EP3348684B1 - Procédé de fabrication de fibre de carbone et appareil de fabrication de fibre de carbone - Google Patents

Procédé de fabrication de fibre de carbone et appareil de fabrication de fibre de carbone Download PDF

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Publication number
EP3348684B1
EP3348684B1 EP17000054.1A EP17000054A EP3348684B1 EP 3348684 B1 EP3348684 B1 EP 3348684B1 EP 17000054 A EP17000054 A EP 17000054A EP 3348684 B1 EP3348684 B1 EP 3348684B1
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Prior art keywords
carbon fiber
plasma
module
microwave
chamber
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German (de)
English (en)
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EP3348684A1 (fr
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Chih-Yung Wang
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UHT Unitech Co Ltd
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UHT Unitech Co Ltd
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    • 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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • 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
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/40—Fibres of carbon

Definitions

  • the present invention relates to a carbon fiber manufacturing technique, and more particularly to a carbon fiber manufacturing method and a carbon fiber manufacturing apparatus which can greatly improve the sizing quality of a carbon fiber and effectively reduce the cost of the carbon fiber production equipment and the working time.
  • Carbon fibers are classified into carbon fibers or graphite fibers according to their carbon contents, which have excellent mechanical properties and electrical properties and can be widely used in various applications.
  • a conventional carbon fiber is achieved by bundling precursor fibers, such as polyacrylonitrile fibers, to form a carbon fiber precursor fiber bundle, and then the carbon fiber precursor fiber bundle is calcined (high-temperature carbonization) to form the carbon fiber.
  • PAN polyacrylonitrile
  • the carbon fiber precursor fiber bundles are heated to form carbon fibers or graphite fibers by different heating apparatuses according to the application of the carbon fibers.
  • the carbon content of the fibers of graphite fibers is 90% or more, forming a two-dimensional carbocyclic planar net structure and a graphite layer structure having parallel layers.
  • the results show that the crystalline region of a high-strength carbon fiber is composed of 5-6 graphite layers, and the crystalline region of a high-strength and high-modulus carbon fiber is composed of 10-20 graphite layers. Theoretically and practically, it is pointed out that the larger the crystalline thickness of the graphite layer is, the higher the tensile modulus of the carbon fiber is.
  • the surface of the carbon fiber after the high-temperature carbonization step is usually coated with a layer of oiling agent (a resin oiling agent is generally used, it is called as a sizing step) before it leaves the factory.
  • the layer of oiling agent is used to protect the fiber from breakage due to friction in the subsequent step to affect the overall quality of the carbon fiber.
  • the surfaces of untreated carbon fibers adsorb impurities thereon. Since these impurities are present between the surface of the carbon fiber and the resin oiling agent, the adhesion between the carbon fiber and the resin oiling agent is insufficient, and the purpose of protecting the fiber cannot be achieved
  • the surface of the carbon fiber is excessively finely formed due to high-temperature sintering, and there are few functional groups on the surface.
  • the fiber and the resin oiling agent cannot be bonded fully in the sizing step.
  • a heat treatment or electrolysis technique can be applied to the surface treatment of the fiber after the high-temperature carbonization step, and then the sizing step is performed in order to improve the bonding of the fiber and the resin oiling agent.
  • the surface treatment of the carbon fiber is performed by means of heat treatment
  • the carbon fiber is treated at a temperature in the range of 500°C to 800°C for 1-10 minutes.
  • a relatively long period of time is required.
  • the heat treatment is always performed with a large number of fibers at a time, so it is difficult to control the processing quality.
  • the surface treatment of the carbon fiber is performed by means of electrolysis, at least one drying process is required before the surface of the fiber is coated with the oiling agent. This also takes more time.
  • a change of the electrolyte may affect the processing quality. Even the surface of the fiber may have depositions.
  • US 2016257797 discloses a process for preparing a carbon fiber containing an epoxy or amine sizing agent bound to its surface whereby initial functionalization may be provided for example by a plasma surface treatment.
  • the primary object of the present invention is to provide a carbon fiber manufacturing method according to claim 1, which can greatly improve the sizing quality of a carbon fiber and effectively reduce the cost of the carbon fiber production equipment and the working time.
  • the carbon fiber manufacturing method of the present invention comprises providing a raw material step, providing a carbon fiber precursor fiber bundle; performing a high-temperature carbonization step, the carbon fiber precursor fiber bundle being heated to form a carbon fiber having a predetermined carbon content; performing a plasma surface treatment step, a plasma gas flow with a predetermined power being provided to act on the carbon fiber at a predetermined time so that a surface of the carbon fiber is formed with a plasma-modified configuration; performing a sizing step, the plasma-modified configuration being coated with a resin oiling agent; and performing a drying step, the resin oiling agent coated on the plasma-modified configuration being processed with drying so that the resin oiling agent is firmly adhered to the surface of the carbon fiber.
  • the surface of the carbon fiber is roughened and provided with functional groups, which is beneficial to enhance the interface bonding of the resin oiling agent and the carbon fiber in the subsequent sizing step so as to improve the sizing quality of the carbon fiber greatly.
  • the structure of the carbon fiber is more stable and reliable.
  • the plasma surface treatment belongs to a dry-type and fast surface treatment technique to effectively reduce the cost of the carbon fiber production equipment and the working time.
  • the carbon fiber precursor fiber bundle is guided into a chamber.
  • the chamber is formed with at least one microwave field concentration area therein, and is provided with a gas supply assembly to supply an inert gas and a microwave generating assembly to supply a high-frequency microwave.
  • the electric field of the high-frequency microwave produces a sensing current to heat up and produce a high temperature quickly with the carbon fiber precursor fiber bundle passing through the microwave field concentration area.
  • the chamber is provided with at least one pair of microwave-sensitive materials.
  • the microwave-sensitive materials are one of graphite, carbide, magnetic compound, nitride, and ionic compound or a combination thereof.
  • the inert gas is nitrogen, argon, helium, or a combination thereof.
  • the frequency of the high-frequency microwave is in the range of 300-30,000 MHz, and its microwave power density is in the range of 1-1000kW/m3.
  • the chamber is a flat panel chamber.
  • the chamber is an elliptic chamber.
  • the plasma gas flow with a power of 100-10000 watts acts on the carbon fiber for 10-1000 milliseconds.
  • an atmospheric plasma gas flow with a power of 100-10000 watts acts on the carbon fiber for 10-1000 milliseconds.
  • a low-pressure plasma gas flow with a power of 100-10000 watts acts on the carbon fiber for 10-1000 milliseconds.
  • a microwave plasma gas flow with a power of 100-10000 watts acts on the carbon fiber for 10-1000 milliseconds.
  • a glow plasma gas flow with a power of 100-10000 watts acts on the carbon fiber for 10-1000 milliseconds.
  • the carbon fiber precursor fiber bundle has a surface not processed with a pre-oxidation treatment.
  • the carbon fiber precursor fiber bundle has a surface processed with a pre-oxidation treatment in advance.
  • the resin oiling agent is a thermosetting resin oiling agent.
  • the resin oiling agent is a thermoplastic resin oiling agent.
  • the carbon content of the carbon fiber is in the range of 80%-90%.
  • the carbon fiber manufacturing apparatus of the present invention comprises a feeding module, a receiving module, a high-temperature carbonization module, a plasma surface treatment module, and a sizing module.
  • the receiving module is disposed in the vicinity of the feeding module.
  • the feeding module and the receiving module constitute a carbon fiber drag route.
  • the high-temperature carbonization module is disposed at the carbon fiber drag route and located between the feeding module and the receiving module for heating the carbon fiber drag route.
  • the plasma surface treatment module is disposed at the carbon fiber drag route and located between the high-temperature carbonization module and the receiving module for supplying a plasma gas flow to the carbon fiber drag route.
  • the sizing module is disposed at the carbon fiber drag route and located between the plasma surface treatment module and the receiving module for coating a resin oiling agent on the surface of a carbon fiber.
  • the carbon fiber manufacturing apparatus of the present invention can be operated in the integrated operation of the feeding module, the high-temperature carbonization module, the plasma surface treatment module, the sizing module, and the receiving module.
  • a carbon fiber precursor fiber bundle released from the feeding module is sequentially processed at a predetermined speed to perform the steps of high-temperature carbonization, plasma surface treatment, sizing, and so on, in a relatively more active and reliable manner.
  • the carbon fiber precursor fiber bundle is heated to form the carbon fiber, and then the surface of the carbon fiber is formed with the resin oiling agent.
  • the surface of the carbon fiber is roughened and provided with functional groups, which is beneficial to enhance the interface bonding of the resin oiling agent and the carbon fiber in the subsequent sizing procedure so as to improve the sizing quality of the carbon fiber greatly.
  • the structure of the carbon fiber is more stable and reliable.
  • the plasma surface treatment belongs to a dry-type and fast surface treatment technique to effectively reduce the cost of the carbon fiber production equipment and the working time.
  • the high-temperature carbonization module has a chamber for the carbon fiber drag route or the carbon fiber precursor fiber bundle to pass therethrough.
  • the chamber is formed with at least one microwave field concentration area and supplies an inert gas and a high-frequency microwave. Under the protection of the inert gas atmosphere, the electric field of the high-frequency microwave produces a sensing current to heat up and produce a high temperature quickly with the carbon fiber precursor fiber bundle passing through the microwave field concentration area.
  • the high-temperature carbonization module has a chamber for the carbon fiber drag route or the carbon fiber precursor fiber bundle to pass therethrough.
  • the chamber is formed with at least one microwave field concentration area and provided with a gas supply assembly to supply an inert gas and a microwave generating assembly to supply a high-frequency microwave.
  • the electric field of the high-frequency microwave produces a sensing current to heat up and produce a high temperature quickly with the carbon fiber precursor fiber bundle passing through the microwave field concentration area.
  • the plasma surface treatment module is provided with at least one plasma generator.
  • the plasma surface treatment module is provided with at least one plasma generator located at upper and lower positions of the carbon fiber drag route, respectively.
  • the chamber is a flat plate chamber.
  • the chamber is a flat plate chamber, and the chamber is provided with at least one pair of microwave-sensitive materials.
  • the chamber is an elliptic chamber.
  • the chamber is an elliptic chamber, and the chamber is provided with at least one pair of microwave-sensitive materials.
  • the plasma generator is able to generate the plasma gas flow having a power in the range of 100-10000 Watts.
  • the plasma generator is able to generate an atmospheric plasma gas flow having a power in a range of 100-10000 Watts.
  • the plasma generator is able to generate a low-pressure plasma gas flow having a power in the range of 100-10000 Watts.
  • the plasma generator is able to generate a microwave plasma gas flow having a power in the range of 100-10000 Watts.
  • the plasma generator is able to generate a glow plasma gas flow having a power in the range of 100-10000 Watts.
  • the sizing module is provided with at least one reservoir.
  • the carbon fiber manufacturing apparatus further comprises a drying module.
  • the drying module is disposed at the carbon fiber drag route between the sizing module and the receiving module for the resin oiling agent to be adhered to the surface of the carbon fiber firmly.
  • the surface of the carbon fiber can be roughened and provided with the functional groups, which is beneficial to enhance the interface bonding of the resin oiling agent and the carbon fiber in the subsequent sizing step.
  • the structure of the carbon fiber is more stable and reliable.
  • the microwave focusing heating way the same apparatus can be applied to a carbon fiber precursor fiber bundle whose surface has not been processed with a pre-oxidation treatment or a carbon fiber precursor fiber bundle whose surface has been processed with a pre-oxidation treatment in advance.
  • the apparatus can be used to produce general carbon fibers or high modulus carbon fibers (graphite fibers) so as reduce the cost of the carbon fiber production equipment and the working time effectively.
  • the present invention discloses a carbon fiber manufacturing method which can greatly improve the sizing quality of carbon fibers and effectively reduce the cost of the carbon fiber production equipment and the working time.
  • the carbon fiber manufacturing method of the present invention comprises providing a raw material step, performing a high-temperature carbonization step, performing a plasma surface treatment step, and performing a sizing step.
  • the carbon fiber manufacturing method further comprises performing a drying step after the sizing step. Referring to FIG. 1 through FIG. 5 , the steps are described in details as below.
  • a carbon fiber precursor fiber bundle is provided to be processed to form a carbon fiber.
  • the carbon fiber precursor fiber bundle may be formed of rayon, poly vinyl alcohol, vinylidene chloride, polyacrylonitrile (PAN), pitch, and the like.
  • the surface of the carbon fiber precursor fiber bundle may have not been processed with a pre-oxidation treatment or have been processed with a pre-oxidation treatment in advance.
  • the carbon fiber precursor fiber bundle is heated to form the carbon fiber having a predetermined carbon content.
  • the carbon fiber precursor fiber bundle 70A is guided into a chamber 31 of a high-temperature carbonization module 30.
  • the chamber 31 is formed with at least one microwave field concentration area 311 therein, and is provided with a gas supply assembly 32 to supply an inert gas and a microwave generating assembly 33 to supply a high-frequency microwave.
  • the electric field of the high-frequency microwave produces a sensing current to heat up and produce a high temperature quickly with the carbon fiber precursor fiber bundle 70A passing through the microwave field concentration area 311, enabling the carbon fiber precursor fiber bundle to form the carbon fiber 70B having a predetermined carbon content.
  • the carbon content of the carbon fiber 70B is in the range of 80%-90%.
  • a plasma gas flow with a predetermined power is provided to act on the carbon fiber 70B at a predetermined time, such that the surface of the carbon fiber 70B is formed with a plasma-modified configuration 71, shown in FIG. 3 , which is rougher or has more functional groups relative to the carbon fiber precursor fiber bundle 70A.
  • the plasma-modified configuration 71 on the surface of the carbon fiber 70B is coated with a resin oiling agent 80, so that the surface of the carbon fiber 70B has the resin oiling agent 80, as shown in FIG. 4 .
  • the resin oiling agent 80 is coated on the surface of the carbon fiber 70B by soaking or immersing.
  • the resin oiling agent 80 may be a thermosetting resin oiling agent or a thermoplastic resin oiling agent.
  • a drying treatment is applied to the resin oiling agent 80 coated on the plasma-modified configuration 71 so that the resin oiling agent 80 is firmly adhered to the surface of the carbon fiber 70B.
  • the drying treatment is carried out by ultraviolet irradiation, cooling, drying or air-drying for the resin oiling agent to be bonded to the surface of the carbon fiber.
  • an atmospheric plasma gas flow, a low-pressure plasma gas flow, a microwave plasma gas flow, or a glow plasma gas flow with a power of 100-10000 watts may be used to act on the carbon fiber 10B for 10-1000 milliseconds. Since the plasma gas flow contains particles having energy, the impurities that originally adhere to the surface of the carbon fiber 10B can be broken to form small molecules by the impact of the plasma gas flow through the physical reaction (collision) of the plasma gas flow, and then the small molecules are blown away from the surface of the carbon fiber 70B by the air flow, so that the surface of the carbon fiber 70B is clean.
  • the resin oiling agent 80 can be completely in contact with the carbon fiber 70B to increase the bonding effect.
  • the impact of the plasma gas flow will also form the plasma-modified configuration 71 on the surface of the carbon fiber 70B.
  • the plasma-modified configuration 71 is rougher relative to the carbon fiber precursor fiber bundle 70A, and is further formed with pores.
  • the surface of the carbon fiber 70B is roughened or formed with the pores, which is beneficial to increase the contact area between the resin oiling agent 80 and the carbon fiber 70B in the subsequent sizing step.
  • the resin oiling agent 80 penetrates into the pores, and the resin oiling agent 80 is anchored between the pores to form an anchor effect to enhance the bonding effect of the resin oiling agent 80 and the carbon fiber 70B.
  • the plasma gas flow also makes the surface of the carbon fiber 70B generate a chemical reaction at the same time, so that at least one functional group (such as -OH, -N, etc.) is added to the surface of the carbon fiber 70B.
  • the surface tension of the surface of the carbon fiber 70B is increased due to the presence of the functional group, which is beneficial to improve the wetting effect for the resin oiling agent 80 to be coated on the carbon fiber 70B. That is, the contact angle of the resin oiling agent 80 to the carbon fiber 70B becomes small, so that the resin oiling agent 80 can be quickly or instantaneously coated on the carbon fiber 70B, and the speed of the sizing step is increased, thereby accelerating the overall production speed of the carbon fiber 70B.
  • the presence of the functional group such as the OH group reacts with the resin oiling agent 80, such as epoxy resin (Epoxy), to generate hydrogen bonding, thereby increasing the bonding effect.
  • the surface of the carbon fiber 70B is roughened and provided with functional groups, which is beneficial to enhance the interface bonding of the resin oiling agent 80 and the carbon fiber 70B in the subsequent sizing step so as to improve the sizing quality of the carbon fiber 70B greatly.
  • the structure of the carbon fiber is more stable and reliable.
  • the plasma surface treatment belongs to a dry-type and fast surface treatment technique to effectively reduce the cost of the carbon fiber production equipment and the working time.
  • the foregoing inert gas may be nitrogen, argon, helium, or a combination thereof.
  • the frequency of the high-frequency microwave may be in the range of 300-30,000 MHz, and its microwave power density may be in the range of 1-1000kW/m3.
  • the chamber 31 of the high-temperature carbonization module 30 may be an elliptic chamber, or the chamber 31 may be a flat plate chamber as shown in FIG. 5 .
  • the chamber 31 is provided with a pair of microwave-sensitive materials 34 therein, thereby enhancing the focusing effect on the microwave field in order to further accelerate the high-temperature carbonization process.
  • the microwave-sensitive materials 34 may be one of graphite, carbide, magnetic compound, nitride, and ionic compound or a combination thereof.
  • the carbonization of the carbon fiber is enhanced rapidly and more crystalline carbons are formed and stacked, which leads to the formation of larger graphite crystalline molecules, namely, larger graphite crystalline thickness, while deriving a higher microwave induction heating effect is derived.
  • Such a cycle generates an autocatalytic reaction, enabling the carbon fiber to be rapidly heated to the graphitization temperature (1500- 3000°C), and carbon atoms are reconstructed and rearranged more rapidly to form a graphite layer.
  • the same apparatus can be applied to a carbon fiber precursor fiber bundle whose surface has not been processed with a pre-oxidation treatment or a carbon fiber precursor fiber bundle whose surface has been processed with a pre-oxidation treatment in advance. It is only necessary to adjust the microwave power for the production, the apparatus can be used to produce general carbon fibers (1000-1500°C) or high modulus carbon fibers (graphite fibers).
  • an object to be tested that the resin oiling agent after the drying step is firmly adhered to the surface of the carbon fiber, and the treatment conditions in the plasma surface treatment step are shown in Table 1 below: Table 1: the conditions of the plasma surface treatment plasma gas consumption N 2 200 L/min CDA 0.4 L/min plasma gas amount 200.4 L/min plasma power 0 ⁇ 1000 W plasma surface treatment time 0.025 ⁇ 0.100 sec. carbon fiber yarn width 7 mm yarn per unit time receiving capacity 0.28 J/s distance 1 mm
  • the ILSS strength (interlayer bonding force) was measured for an object to be tested in an environment of a temperature of 23°C and a humidity of 50% RH by using an INSTRON measuring machine according to ASTM 2344, and the results are shown in Table 2 below: Table 2: the relationship between the plasma surface treatment power (W), the processing time (sec.), and the interlayer bonding force (MPa) (epoxy resin used as the resin oiling agent) of PAN carbon fiber 12K.
  • the carbon fiber without the plasma surface treatment the interlayer bonding force of the object to be tested is only 70MPa.
  • the processing time is 0.075 seconds and the plasma power is increased from the untreated (0W, without plasma power) to 1000W, the interlayer bonding force is increased from 70MPa to 89MPa. That is, the interlayer bonding force is increased to 127%.
  • FIG. 6a shows a SEM image of the object to be tested without the plasma treatment.
  • FIG. 6b shows a SEM image of the object to be tested with the plasma treatment.
  • the SEM image of the object to be tested without the plasma surface treatment illustrates a void H between the resin oiling agent 80 and the carbon fiber 70B because the surface of the carbon fiber 70B is smooth and doesn't have functional groups.
  • the void H causes a decrease in the strength of the object to be tested. That is to say, the bonding force between the carbon fiber and the resin oiling agent is insufficient for protecting the fiber.
  • the SEM image of the object to be tested with the plasma surface treatment illustrates that there is no void between the resin oiling agent 80 and the carbon fiber 70B because the surface of the carbon fiber 70B is rough and has functional groups (such as -OH, -N, etc.).
  • the resin oiling agent 80 and the carbon fiber 70B are bonded tightly, so that the strength of the object to be tested is enhanced. That is, the adhesion between the carbon fiber and the resin oiling agent is enhanced, so that the purpose of protecting the fiber can be achieved.
  • the present invention further discloses a carbon fiber manufacturing apparatus which can greatly improve the sizing quality of carbon fibers and effectively reduce the cost of the carbon fiber production equipment and the working time.
  • the carbon fiber manufacturing apparatus of the present invention comprises a feeding module 10, a receiving module 20, a high-temperature carbonization module 30, a plasma surface treatment module 40, and a sizing module 50.
  • the feeding module 10 is to perform the step of providing a raw material in the carbon fiber manufacturing method, and is used to supply a carbon fiber precursor fiber bundle 70A to be processed into a carbon fiber 70B.
  • the receiving module 20 is disposed in the vicinity of the feeding module 10, and corresponds to the feeding module 10 to constitute a carbon fiber drag route.
  • the receiving module 20 includes a yarn winding assembly 21 to receive the carbon fiber 70B.
  • the yarn winding assembly 21 performs a drag action on the carbon fiber 70B to be received.
  • the high-temperature carbonization module 30 is to perform the high-temperate carbonization step in the carbon fiber manufacturing method.
  • the high-temperature carbonization module 30 is disposed at the carbon fiber drag route between the feeding module 10 and the receiving module 20 for heating the carbon fiber precursor fiber bundle 70A, enabling the carbon fiber precursor fiber bundle 70A to become the carbon fiber 70B having a predetermined carbon content.
  • the plasma surface treatment module 40 is to perform the plasma surface treatment step in the carbon fiber manufacturing method.
  • the plasma surface treatment module 40 is disposed at the carbon fiber drag route between the high-temperature carbonization module 30 and the receiving module 20 to provide a plasma gas flow with a predetermined power to act on the carbon fiber 70B, such that the surface of the carbon fiber 70B is formed with a plasma-modified configuration 71 which is rougher or has more functional groups relative to the carbon fiber precursor fiber bundle 70A.
  • the sizing module 50 is to perform the sizing step in the carbon fiber manufacturing method.
  • the sizing module 50 is disposed at the carbon fiber drag route between the plasma surface treatment module 40 and the receiving module 20 for the plasma-modified configuration 71 on the surface of the carbon fiber 70B to be coated with a resin oiling agent 80.
  • the sizing module 50 is provided with at least one reservoir 51 for storing the resin oiling agent 80.
  • the carbon fiber manufacturing apparatus of the present invention may further comprise a drying module 60.
  • the drying module 60 is to perform the drying step in the carbon fiber manufacturing method.
  • the drying module 60 is disposed at the carbon fiber drag route between the sizing module 50 and the receiving module 20 for the resin oiling agent 80 to be firmly adhered to the surface of the carbon fiber 70B.
  • the drying module 60 is provided with at least one blast furnace 61 to generate hot blast.
  • the carbon fiber manufacturing apparatus of the present invention can be operated in the integrated operation of the feeding module 10, the high-temperature carbonization module 30, the plasma surface treatment module 40, the sizing module 50, and the receiving module 20.
  • the carbon fiber precursor fiber bundle 70A released from the feeding module 10 is sequentially processed at a predetermined speed to perform the steps of high-temperature carbonization, plasma surface treatment, sizing, and so on, in a relatively more active and reliable manner.
  • the carbon fiber precursor fiber bundle 70A is heated to form the carbon fiber 70B, and then the surface of the carbon fiber 70B is formed with the resin oiling agent 80.
  • the plasma surface treatment module 40 is provided with at least one plasma generator 41 for generating a plasma gas flow.
  • the plasma surface treatment module 40 is provided with at least one plasma generator 41 disposed at the upper and lower positions of the carbon fiber drag route respectively for generating a plasma gas flow to act on the surface of the carbon fiber 70B.
  • the surface of the carbon fiber can be roughened and provided with the functional groups by the plasma surface treatment step, which is beneficial to enhance the interface bonding of the resin oiling agent and the carbon fiber in the subsequent sizing step.
  • the structure of the carbon fiber is more stable and reliable to improve the quality of the carbon fiber, thereby accelerating the overall production speed of the carbon fiber.
  • the microwave focusing heating way the same apparatus can be applied to a carbon fiber precursor fiber bundle whose surface has not been processed with a pre-oxidation treatment or a carbon fiber precursor fiber bundle whose surface has been processed with a pre-oxidation treatment in advance.
  • the apparatus can be used to produce general carbon fibers or high modulus carbon fibers (graphite fibers) so as reduce the cost of the carbon fiber production equipment and the working time effectively.

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Claims (18)

  1. Un procédé de fabrication de fibre de carbone, comprenant :
    une étape de fourniture de matière première, fournissant un faisceau de fibres précurseur de fibre de carbone (70A) ; la réalisation d'une étape de carbonisation à haute température, le faisceau de fibres précurseurs de fibre de carbone (70A) étant chauffé pour former une fibre de carbone (70B) ayant une teneur en carbone dans une fourchette allant de 80% à 90% ; la réalisation d'une étape de traitement de surface par plasma, un flux de gaz plasma d'une puissance de 100 à 1.000 watts agissant sur la fibre de carbone (70B) pendant 10 à 1.000 millisecondes de sorte qu'une surface de la fibre de carbone (70B) est formée avec une configuration modifiée par plasma (71) ; la réalisation d'une étape de dimensionnement, la configuration modifiée par plasma (71) étant revêtue d'un agent d'huilage de résine (80); et la réalisation d'une étape de séchage, l'agent d'huilage de résine (80) déposé sur la configuration modifiée par plasma (71) étant traité par séchage de sorte que l'agent d'huilage de résine (80) adhère fermement à la surface de la fibre de carbone (70B) ; dans lequel pendant l'étape de carbonisation à haute température, le faisceau de fibres précurseur de fibre de carbone (70A) est guidé dans une chambre (31), la chambre (31) étant formée avec au moins une zone de concentration de champ micro-ondes (311) et étant pourvue d'un ensemble d'alimentation en gaz (32) pour fournir un gaz inerte et d'un ensemble de génération de micro-ondes (33) pour fournir une micro-onde de haute fréquence sous la protection de l'atmosphère de gaz inerte, un champ électrique de micro-onde de haute fréquence produisant un courant de détection pour chauffer et produire rapidement une température élevée avec le faisceau de fibres précurseur de fibre de carbone (70A) traversant la zone de concentration du champ micro-ondes (311) ; dans lequel la chambre (31) est pourvue d'au moins une paire de matériaux sensibles aux micro-ondes (34).
  2. Le procédé de fabrication de fibre de carbone selon la revendication 1, dans lequel les matériaux sensibles aux micro-ondes (34) sont l'un des suivants : graphite, carbure, composé magnétique, nitrure, composé ionique ou une combinaison de ceux-ci.
  3. Le procédé de fabrication de fibre de carbone selon la revendication 1, dans lequel le gaz inerte est l'un des suivants : azote, argon, hélium ou une combinaison de ceux-ci.
  4. Le procédé de fabrication de fibre de carbone selon la revendication 1, dans lequel la fréquence du micro-onde de haute fréquence se situe dans la fourchette allant de 300 à 30.000 MHz et sa densité de puissance micro-ondes dans la fourchette allant de 1 à 1.000 kW/m3.
  5. Le procédé de fabrication de fibre de carbone selon la revendication 1, dans lequel la chambre (31) est une chambre elliptique.
  6. Le procédé de fabrication de fibre de carbone selon la revendication 1, dans lequel la chambre (31) est une chambre à panneau plat.
  7. Le procédé de fabrication de fibre de carbone selon l'une quelconque des revendications précédentes, dans lequel pendant l'étape de traitement de surface par plasma, le flux de gaz plasma est soit un flux de gaz plasma atmosphérique, soit un flux de gaz plasma basse pression, soit un flux de gaz plasma micro-ondes ou soit un flux de gaz plasma luminescent ; le flux de gaz plasma agit sur la fibre de carbone (70B).
  8. Le procédé de fabrication de fibre de carbone selon l'une quelconque des revendications précédentes, dans lequel le faisceau de fibres précurseur de fibre de carbone (70A) a une surface non traitée par un traitement de pré-oxydation.
  9. Le procédé de fabrication de fibre de carbone selon l'une quelconque des revendications 1 à 7, dans lequel le faisceau de fibres précurseur de fibre de carbone (70A) a une surface traitée à l'avance avec un traitement de pré-oxydation.
  10. Le procédé de fabrication de fibre de carbone selon l'une quelconque des revendications précédentes, dans lequel l'agent d'huilage de résine (80) est un agent d'huilage de résine thermodurcissable.
  11. Le procédé de fabrication de fibre de carbone selon l'une quelconque des revendications 1 à 9, dans lequel l'agent d'huilage de résine (80) est un agent d'huilage de résine thermoplastique.
  12. Un appareil de fabrication de fibre de carbone, comprenant :
    un module d'alimentation (10) et un module de réception (20), le module de réception (20) étant disposé à proximité du module d'alimentation (10), le module d'alimentation (10) et le module de réception (20) constituant une voie de traînée pour la fibre de carbone ; un module de carbonisation à haute température (30), disposé au niveau de la voie de traînée pour la fibre de carbone et situé entre le module d'alimentation (10) et le module de réception (20) pour chauffer la voie de traînée pour la fibre de carbone ; un module de traitement de surface par plasma (40), disposé sur la voie de traînée pour la fibre de carbone et situé entre le module de carbonisation à haute température (30) et le module de réception (20) pour fournir un flux de gaz plasma à la voie de traînée pour la fibre de carbone; et un module de dimensionnement (50), disposé au niveau de la voie de traînée pour la fibre de carbone et situé entre le module de traitement de surface par plasma (40) et le module de réception (20) ; dans lequel le module de carbonisation à haute température (30) a une chambre (31), un ensemble d'alimentation en gaz (32) et un ensemble de génération de micro-ondes (33), la voie de traînée pour la fibre de carbone passe à travers la chambre (31), l'ensemble d'alimentation en gaz (32) est utilisé pour fournir un gaz inerte, et l'ensemble de génération de micro-ondes (33) est utilisé pour fournir une micro-onde de haute fréquence ; dans lequel la chambre (31) est une chambre à panneau plat et pourvue d'au moins une paire de matériaux sensibles aux micro-ondes (34).
  13. L'appareil de fabrication de fibre de carbone selon la revendication 12, dans lequel le module de traitement de surface par plasma (40) est pourvu d'au moins un générateur de plasma (41).
  14. L'appareil de fabrication de fibre de carbone selon la revendication 12 ou 13, dans lequel le module de traitement de surface par plasma (40) est pourvu d'au moins un générateur de plasma (41), situé en position supérieure et d'un situé en position inférieure de la voie de traînée pour la fibre de carbone, respectivement.
  15. L'appareil de fabrication de fibre de carbone selon l'une quelconque des revendications 12 à 14, dans lequel la chambre (31) est une chambre elliptique.
  16. L'appareil de fabrication de fibre de carbone selon la revendication 13 ou 14, dans lequel le générateur de plasma est capable de générer un flux de gaz plasma, un flux de gaz plasma atmosphérique, un flux de gaz plasma basse pression, un flux de gaz plasma micro-ondes ou un flux de gaz plasma luminescent ayant une puissance dans la fourchette allant de 100 à 10.000 watts.
  17. L'appareil de fabrication de fibre de carbone selon l'une quelconque des revendications 12 à 16, dans lequel le module de dimensionnement (50) est pourvu d'au moins un réservoir (51).
  18. L'appareil de fabrication de fibre de carbone selon l'une quelconque des revendications 12 à 17, comprenant en outre une module de séchage (60), le module de séchage (60) étant disposé sur la voie de traînée de la fibre de carbone, entre le module de dimensionnement (50) et le module de réception (20).
EP17000054.1A 2017-01-12 2017-01-12 Procédé de fabrication de fibre de carbone et appareil de fabrication de fibre de carbone Active EP3348684B1 (fr)

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