnet, daß
    die diskontinuierlichen Fasern durch gesteuertes Strecken und Reißen erhalten werden.
  4. Verfahren nach einem der Ansprüche 1 - 3,
    dadurch gekennzeichnet, daß
    der Umspinnungsfaden aus einem lösbaren Polymer besteht.
  5. Verfahren nach einem der Ansprüche 1 - 4,
    dadurch gekennzeichnet, daß
    der Umspinnungsfaden aus einem durch Wärme entfernbaren Material besteht.
  6. Verfahren nach einem der Ansprüche 1 - 5,
    dadurch gekennzeichnet, daß
    der Faden im wesentlichen aus diskontinuierlichen Fasern aus einem Zwischenprodukt aus einem Keramikmaterial zusammengesetzt wird, und daß die Umwandlung des Zwischenproduktes aus keramischem Material nach dem Entfernen des Umspinnungsfadens durchgefüht wird.
  7. Verfahren nach einem der Ansprüche 1 - 6,
    gekennzeichnet durch
    eine Nadelungsstufe, die am faserigen Vorformling nach Entfernen des Umspinnungsfadens durchgeführt wird.
  8. Zusammengesetzter Faden, der im wesentlichen aus Fasern aus einem hitzebeständigen Material oder aus einem Zwischenprodukt hiervon und einem Umspinnungsfaden aus einem flüchtigen Material zusammengesetzt ist,
    dadurch gekennzeichnet, daß
    die Fasern diskontinuierlich und parallel zueinander sowie im ungezwirnten Zustand angeordnet sind, und daß der Umspinnungsfaden, der die Integrität des zusammengesetzten Fadens bewirkt, ein Denier niedriger als ein Zehntel desjenigen der zusammengesetzten diskontinuierlichen Fasern hat.
  9. Zusammengesetzter Faden nach Anspruch 8,
    dadurch gekennzeichnet, daß
    das hitzebeständige Material aus Kohlenstoff und Keramikmaterialien ausgewählt ist.
  10. Zusammengesetzter Faden nach Anspruch 8 oder 9,
    dadurch gekennzeichnet, daß
    das unbeständige Material ein lösliches Polymer ist.
  11. Zusammengesetzter Faden nach Anspruch 8 oder 9,
    dadurch gekennzeichnet, daß
    das unbeständige Material ein durch Wärme entfernbares Material ist.
EP91403260A 1990-12-03 1991-12-02 Verfahren zur Fabrikation einer faserigen Rohrform gebildet aus feuerfesten Fasern zur Herstellung eines Verbundwerkstoffes Expired - Lifetime EP0489637B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR909015128A FR2669940B1 (fr) 1990-12-03 1990-12-03 Fil forme a partir de fibres refractaires ou de leurs precurseurs et son application a la fabrication de pieces en materiau composite.
FR9015128 1990-12-03

Publications (2)

Publication Number Publication Date
EP0489637A1 EP0489637A1 (de) 1992-06-10
EP0489637B1 true EP0489637B1 (de) 1995-03-29

Family

ID=9402850

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91403260A Expired - Lifetime EP0489637B1 (de) 1990-12-03 1991-12-02 Verfahren zur Fabrikation einer faserigen Rohrform gebildet aus feuerfesten Fasern zur Herstellung eines Verbundwerkstoffes

Country Status (6)

Country Link
US (1) US5228175A (de)
EP (1) EP0489637B1 (de)
JP (1) JP2854178B2 (de)
CA (1) CA2056789C (de)
DE (1) DE69108530T2 (de)
FR (1) FR2669940B1 (de)

Families Citing this family (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE69229007T2 (de) * 1991-01-16 1999-10-21 Sgl Carbon Composites, Inc. Verbundwerkstoffe aus siliciumcarbidfaserarmiertem Kohlenstoff
US6465100B1 (en) * 1993-06-15 2002-10-15 Alliant Techsystems Inc. Densification of composite preforms by liquid resin infiltration assisted by rigid-barrier actinic gelation
JP2755361B2 (ja) * 1993-06-30 1998-05-20 徹 糸井 多重織物の製造方法
FR2734581B1 (fr) * 1995-05-24 1997-08-14 Europ Propulsion Fil hybride pour la fabrication de preformes fibreuses de pieces en materiau composite et procede pour sa preparation
US6248417B1 (en) * 1997-09-08 2001-06-19 Cytec Technology Corp. Needled near netshape carbon preforms having polar woven substrates and methods of producing same
US5952075A (en) * 1997-09-08 1999-09-14 Fiberite, Inc. Needled near netshape carbon preforms having polar woven substrates and methods of producing same
FR2770233B1 (fr) * 1997-10-27 2000-01-14 Messier Bugatti Procede de fabrication de preformes en fibres de carbone
DE10061028A1 (de) * 2000-12-08 2002-06-20 Eads Deutschland Gmbh Verfahren zum Herstellen von mehrschichtigen TFP-Preforms mittels schmelzbaren Fixierfäden
US6820406B2 (en) 2001-05-14 2004-11-23 Cargill, Incorporated Hybrid yarns which include plant bast fiber and thermoplastic fiber, reinforcement fabrics made with such yarns and thermoformable composites made with such yarns and reinforcement fabrics
US20030157323A1 (en) * 2001-05-14 2003-08-21 Mikhail Khavkine Hybrid yarns which include oil seed flax plant bast fiber and other fibers and fabrics made with such yarns
US6833399B2 (en) 2001-09-21 2004-12-21 Cargill, Limited Flowable flax bast fiber and flax shive blend useful as reinforcing agent
WO2005090664A1 (ja) * 2004-03-22 2005-09-29 Otas Company, Limited 等方性ピッチ系炭素繊維紡績糸、それを用いた複合糸及び織物、並びにそれらの製造方法
FR2902802B1 (fr) * 2006-06-21 2008-12-12 Snecma Propulsion Solide Sa Structure fibreuse de renfort pour piece en materiau composite et piece la comportant
PL2532775T3 (pl) * 2011-06-07 2013-12-31 Climatex Ag Podłoże tekstylne z wielu w różny sposób możliwych do utylizacji i/lub możliwych do wykorzystania materiałów, zastosowanie takiego podłoża tekstylnego i sposób przetwarzania takiego podłoża tekstylnego
US10648106B2 (en) 2012-03-05 2020-05-12 Goodrich Corporation Systems and methods for reduced crimp carbon fiber helical fabric
ITUB20152386A1 (it) 2015-07-22 2017-01-22 Freni Brembo Spa Materiale sagomato e procedimento di fabbricazione
JP6652000B2 (ja) * 2016-06-29 2020-02-19 株式会社豊田自動織機 繊維強化複合材用プリフォーム及び繊維強化複合材
JP6620771B2 (ja) * 2017-02-08 2019-12-18 株式会社豊田自動織機 繊維構造体及び繊維強化複合材
FR3162761A1 (fr) * 2024-06-03 2025-12-05 Safran Ceramics Préforme fIbreuse figée par le materieu de guipage

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3994762A (en) * 1972-07-21 1976-11-30 Hyfil Limited Carbon fiber composites
GB2021660B (en) * 1978-04-26 1982-09-22 Tba Industrial Products Ltd Cored staple-fibre yarns
JPS5898443A (ja) * 1981-12-02 1983-06-11 新興機械株式会社 ステ−プル状炭素繊維よりなる糸
US4482601A (en) * 1983-05-31 1984-11-13 Albany International Corp. Wet press papermakers felt and method of fabrication
FR2608641B1 (fr) * 1986-12-18 1990-02-23 Schappe Sa File de fibres de carbone
US4885973A (en) * 1988-12-14 1989-12-12 Airfoil Textron Inc. Method of making composite articles
JPH02210036A (ja) * 1989-02-09 1990-08-21 Gunze Ltd 強化材用複合糸条
JPH07316144A (ja) * 1994-03-29 1995-12-05 Sankyo Co Ltd ジフェニルメチルピペラジン誘導体

Also Published As

Publication number Publication date
JPH0586534A (ja) 1993-04-06
CA2056789C (en) 1999-01-05
FR2669940A1 (fr) 1992-06-05
JP2854178B2 (ja) 1999-02-03
DE69108530T2 (de) 1995-12-21
US5228175A (en) 1993-07-20
EP0489637A1 (de) 1992-06-10
CA2056789A1 (en) 1992-06-04
FR2669940B1 (fr) 1994-10-21
DE69108530D1 (de) 1995-05-04

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