EP0098025B1 - Verfahren zur Herstellung von aus Polyacrylnitril hergestellten Kohlenstoffasern - Google Patents

Verfahren zur Herstellung von aus Polyacrylnitril hergestellten Kohlenstoffasern Download PDF

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Publication number
EP0098025B1
EP0098025B1 EP19830200964 EP83200964A EP0098025B1 EP 0098025 B1 EP0098025 B1 EP 0098025B1 EP 19830200964 EP19830200964 EP 19830200964 EP 83200964 A EP83200964 A EP 83200964A EP 0098025 B1 EP0098025 B1 EP 0098025B1
Authority
EP
European Patent Office
Prior art keywords
temperature
fiber
heat treatment
pan
threadline
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
Application number
EP19830200964
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English (en)
French (fr)
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EP0098025A2 (de
EP0098025A3 (en
Inventor
David Arthur Schulz
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.)
BP Corp North America Inc
Original Assignee
BP Corp North America Inc
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Filing date
Publication date
Application filed by BP Corp North America Inc filed Critical BP Corp North America Inc
Publication of EP0098025A2 publication Critical patent/EP0098025A2/de
Publication of EP0098025A3 publication Critical patent/EP0098025A3/en
Application granted granted Critical
Publication of EP0098025B1 publication Critical patent/EP0098025B1/de
Expired legal-status Critical Current

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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
    • 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

Definitions

  • step c is carried out in a threadline operation.
  • step c is carried out completely integrated with the above steps a and b as explained in Example 3 hereinbelow. That means that the infusibilized PAN fiber is heatged on a bobbin first according to the requirement of step a, thereafter according to the requirement of step b and finally according to the requirement of step c.
  • Step c is preferably carried out in an inert atmosphere.
  • the cylindrical body of the bobbin can have an inside diameter of 7.62 cm and an outside diameter of about 8.89 cm with an overall length of about 27.94 cm.
  • the heat treatment of the fibers on the bobbins conveniently allows the bulk heat treatment of a large amount of fibers, at a relatively slow rate of increase in temperature to an elevated final temperature.
  • the surprising advantage of this heat treatment is that both the rate of reduction in nitrogen content of the fibers and the final nitrogen content are much lower as to compared to a heat treatment to the same final temperature using a conventional threadline arrangement.
  • the subsequent threadline heat treatment can be carried out at a high rate of movement of the yarn through the heating unit even if a considerably elevated temperature is used.
  • This threadline treatment straightens out the fibers and establishes the final fiber mechanical properties.
  • the first heat treatment is carried out by increasing the temperature at the rate of about 50°C for an hour from room temperature to about 800°C and thereafter increasing the temperature at a rate of 250°C per hour until the predetermined maximum temperature is reached and the maximum temperature is maintained for an additional two hours.
  • the maximum temperature is maintained in order to give all of the fibers on the bobbin the opportunity to reach a temperature equilibrium.
  • the first step is a carbonising in a threadline to a temperature of about 1300°C while the second step is a threadline operation at a higher temperature to improve the mechanical properties of the resulting carbon yarn.
  • Fig. 1 shows the weight percent of the aforementioned gases and carbon as a result of a first heat treatment in accordance with the invention.
  • the reduction in nitrogen content is particularly important because the loss of nitrogen during a subsequent threadline heat treatment at a higher temperature can result in serious degradation of the fibers.
  • the package was placed horizontally in a graphite tube induction furnace which was purged with nitrogen and fired at the rate of 50°C per hour to 800°C and thereafter temperature was raised at 250°C per hour to 1300°C. The final temperature was maintained for two hours and the package was allowed to cool back to room temperature. As a result of the heat treatment, the package had shrunk longitudinally about 3.81 cm to 5.08 cm from its original 25.4 cm length. The elemental nitrogen content was 0.9%.
  • the average tensile strength of the resulting fiber was 3447.10 3 kPa with a coefficient of variation of 1.3%.
  • the average Young's modulus for the resulting fiber was about 284.10 6 kPa with a coefficient of variation of 2.9%.
  • the average density of the fibers was 1.766 Mg per cubic meter with a coefficient of variation of 0.6%.
  • the average yield was 2397 m per kg with a coefficient of variation of 2.1%.
  • the carbon yarn obtained had an excellent appearance and was equivalent in quality to a carbon yarn produced by carbonizing with two separate threadlines in accordance with the prior art.
  • the second heat treatment was different in this example for Example 1 in that the furnace temperature was held at 2460°C, the take off tension was 100 grams, the line tension was 1950 grams, the line speed was 2134 cm per minute, and only water was applied to the carbon yarn instead of a finish.
  • the average properties of the fibers so obtained was a tensile strength of 2482.10 3 kPa, Young's modulus of 668.10 6 kPa, density of 2.080 Mg per cubic meter, and a yield of 2832 m per kg.
  • the reduction in strength over the values obtained from Example 1 indicates that new flaws were introduced during the subsequent thermal processing and handling.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Inorganic Fibers (AREA)

Claims (1)

  1. Verfahren zur Herstellung einer Kohlenstoffaser auf PAN-Basis, gekennzeichnet durch die Schritte:
    a. Erhitzen einer unschmelzbar gemachten PAN-Faser aus einer Spule mit einem Anstieg von 50 bis 500°C pro Stunde bis auf eine Temperatur im Bereich von etwa 1300 bis 1700°C;
    b. Halten der Faser auf einer Temperatur innerhalb dieses Bereichs bis der Gehalt der Faser an elementaren Stickstoff höchstens 1 Gew.% beträgt und
    c. weiteres Erhitzen der Faser auf eine Temperatur von 1900°C oder darüber.
EP19830200964 1982-06-29 1983-06-28 Verfahren zur Herstellung von aus Polyacrylnitril hergestellten Kohlenstoffasern Expired EP0098025B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US39339282A 1982-06-29 1982-06-29
US393392 1982-06-29

Publications (3)

Publication Number Publication Date
EP0098025A2 EP0098025A2 (de) 1984-01-11
EP0098025A3 EP0098025A3 (en) 1986-03-26
EP0098025B1 true EP0098025B1 (de) 1989-05-24

Family

ID=23554509

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19830200964 Expired EP0098025B1 (de) 1982-06-29 1983-06-28 Verfahren zur Herstellung von aus Polyacrylnitril hergestellten Kohlenstoffasern

Country Status (4)

Country Link
EP (1) EP0098025B1 (de)
JP (1) JPS5953720A (de)
CA (1) CA1181555A (de)
DE (1) DE3379907D1 (de)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1219410A (en) * 1982-09-27 1987-03-24 David A. Schulz Process for improving carbon fibers
JPH0633529B2 (ja) * 1984-09-14 1994-05-02 呉羽化学工業株式会社 炭素繊維の製造方法
US5268158A (en) * 1987-03-11 1993-12-07 Hercules Incorporated High modulus pan-based carbon fiber
JP5635740B2 (ja) * 2009-03-26 2014-12-03 東邦テナックス株式会社 ポリアクリロニトリル系炭素繊維ストランド及びその製造方法
CN102465376A (zh) * 2010-11-09 2012-05-23 张孟福 一种高碳化纤维编织填料的制备方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1217852A (en) * 1967-03-09 1970-12-31 Courtaulds Ltd Continuous filaments of carbon
FR1581203A (de) * 1967-08-15 1969-09-12
GB1257313A (de) * 1968-05-15 1971-12-15
CA1015514A (en) * 1971-06-11 1977-08-16 Charles M. Clarke Production of filamentary materials
DE2235453A1 (de) * 1971-08-05 1973-02-22 Hughes Aircraft Co Hohlleiter-bauteil und verfahren zu dessen herstellung

Also Published As

Publication number Publication date
CA1181555A (en) 1985-01-29
JPS5953720A (ja) 1984-03-28
JPH0213046B2 (de) 1990-04-03
EP0098025A2 (de) 1984-01-11
DE3379907D1 (en) 1989-06-29
EP0098025A3 (en) 1986-03-26

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