US3700511A - Method of producing tapes of longitudinally aligned carbon fibres - Google Patents

Method of producing tapes of longitudinally aligned carbon fibres Download PDF

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Publication number
US3700511A
US3700511A US59874A US3700511DA US3700511A US 3700511 A US3700511 A US 3700511A US 59874 A US59874 A US 59874A US 3700511D A US3700511D A US 3700511DA US 3700511 A US3700511 A US 3700511A
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United States
Prior art keywords
sheet
furnace
fibres
tapes
fibre
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
US59874A
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English (en)
Inventor
Ian Whitney
Edward Bailey White
Michael Roger Rowland
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UK Secretary of State for Defence
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UK Secretary of State for Defence
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Application filed by UK Secretary of State for Defence filed Critical UK Secretary of State for Defence
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Publication of US3700511A publication Critical patent/US3700511A/en
Anticipated expiration legal-status Critical
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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/32—Apparatus therefor
    • 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
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S264/00—Plastic and nonmetallic article shaping or treating: processes
    • Y10S264/19—Inorganic fiber
    • 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
    • Y10T156/00—Adhesive bonding and miscellaneous chemical manufacture
    • Y10T156/10—Methods of surface bonding and/or assembly therefor
    • 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
    • Y10T156/00—Adhesive bonding and miscellaneous chemical manufacture
    • Y10T156/10—Methods of surface bonding and/or assembly therefor
    • Y10T156/1052—Methods of surface bonding and/or assembly therefor with cutting, punching, tearing or severing
    • Y10T156/1084—Methods of surface bonding and/or assembly therefor with cutting, punching, tearing or severing of continuous or running length bonded web
    • Y10T156/1087—Continuous longitudinal slitting

Definitions

  • This invention relates to a method of producing tapes of longitudinally aligned carbon fibres.
  • the most convenient form for the fibrous material to be wound comprises a tape of longitudinally aligned fibres.
  • carbon fibres have been introduced as fibrous reinforcements, and there has grown a demand for such fibres in tape form.
  • the present invention provides a method of manufacturing such a tape of carbon fibres.
  • a method of producing tapes of longitudinally aligned carbon fibres comprises the pyrolysis of a sheet of longitudinally aligned polyacrylonitrile fibres and the subsequent division of the sheet into a plurality of tapes.
  • said pyrolysis is preceded by a pre-oxidation step in which the fibres are heated in air.
  • the pyrolysis is preferably followed by a resin impregnation step in which the sheet of fibre is impregnated with a resin matrix material, and said division preferably takes place after said impregnation.
  • the pre-oxidation heat treatment may take place with the fibre heated to between 150 C. and 300 C.
  • Said division may be effected by a plurality of knifeedge slitting wheels; thus the wheels may comprise two or more separate sets which effect the desired splitting in two or more stages.
  • FIG. 1 is a fiow diagram of apparatus for carrying out the method of the present invention
  • FIG. 2 is a perspective view of the sheet slitting apparatus of FIG. 1.
  • 10 indicates a creel unit in which a plurality of creels 11 hold tows of polyacrylonitrile fibres of 1 /2 denier.
  • this creel unit there is embodied a sheet forming and retaining unit (not shown) such for instance as is described in co-pending application Ser. No. 759,730, filed Sept. 13, 1968, now abanndoned.
  • the creel unit produces sheets held together by a weft thread introduced at intervals into the warp fibres, each sheet being of approximately 18 inches width and each containing 50 tows, each tow comprising 10 fibres.
  • the eight sheets are maintained with a separation of some three inches between sheets, the sheets lying one above the other, and are fed into a roller unit generally indicated at 12.
  • the roller drive unit 12 comprises eight separate sets of four rollers, one of which is indicated at 13. These sets of rollers are mounted in parallel so that each roller set receives a single sheet which then passes round the four driven rollers 3,700,5 1 l Patented Oct. 24., 1972 which comprise the set and then passes out from the drive unit horizontally aligned with its entry.
  • the eight sheets are brought closer together as shown at 14 and pass through closely fitting orifices at 15 into a pre-oxidation furnace 16.
  • the atmosphere inside the furnace is maintained by a blower system and heater units (not shown) so that the ambient atmosphere within the furnace comprises air heated to a temperature of some 220 C.
  • a blower system 17 is provided to effect a controlled flow of air in the furnace.
  • the eight sheets pass over these rollers which cause them to move over a castellated path within the furnace, in this way achieving a long path length (40 feet) within a relatively compact furnace; the sheets are arranged to take some seven hours to pass through the furnace.
  • the fibres On emerging from the furnace through closely fitting orifices at 19 the fibres, still in their sheet form, pass into a second roller drive unit 20, which is identical to that shown at 12.
  • a second roller drive unit 20 By arranging the drive units 12 and 20 at either end of the furnace 16 the fibre can be arranged to be held under tension while it is being pre-oxidised. This prevents the shrinkage which would otherwise take place during this stage of the process.
  • a nitrogen atmosphere is maintained, a duct 23 being provided for the influx of nitrogen while a duct 24 is provided for the effiux of nitrogen plus waste gases.
  • the sheets are suspended above a floor (not shown).
  • the temperature is arranged to rise steadily from room temperature adjacent to seal unit 22 up to approximately 1000 C. at a point 25.
  • the dimensions of the furnace are so chosen that at the point 25 the majority of the pyrolysis of the fibres has taken place; this being so there is no necessity to arrange for any additional purging of reaction products in the subsequent treatment.
  • the compacted fibres next pass through a higher temperature portion 26 of the furnace.
  • sectional area of this part of the furnace is reduced by wall assemblies 27 which comprise heating units; this reduction in area helps to reduce the power required to provide the higher temperature heating.
  • the fibres are further heated to a temperature in the region of 1600 C.
  • the compacted fibres finally emerge from the furnace 21 by way of a second seal unit 28 which again uses a roller seal.
  • the seal unit 28 On leaving the seal unit 28 the fibres pass into a further furnace 29.
  • this furnace is shown as being separate from the furnace 21, it is in fact connected directly to the seal 28 and the entire apparatus forms a linear lay-out.
  • the seal 28 in fact divides the atmosphere within the furnace 21 from that in the furnace 29.
  • an atmosphere of argon is maintained and once again an input pipe 30 supplies argon while an output pipe 31 allows egress of argon and any products of reaction.
  • the fibre Within the furnace 29 the fibre is heated, still in its compacted form, to a temperature in this case of 2500 C., but which may be in the range of 1500 C. upwards.
  • the structure of the carbon fibre is made more pseudographitic. This stage can in fact be omitted completely and it is possible to produce useful carbon fibre with a carbonising furnace which merely heats the fibre up to a temperature of 1000 C. to 1200 C.
  • a seal unit 32 which is again similar to the unit 28 and prevents large escape of gases from the furnace 29.
  • the compacted fibres pass between a pair of driven rollers 33 and after passing through these rollers the compacted fibres are again split up into their eight discrete sheets into a resin impregnation unit generally indicated at 34.
  • the resin impregnation unit 34 is of the type described and claimed in co-pending application Ser. No. 887,864, filed December 24, 1968, now abandoned and uses coated paper as a transferring agent for an epoxy novolac resin. For simplicity, the course of a single sheet will be described; the remaining sheets follow an exactly similar course.
  • the upper sheet on entering the unit 34 it passes between a pair of reels 35 and 36 of resin coated release paper.
  • the release paper is itself impregnated with a release agent which affords the resin no permanent adhesion to the paper.
  • the reels 35 and 36 are mounted within a chamber 37 which is refrigerated so that the resin is maintained non-tacky.
  • the paper from the reels 35 and 36 is fed on to either side of the fibre sheet so that the coated side of the paper is against the fibre.
  • the sandwich" thus formed passes from the chamber 37 into a second chamber 38 and between a pair of heated rollers 39. On passing between these rollers, the combined effect of the heat and pressure evolved causes the resin to transfer from the release paper to the fibre sheet, thus impregnating the sheet with resin.
  • Each sheet then passes through a separate slitting device; only the device for the sheet passing through the rollers 40 is shown on the drawing, and is generally indicated at 41.
  • the slitting device 41 comprises two pairs of rollers 42 and 43, first and second sets of slitting wheels 44 and 45, which are rotated by drive means (not shown), and a take-up roller 46.
  • the sheet passes between the pairs of rollers 42 and 43, which maintains its overall sheet form, and intermediate these rollers the first set of slitting wheels 44 is mounted so that the saw-toothed wheels divide the sheet, in the present instance into three equal longitudinal portions.
  • the sheet thus divided passes through the rollers 43 and is then further divided by the slitting wheels 45.
  • the wheels 45 are mounted to divide the sheet (already divided into three parts) into six tapes.
  • cold air from a vortex tube is arranged to circulate in the vicinity of all the slitting wheels.
  • the sheet is thus formed into six tapes, and these tapes are then rolled on the take-up roller 46 to form six reels of tape on a single roller.
  • the roller may then be used to store the tapes, or may be itself divided into six parts carrying one tape reel.
  • the reel of tape thus produced may be used in various ways, particularly for the laying-up of composite articles by winding techniques.
  • the slitting device 41 may be used at any stage of the carbon fibre forming process described above but subsequent to the carbonising stage which takes place in the furnace 21. If the device 41 is interposed at any of the suitable positions upstream of the impregnation unit 34, it becomes necessary to maintain the separation of the tapes throughout the following treatment stages which could be difficult.
  • dry fibre is collected on a reel just prior to the impregnation stage and subsequently split by stationary knives in device 41 and wound onto smaller reels from which it may subsequently be reprocessed through 41 to produce still narrower tapes e.g. 10,000 filaments.
  • stationary knives are preferably angled to the longitudinal axis of the sheet in such a way that any snag not immediately cut by the knife causes the sheet to ride up the knife and cause the elfect of gravity to add to the cutting efiect.
  • the device 41 is only one way of dividing the sheet into tapes; various forms of stationary or moving knives or other dividers could be used, and the take-up arrangement could for instance comprise one or more rollers or further transverse slitting devices which produce stacks of the tapes cut to a pedetermined length.
  • each sheet is wound onto a reel the lower release paper being pulled away so as to wind only fibre plus top release paper.
  • the fibre is wound so as to be under the release paper.
  • the reel of fibre plus release paper is then taken to a separate slitting machine 41.
  • the release paper may be replaced by another paper or plastic film, which may be easily extensible and compressible, e.g. may be embossed or crinkled.
  • This extensibility helps winding, while the compressibility helps to compensate for variations in sheet thickness.
  • the re-winding is preferably performed with an edge guide so as to produce an accurately square-edged roll and make the slitting process more accurate.
  • a method of producing a tape of longitudinally aligned carbon fibers comprising the steps of:
  • step (b) pyrolyzing said sheet of step (a) in an inert pyrolyzing atmosphere and at elevated temperature and thereby converting said polyacrylonitrile fibers to carbon fibers;
  • step (a) A method as claimed in claim 1 and in which said pyrolysis is preceded by a pre-oxidation step in which the polyacrylonitrile fibres of step (a) are heated in air to a temperature between C. and 300 C.
  • a method of producing a tape of longitudinally aligned carbon fibers comprising the successive steps of: (a) providing a sheet of longitudinally aligned polyacrylonitrile fibers by assemblying a plurality of tows comprising individual polyacrylonitrile fibers into a sheet of material; (b) preoxidizing the fiber sheet of step (a) in heated air at a temperature of about 150 C. to about 300 C.; (c) pyrolyzing the preoxidized sheet of step (b) in an inert atmosphere at a temperature of at least 1000 C.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Reinforced Plastic Materials (AREA)
  • Treatment Of Fiber Materials (AREA)
  • Inorganic Fibers (AREA)
  • Carbon And Carbon Compounds (AREA)
US59874A 1969-08-04 1970-07-31 Method of producing tapes of longitudinally aligned carbon fibres Expired - Lifetime US3700511A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB38869/69A GB1286534A (en) 1969-08-04 1969-08-04 A method of producing carbon fibres

Publications (1)

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US3700511A true US3700511A (en) 1972-10-24

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US59874A Expired - Lifetime US3700511A (en) 1969-08-04 1970-07-31 Method of producing tapes of longitudinally aligned carbon fibres

Country Status (6)

Country Link
US (1) US3700511A (fr)
BE (1) BE754321A (fr)
CH (1) CH513771A (fr)
DE (1) DE2038784A1 (fr)
FR (1) FR2056490A5 (fr)
GB (1) GB1286534A (fr)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3873389A (en) * 1971-12-08 1975-03-25 Philco Ford Corp Pneumatic spreading of filaments
US4073670A (en) * 1975-11-27 1978-02-14 Ciba-Geigy Corporation Method of forming narrow ribbons of fibers in plastic material
US4080413A (en) * 1975-12-15 1978-03-21 United Technologies Corporation Porous carbon fuel cell substrates and method of manufacture
US4100004A (en) * 1976-05-11 1978-07-11 Securicum S.A. Method of making carbon fibers and resin-impregnated carbon fibers
US4131502A (en) * 1976-11-06 1978-12-26 Ciba-Geigy Corporation Method of laminating adhesive to a plurality of spaced fiber strips
US4301136A (en) * 1978-02-27 1981-11-17 Toray Industries, Incorporated Process for continuous graphitization of graphitizable precursor fibers
US4532169A (en) * 1981-10-05 1985-07-30 Ppg Industries, Inc. High performance fiber ribbon product, high strength hybrid composites and methods of producing and using same
JPH07115352B2 (ja) 1990-01-23 1995-12-13 東レ株式会社 プリプレグの製造方法
RU2342475C1 (ru) * 2007-06-21 2008-12-27 Закрытое акционерное общество "Институт новых углеродных материалов и технологий" (ЗАО "ИНУМиТ") Способ получения углеродных лент и устройство для его осуществления
US20160236454A1 (en) * 2015-02-12 2016-08-18 Zodiac Seats Uk Limited Tool for curing a composite component

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2507675C3 (de) * 1975-02-22 1981-09-17 M.A.N. Maschinenfabrik Augsburg-Nürnberg AG, 8000 München Verfahren zur Imprägnierung von Kohlenstoffasersträngen und -bändern

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3873389A (en) * 1971-12-08 1975-03-25 Philco Ford Corp Pneumatic spreading of filaments
US4073670A (en) * 1975-11-27 1978-02-14 Ciba-Geigy Corporation Method of forming narrow ribbons of fibers in plastic material
US4080413A (en) * 1975-12-15 1978-03-21 United Technologies Corporation Porous carbon fuel cell substrates and method of manufacture
US4100004A (en) * 1976-05-11 1978-07-11 Securicum S.A. Method of making carbon fibers and resin-impregnated carbon fibers
US4131502A (en) * 1976-11-06 1978-12-26 Ciba-Geigy Corporation Method of laminating adhesive to a plurality of spaced fiber strips
US4301136A (en) * 1978-02-27 1981-11-17 Toray Industries, Incorporated Process for continuous graphitization of graphitizable precursor fibers
US4532169A (en) * 1981-10-05 1985-07-30 Ppg Industries, Inc. High performance fiber ribbon product, high strength hybrid composites and methods of producing and using same
JPH07115352B2 (ja) 1990-01-23 1995-12-13 東レ株式会社 プリプレグの製造方法
RU2342475C1 (ru) * 2007-06-21 2008-12-27 Закрытое акционерное общество "Институт новых углеродных материалов и технологий" (ЗАО "ИНУМиТ") Способ получения углеродных лент и устройство для его осуществления
US20160236454A1 (en) * 2015-02-12 2016-08-18 Zodiac Seats Uk Limited Tool for curing a composite component
US11305499B2 (en) * 2015-02-12 2022-04-19 Safran Seats GB Limited Tool for curing a composite component
US11724469B2 (en) 2015-02-12 2023-08-15 Safran Seats GB Limited Tool for curing a composite component

Also Published As

Publication number Publication date
GB1286534A (en) 1972-08-23
FR2056490A5 (fr) 1971-05-14
BE754321A (fr) 1971-01-18
CH513771A (de) 1971-10-15
DE2038784A1 (de) 1971-02-18

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