WO1991016277A1 - Method for fiber-reinforced ceramic honeycomb - Google Patents

Method for fiber-reinforced ceramic honeycomb Download PDF

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Publication number
WO1991016277A1
WO1991016277A1 PCT/US1991/002631 US9102631W WO9116277A1 WO 1991016277 A1 WO1991016277 A1 WO 1991016277A1 US 9102631 W US9102631 W US 9102631W WO 9116277 A1 WO9116277 A1 WO 9116277A1
Authority
WO
WIPO (PCT)
Prior art keywords
ceramic
accordance
sheets
liquid
impregnant
Prior art date
Application number
PCT/US1991/002631
Other languages
English (en)
French (fr)
Inventor
Jong Hoon Han
Andreas G. Hegedus
Original Assignee
Hexcel Corporation
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Hexcel Corporation filed Critical Hexcel Corporation
Priority to DE1991908858 priority Critical patent/DE478765T1/de
Publication of WO1991016277A1 publication Critical patent/WO1991016277A1/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0006—Honeycomb structures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24149—Honeycomb-like

Definitions

  • This invention lies in the fields of ceramic materials, fiber-resin composites and honeycomb structures.
  • Honeycomb has long been known for use in structural elements which require a combination of lightness and strength.
  • the use of ceramics for the honeycomb walls provides the further advantage of high temperature performance.
  • Ceramic honeycomb One existing method of forming ceramic honeycomb is by extrusion of ceramic precursor materials through dies which form the cellular array.
  • the structures produced by this method are monolithic (single-phase) structures, which are brittle and thereby limited in the ease and degree with which they can be handled and further processed for use.
  • the extrusion process also limits the size and shape of the piece.
  • Ceramic honeycomb of increased toughness has been formed by the use of a ceramic fiber tape embedded in ceramic material to form the honeycomb walls.
  • the existing procedure to form such a structure involves incorporating a ceramic frit into the fiber tape, then forming the combination into the corrugated shape required for the honeycomb walls, then hot pressing this corrugated form to consolidate the frit into a matrix. This is all done prior to assembling the corrugated strips into the honeycomb structure.
  • the hot press limits the size of the part which can be formed in this manner and adds greatly to the cost.
  • fiber-reinforced ceramic honeycomb may be manufactured by the use of a liquid impregnant which is convertible to a ceramic material upon exposure to elevated temperature.
  • a fabric tape or sheet formed of fibers of high-temperature material is impregnated with the liquid ceramic precursor, which contains either a preceramic polymer dissolved in a liquid vehicle, a colloidal suspension of a preceramic material, or any other suitable liquid form of a precursor.
  • the impregnated tape or sheet is then heated to evaporate the vehicle, the tapes or sheets are formed into the corrugated shape and assembled in the honeycomb configuration, and the assembly is given a final cure to consolidate and solidify the ceramic into a solid continuous phase.
  • the procedure entails essentially no shrinkage and is not subject to the size limitations inherent in procedures of the prior art.
  • Honeycomb panels and parts formed in accordance with this invention are useful in any application which requires high-temperature performance.
  • the continuous ceramic phase formed by the impregnant in accordance with the practice of the present invention may be any ceramic material which can be formed into a continuous solid phase from a liquid precursor form.
  • the choice of ceramic material is not critical and may include any of the wide variety of ceramic materials known in the ceramics art.
  • the main classes of such materials are metal and non-metal oxides, borides, carbides, nitrides, sulfides and suicides.
  • Both naturally occurring and synthetic ceramic materials may be used, the naturally occurring materials including both clay-derived and non-clay-derived materials.
  • minerals and compounds of various kinds which may be used as the ceramic material are as follows: silica, kaolinite, montmorillonite, illite, gibbsite, diaspore, bauxite, hallyosite, dickite, macrite, nontronite, beidellite, hectorite, saponite, bentonite, muscovite, hydro icas, phengite, brammallite, glauco ite, celadonite, olivine, anthophyllite, tremolite, actinolite, chrysolite, forsterite, fayalite, spodumene, lepidolite, amblygonite, petalite, barite, witherite, fluorspar, apatite, baddeleyite, zirkite, zircon, titania,
  • Silicates are silicates, aluminates, titanates, zirconates, aluminosilicates, silicon carbides, and silicon nitrides.
  • silicates, aluminosilicates and silicon carbides are more preferred.
  • Silicon-containing materials in general are particularly preferred, either as silicates or silicon carbides, either alone or in combination with aluminum-containing materials such as aluminum oxides.
  • the fabric is impregnated with the continuous ceramic phase by applying the ceramic material to the fabric in liquid form.
  • the liquid may be a solution, suspension or colloidal suspension (for example, sol gels) of the ceramic material, or of a precursor to the ceramic material, in either case one which converts to the desired form upon heating.
  • the heating may involve a fusing of the material, a pyrolysis of the material, or any other physical or chemical change which results in a continuous solid ceramic phase.
  • the precursor may be a polymeric precursor or any other form which undergoes conversion to the ceramic by chemical reaction at elevated temperature.
  • polysilanes including polycarbosilanes, polysiloxanes, and poly( etallosiloxanes) .
  • the liquid vehicle for the solution or suspension may be any conventional solvent or suspending liquid. Common examples are water and organic solvents such as hexane and xylene. Examples of commercially available materials suitable for use in forming the continuous ceramic phase are as follows:
  • Sol gel precursors Nalco 1050, a colloidal suspension of Si0 2 particles, approximately 3nm in size, in water, available from Nalco
  • T, TB and TZ silicon carbide precursors available from Ethyl Corporation, Baton Rouge, Louisiana; Pyrofine
  • Fillers or other additives may optionally be included with the ceramic materials for purposes of controlling certain parameters to desired levels. These parameters include those of relevance to the impregnation procedure, the honeycomb forming procedure, or the characteristics of the final product, or combinations of these. Such parameters include viscosity, pH, color and density.
  • the fillers may be other ceramic materials, usually in the form of powders or whiskers, clays, or any other additives known among those skilled in the art for similar purposes.
  • One example of a filler, used with a Si0 2 gel sol ceramic precursor, is pure mullite at a level of 10% by volume.
  • the fibers forming the fabric may be any fiber material which is capable of withstanding and remaining stable at high temperatures, notably those on the order of approximately 1000*C (1832*F).
  • the actual material is not critical and may include any of the wide variety of materials meeting this description.
  • Such materials include certain nonmetallic elements as well as the metal and non- metal oxides, borides, carbides, nitrides, sulfides and suicides mentioned above in connection with the continuous ceramic phase.
  • further examples are asbestos, graphite and other forms of carbon, boron, Fiberglas, and coated materials such as silicon carbide- coated boron, boron carbide-coated silicon, and silicon- coated silicon carbide.
  • Preferred fiber materials are ceramic materials, particularly silicates, aluminates, titanates, zirconates, aluminosilicates, silicon carbides, and silicon nitrides, as mentioned above in connection with the continuous ceramic phase.
  • the fibers may be in the form of either woven or non-woven cloth.
  • the cloth may vary widely in terms of surface finish, weight and, if woven, the type of weave. These parameters are not critical and may be selected in accordance with the desired properties of the final product, which may depend on the scale and physical dimensions of the product and its intended use, as well as the procedures selected for use in processing these materials into the final honeycomb shape.
  • Fibers which are commercially available and may be used in the practice of the invention are Astroquartz, a quartz fiber available from J.P. Stevens & Co., Inc., New York, New York; Nextel 312, Nextel 440 and Nextel 480, mullite-based fibers available from 3M Co., St. Paul, Minnesota; aluminum oxide-based fibers from E.I. du Pont de Nemours & Co. , Inc., Wilmington, Delaware, and
  • the continuous ceramic phase is applied to the fabric in liquid form, as either a solution or a suspension.
  • Various methods of application may be used, such as for example, dipping, sponging, or spraying. Dipping the fabric in a vessel containing the liquid impregnant is particularly convenient, and the impregnant may be applied to the fabric in single or multiple dips. Multiple dips are a convenient way of controlling or adjusting density and may include liquid phases varying in the solids loading.
  • Successive dips may be performed with intervening heat treatments to remove the liquid vehicle.
  • a mild heat treatment typically on the order of 40- 50 ⁇ C or 104-122*F
  • a higher temperature typically on the order of 1000*C or 1832*F
  • Additional dips may also be performed on the honeycomb structure itself, once the corrugated sheets have been bonded together.
  • a first dip using a solution of approximately 50% solids content and a viscosity of slightly under 100 centipoise was used, followed by a second dip using a 30-40% solids content and a viscosity of slightly under 50 centipoise.
  • the impregnated sheets were fired in nitrogen at 1000°C for one hour in between dips. Multiple dips may also be used where fillers are present in the first dip only.
  • Formation of the honeycomb structure is achieved by conventional means, analogous to methods known for use in manufacturing honeycomb panels of more conventional materials.
  • the ceramic-impregnated fabric sheets or strips are shaped into a corrugated form by conventional shaping equipment.
  • the corrugated sheets are then assembled to form a honeycomb structure by joining adjacent sheets at node lines along their concave surfaces, using a ceramic adhesive material or a solvent capable of dissolving the ceramic material forming the continuous phase to form the bond.
  • Ceramic adhesives are products bearing the name Aremco-Seal, available from Aremco Products, Inc., Ossining, New York.
  • Non-sacrificial adhesives may also be used, particularly those that convert to a ceramic upon pyrolysis after curing.
  • the sheets may be bonded together by simply contacting them when the impregnant is still wet, and curing them together, thereby fusing them at the lines of contact.
  • face sheets may be added, again in accordance with known methods previously used for honeycomb panels of other materials.
  • the same fabric used for the individual sheets of the honeycomb may be used as the face sheets, these sheets being optionally impregnated with the continuous ceramic material as in the honeycomb itself.
  • Conventional ceramic adhesives may again be used to bond the sheets to the honeycomb.
  • the temperatures used in the various heating steps may vary, depending on the particular step in the sequence, and the type and amount of ceramic material or precursor used. Final curing temperatures in most cases generally range from about 400*C to about lOOO'C (752-1832'F) , preferably from about 500*C to about 750*C (534-1382'F) .
  • the atmosphere in which the heating is performed will be selected on the basis of the materials involved. Inert atmospheres such as nitrogen will be appropriate for certain materials, while air will be sufficient for others.
  • the fabric strips are dipped in a bath of the slurry and excess slurry is then wiped off the strips.
  • These impregnated strips i. e. , the "prepreg" are corrugated in accordance with the desired dimensions of a honeycomb structure, and cured at 100*C to retain the corrugated shape.
  • a high temperature ceramic-based adhesive such as for example Aremco 503 with mullite filler or Hexcel preceramic adhesive/binder with mullite filler, is applied to the nodes of the corrugations where the strips will be joined to form the honeycomb, and the sheets are stacked in the honeycomb arrangement.
  • the adhesive is then cured at 100-300 ⁇ C, followed by pyrolysis are 1100*C.
  • the resulting honeycomb is then dipped again in the same slurry used initially, and pyrolysis is once again performed at 1100- 1400°C.
  • Skins i . e. , face sheets
  • Skins for placement over the honeycomb core are prepared from the same fabric and dipping slurry, and attached to the honeycomb with the same high temperature ceramic-based adhesive.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Laminated Bodies (AREA)
  • Catalysts (AREA)
  • Porous Artificial Stone Or Porous Ceramic Products (AREA)
PCT/US1991/002631 1990-04-18 1991-04-17 Method for fiber-reinforced ceramic honeycomb WO1991016277A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE1991908858 DE478765T1 (de) 1990-04-18 1991-04-17 Herstellung von faserverstaerkter keramik mit bienenwaben-struktur.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US07/510,510 US5078818A (en) 1990-04-18 1990-04-18 Method for producing a fiber-reinforced ceramic honeycomb panel
US510,510 1990-04-18

Publications (1)

Publication Number Publication Date
WO1991016277A1 true WO1991016277A1 (en) 1991-10-31

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Country Status (6)

Country Link
US (1) US5078818A (en, 2012)
EP (1) EP0478765A4 (en, 2012)
JP (1) JPH04503798A (en, 2012)
ES (1) ES2034936T1 (en, 2012)
GR (1) GR920300107T1 (en, 2012)
WO (1) WO1991016277A1 (en, 2012)

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EP0573353A1 (fr) * 1992-06-04 1993-12-08 Societe Europeenne De Propulsion Structure en nid d'abeilles en matériau composite thermostructural et son procédé de fabrication
WO1996016000A1 (en) * 1994-11-18 1996-05-30 Du Pont Lanxide Composites Inc. High temperature, thermal shock resistant ceramic structures
EP2769968A1 (en) * 2013-02-22 2014-08-27 Korea Institute of Energy Research Fiber-reinforced ceramic composite material honeycomb and method for preparing the same
EP3044276A4 (en) * 2013-09-12 2016-09-07 United Technologies Corp PREKERAMIC LIQUID COMPOSITION
RU2647024C2 (ru) * 2013-01-29 2018-03-13 Эракль Способ производства изогнутой сотовидной структуры из композиционного материала
US9925680B2 (en) 2013-06-11 2018-03-27 Bell Helicopter Textron Inc. System and method of post-cure processing of composite core
CN110183239A (zh) * 2019-04-22 2019-08-30 湖南远辉复合材料有限公司 一种陶瓷基复合材料点阵结构的组合式制备方法

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CN1308262C (zh) * 2003-01-08 2007-04-04 3M创新有限公司 陶瓷纤维复合材料及其制备方法
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US20070152364A1 (en) * 2005-11-16 2007-07-05 Bilal Zuberi Process for extruding a porous substrate
US20100048374A1 (en) * 2005-11-16 2010-02-25 James Jenq Liu System and Method for Fabricating Ceramic Substrates
US7938876B2 (en) * 2005-11-16 2011-05-10 GE02 Technologies, Inc. Low coefficient of thermal expansion materials including nonstoichiometric cordierite fibers and methods of manufacture
US7938877B2 (en) * 2005-11-16 2011-05-10 Geo2 Technologies, Inc. Low coefficient of thermal expansion materials including modified aluminosilicate fibers and methods of manufacture
US20090166910A1 (en) * 2005-11-16 2009-07-02 Geo2 Technologies, Inc. System and Method for Twin Screw Extrusion of a Fibrous Porous Substrate
US8038759B2 (en) * 2005-11-16 2011-10-18 Geoz Technologies, Inc. Fibrous cordierite materials
US7640732B2 (en) * 2005-11-16 2010-01-05 Geo2 Technologies, Inc. Method and apparatus for filtration of a two-stroke engine exhaust
US8039050B2 (en) * 2005-12-21 2011-10-18 Geo2 Technologies, Inc. Method and apparatus for strengthening a porous substrate
US7781372B2 (en) * 2007-07-31 2010-08-24 GE02 Technologies, Inc. Fiber-based ceramic substrate and method of fabricating the same
EP2250139B1 (en) * 2007-12-17 2016-10-26 Imerys Ceramic honeycomb structures
CN108794046B (zh) * 2018-07-11 2021-02-09 航天材料及工艺研究所 一种氧化铝陶瓷基复合材料蜂窝及其制备方法

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0573353A1 (fr) * 1992-06-04 1993-12-08 Societe Europeenne De Propulsion Structure en nid d'abeilles en matériau composite thermostructural et son procédé de fabrication
FR2691923A1 (fr) * 1992-06-04 1993-12-10 Europ Propulsion Structure en nid d'abeilles en matériau composite thermostructural et son procédé de fabrication.
US5415715A (en) * 1992-06-04 1995-05-16 Societe Europeenne De Propulsion Method of manufacturing a honey comb structure of thermostructural composite material
US5514445A (en) * 1992-06-04 1996-05-07 Societe Europeenne De Propulsion Honeycomb structure of thermostructural composite material
WO1996016000A1 (en) * 1994-11-18 1996-05-30 Du Pont Lanxide Composites Inc. High temperature, thermal shock resistant ceramic structures
RU2647024C2 (ru) * 2013-01-29 2018-03-13 Эракль Способ производства изогнутой сотовидной структуры из композиционного материала
EP2769968A1 (en) * 2013-02-22 2014-08-27 Korea Institute of Energy Research Fiber-reinforced ceramic composite material honeycomb and method for preparing the same
US9925680B2 (en) 2013-06-11 2018-03-27 Bell Helicopter Textron Inc. System and method of post-cure processing of composite core
US10562202B2 (en) 2013-06-11 2020-02-18 Bell Helicopter Textron Inc. System and method of post-cure processing of composite core
US11065775B2 (en) 2013-06-11 2021-07-20 Textron Innovations Inc. System and method of post-cure processing of composite core
EP3044276A4 (en) * 2013-09-12 2016-09-07 United Technologies Corp PREKERAMIC LIQUID COMPOSITION
CN110183239A (zh) * 2019-04-22 2019-08-30 湖南远辉复合材料有限公司 一种陶瓷基复合材料点阵结构的组合式制备方法

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EP0478765A4 (en) 1993-06-23
US5078818A (en) 1992-01-07
GR920300107T1 (en, 2012) 1993-02-17
EP0478765A1 (en) 1992-04-08
ES2034936T1 (es) 1993-04-16
JPH04503798A (ja) 1992-07-09

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