CN106521712A - Controllable laser type ultrahigh-temperature graphitization device for carbon fiber - Google Patents

Controllable laser type ultrahigh-temperature graphitization device for carbon fiber Download PDF

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Publication number
CN106521712A
CN106521712A CN201611125979.0A CN201611125979A CN106521712A CN 106521712 A CN106521712 A CN 106521712A CN 201611125979 A CN201611125979 A CN 201611125979A CN 106521712 A CN106521712 A CN 106521712A
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carbon fiber
heater
argon
laser
inlet
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CN201611125979.0A
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CN106521712B (en
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谭晶
黎三洋
丁玉梅
杨卫民
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof

Abstract

The invention discloses a controllable laser type ultrahigh-temperature graphitization device for carbon fiber. The device mainly comprises a fiber storage device, a sealing device, a furnace body, a controllable laser, an observing camera, a gas valve, a gas pipe, a miniature air extracting pump, a quartz glass window, an ultrahigh-temperature infrared thermometer, an argon purifier and a fiber collecting device, wherein an inlet seal and an outlet seal are arranged at a carbon fiber inlet and a carbon fiber outlet in the side wall of the furnace body, argon injection ports are formed in the inlet seal and the outlet seal, the carbon fiber penetrates through the inlet seal and the outlet seal, the furnace body is further provided with a gas outlet and an argon inlet, and the gas outlet is connected with the gas valve, the gas pipe and the miniature air extracting pump; the miniature air extracting pump is connected to the gas outlet of the furnace body through the gas pipe; laser heads of the controllable laser are fixed on the furnace body and used for performing ultrahigh-temperature heating on the carbon fiber; the ultrahigh-temperature infrared thermometer can measure the temperature of a heating point in real time through the quartz glass window and transmit data to a controller, and the controller controls the speed of the fiber storage and collecting devices and the power of the controllable laser in real time, so that dynamic balance of the temperature of a heating area is guaranteed.

Description

A kind of controllable laser type superhigh temperature graphitizing device of carbon fiber
Technical field
The present invention relates to a kind of controllable laser type superhigh temperature graphitizing device of carbon fiber, belongs to carbon fiber and graphiteization processing system Make field.
Background technology
High-performance carbon fibre (graphite fibre) is to carry out stone with 2000-3000 DEG C by carbon fiber under the protection of noble gases Inkization and it is obtained.In graphitizing process, carbon fiber can further remove 5% or so non-carbon element, while carbon atom enters The arrangement of row graphite-like structure, is changed from two-dimensional layer graphite-structure to ordered 3 D structure on microcosmic, crystalline size increase, is taken Increase to degree, so that the modulus of carbon fiber is improved.Carbon fiber not only has the intrinsic intrinsic property of material with carbon element, has spinning again concurrently The soft machinability of textured fiber, with high intensity, high-moduluss, excellent heat resistance, chemical stability, the swollen property of low grade fever, stone Black self lubricity, concussion Decay Rate, and fibre density is low, X-ray transmission is good, rub resistance, corrosion-resistant, resisting fatigue the advantages of it is wide It is general to apply in fields such as Aero-Space, auto industry, mechano-electronic industry, new forms of energy, infrastructure and leisure styles.Preparing In terms of high-performance carbon fibre, superhigh temperature graphitizing furnace and superhigh temperature heat treatment technics are crucial technological difficulties, fiber high-moduluss Characteristic derive from its graphite-like structure, numerous studies prove carbon fiber stretch moduluses carry with the rising of graphitization temperature Height, and the raising of degree of graphitization is realized by high-temperature heat treatment.
Main method in terms of commercial application is high-temperature tubular resistance indirectly heat graphitizing furnace and electromagnetism sense at present Indirectly heat graphitizing furnace technology is answered, in both graphitization mode of heatings, carbon fiber is passed through from the middle of graphite-pipe, in graphite Pipe two ends apply unidirectional current or make graphite-pipe produce unidirectional current by electromagnetic induction, the graphite when electric current passes through graphite heater Heater is heated as resistance, and thermal current is realized fine to carbon between graphite heater and carbon fiber by the form of heat transfer The indirectly heat of dimension.It need to be higher than carbon fiber temperature that the method shortcoming is furnace body temperature, and slowly, most of energy is dissipated diabatic process Send out, the thermal efficiency is low, power consumption is big, acts on the difficult control of temperature of carbon fiber;Cavity protection constraint graphite heater is needed, is led Cause cavity body structure complicated, cavity material is had high demands, graphitizing furnace is expensive;Heater hot soak condition, by residual The erosion of oxygen, short life, and burn out rear unrepairable.Meanwhile, started distillation at 2800 DEG C by graphite heater and limited, it is domestic Type graphitizing furnace is only capable of below 2500 DEG C normal operation, it is impossible to realize the stable high temperature of 2800 DEG C of even more high temperature, graphite Change degree is relatively low, it is impossible to realize the continuous controllable standby of high strength high modulus carbon fiber.
The content of the invention
Present invention aims to existing graphitizing furnace equipment energy consumption is big, expensive, short life, be difficult to The problems such as more than 2500 DEG C of superhigh temperature graphitization, so as to proposing a kind of low energy consumption, life-span length, low cost, carrying out to carbon fiber Apparatus and method prepared by superhigh temperature graphitization controllability.
Realize that above-mentioned purpose technical scheme is:A kind of controllable laser type superhigh temperature graphitizing device of carbon fiber, mainly includes Put silk device, sealing device, body of heater, controllable laser instrument, observation camera, air valve, trachea, micro-suction pump, quartz glass to regard Window, superhigh temperature infrared radiation thermometer, purification for argon machine and receipts silk device.Sealing device is located at sidewall of the furnace body carbon fiber gateway, Sealing device includes inlet seal and exit seal, and inlet seal and exit seal have argon inlet and carbon fiber to pass through, Exchange with the air-flow in the external world by the pressure blocking body of heater of argon, be in body of heater, to create oxygen-free environment, form strict in stove Inert gas shielding environment, body of heater has gas outlet and Ar inlet, gas outlet and Ar inlet, and at a distance of as far as possible, far, gas goes out Mouthful body of heater upper end is arranged near filament mouth, Ar inlet is arranged on body of heater lower end near entering silk mouth, gas outlet's connection air valve, Trachea, micro-suction pump, the argon in body of heater in the presence of micro-suction pump circulate, the argon that micro-suction pump is released Gas enters purification for argon machine, and the high purity argon after purification is again from the argon inlet and body of heater of inlet seal and exit seal Ar inlet injection body of heater;Carbon fiber is drawn by silk device and receipts silk device is put, and is moved with certain speed.Body of heater is placed Putting silk device and receiving between silk device;Micro-suction pump is connected to the gas outlet of body of heater by trachea, can enter stove in argon In advance to carrying out taking out in stove air and waste discharge gas disposal being carried out after argon reaches purity requirement before body;Controllable laser instrument Laser head is fixed on body of heater for superhigh temperature heating is carried out to carbon fiber, and the laser head of controllable laser instrument can be single or many Individual, the laser facula of laser head transmitting is irradiated on carbon fiber wire;Superhigh temperature infrared radiation thermometer is arranged on body of heater side, by stone English glass vision panel carries out thermometric;Observation camera is arranged in body of heater, can be to the laser facula heating process monitor in real time in stove And record.
The controllable laser type superhigh temperature graphitizing device of a kind of carbon fiber of the present invention, in order to realize carbon fiber superhigh temperature graphite Change, spy carries out high-temperature process to carbon fiber using the direct-fired mode of laser.This device can be according to the need of actual process condition Select suitable pulsed or continuous wave laser.For carbon fiber can be swashed using single or multiple laser heads Light is heated.In order to improve carbon fiber and graphite efficiency and graphitization uniformity coefficient, typically swashed using multiple laser heads simultaneously Light heat, carbon fibre tow circumferential position by multiple laser heads according to being angularly uniformly distributed, in carbon fibre tow Axial direction using equidistantly distributing make multiple laser simultaneously heating axial direction diverse location region or the axial direction in carbon fibre tow Many laser heads are arranged in axial same plane and heat the identical band of position simultaneously.Design according to said apparatus, positioned at axle The carbon fibre tow of core can be brought rapidly up to more than 2500 DEG C of temperature under the directly heating of laser beam, and when extremely short It is interior just to complete graphitizing process.When high-temperature process is carried out, can be adjusted by the watt level of control laser instrument The graphitization temperature of carbon fiber, makes temperature control in suitable scope.Can be by installing laser additional inside the laser head of this device Beam reshaper enters line translation to the light spot shape, size and the energy distribution of laser that export, so as to change Heating Zone Temperature field point Cloth enables carbon fiber to be efficiently completed graphitizing process under suitable temperature field.
A kind of controllable laser type superhigh temperature graphitizing device of carbon fiber of the present invention, carbon fiber is under the traction of folding and unfolding silk device Moved with certain speed, the graphitization time of carbon fiber is controlled by the speed of control folding and unfolding silk.Put silk device and receive silk Device can carry out some tension control to carbon fiber, make carbon fiber graphited while being taken in the presence of pull strength To and drawing-off, so as to improve carbon fiber and graphite degree.
The controllable laser type superhigh temperature graphitizing device of a kind of carbon fiber of the present invention, in order to ensure that carbon fiber can realize superelevation Warm graphitization, it is to avoid carbon fiber is oxidized in heating, and the heating region of carbon fiber is needed in high-purity inert gas shielding In carry out graphitization.This device using the ultrapure argon after purification for argon machine is cleaned as shielding gas, argon after purification The content of middle impurity is controlled in CH4≤0.1ppm, O2≤0.1ppm, N2≤0.2ppm, phosphorus content≤0.2ppm, and dew point≤ 0.2ppm, hydro carbons≤0.1ppm.In order to maintain inert gas shielding environment pure in stove, first using micro-suction pump in stove Pumping process is carried out, then ultrapure argon is input into in stove by copper pipe or steel pipe, purity of argon reaches technique in the stove After required standard, reduce the speed of evacuation of micro-suction pump, to ensure that argon steadily and slowly flows in stove, while Can be by outside waste gas timely grate furnace;In order that ultrapure argon environmental protection is maintained in stove, sealing device is installed at body of heater two ends, every Foreign gas extraneous absolutely is entered, and can be sealed using hermetic device or close using device for sealing magnetic fluid in this device Envelope.
A kind of controllable laser type superhigh temperature graphitizing device of carbon fiber of the present invention, superhigh temperature infrared radiation thermometer can pass through stone English glass vision panel measures hot spot temperature in real time, and transfers data to controller, controller real-time control folding and unfolding silk device The power of speed and controllable laser instrument, so as to the temperature for ensureing heating region keeps dynamic equilibrium.Observation camera is used for observing Graphitizing process in stove, while can be recorded to the phenomenon for observing with selectivity.
Description of the drawings
Fig. 1 is a kind of structural representation of the controllable laser type superhigh temperature graphitizing device of carbon fiber of the invention.
Fig. 2 is a kind of laser head arrangement schematic diagram of the controllable laser type superhigh temperature graphitizing device of carbon fiber of the invention.
In figure:1- puts silk device, and 2- enters a hole, and 3a inlet seals, 3b- exit seals, 4- bodies of heater, 5- laser heads, 6- are seen Video camera is surveyed, 7- ventholes, 8- air valves, 9- tracheas, 10- micro-suction pumps, 11- filament mouths, 12- receive silk device, 13- quartz glass Glass form, 14- superhigh temperature infrared radiation thermometers, 15- air inlets, 16- argon, 17- carbon fibers.
Specific embodiment
A kind of controllable laser type superhigh temperature method for graphitizing of carbon fiber of the present invention and device, as shown in figure 1, main include putting Silk device 1, sealing device, body of heater 4, controllable laser instrument, observation camera 6, air valve 8, trachea 9, micro-suction pump 10, quartzy glass Glass form 13, superhigh temperature infrared radiation thermometer 14, purification for argon machine and receipts silk device 12.Sealing device is located at sidewall of the furnace body carbon fiber At 17 gateways, sealing device includes inlet seal 3a and exit seal 3b, and inlet seal 3a and exit seal 3b have argon Inlet and carbon fiber 17 are passed through, and are exchanged with the air-flow in the external world by the pressure blocking body of heater of argon, are that anaerobic is created in body of heater Environment, forms strict inert gas shielding environment in stove, and body of heater has venthole 7 and argon inlet mouth 15, venthole 7 and argon At a distance of as far as possible, far, venthole 7 is arranged on body of heater upper end near filament mouth 11 to gas air inlet 15, and argon inlet mouth 15 is arranged on body of heater 4 lower ends connect air valve 8, trachea 9, micro-suction pump 10 near silk mouth 2, venthole 7 is entered, and the argon in body of heater 4 is in miniature pumping Circulation in the presence of pump 10 is got up, and the argon that micro-suction pump 10 is released enters purification for argon machine, the high-purity argon after purification The injection body of heater of argon inlet mouth 15 again from the argon inlet and body of heater 4 of inlet seal 3a and exit seal 3b of gas 16;Carbon Fiber 17 is drawn by silk device 1 and receipts silk device 12 is put, and is moved with certain speed.Body of heater is placed on silk device 1 and receives Between silk device 12;Micro-suction pump 10 is connected to the venthole 7 of body of heater 4 by trachea 9, can be before argon enters body of heater first Row is to carrying out taking out in stove air and waste discharge gas disposal being carried out after argon reaches purity requirement;The laser head 5 of controllable laser instrument Be fixed on body of heater for carrying out superhigh temperature heating to carbon fiber 17, the laser head 5 of controllable laser instrument can be it is single or multiple, The laser facula of the transmitting of laser head 5 is irradiated on carbon fiber wire 17;Superhigh temperature infrared radiation thermometer 14 is arranged on 4 side of body of heater, leads to Crossing quartz glass window 13 carries out thermometric;Observation camera 6 is arranged in body of heater 4, can be to the laser facula heating process in stove Monitor in real time is simultaneously recorded.
Micro-suction pump 10 carries out fast pump to body of heater 5 at the beginning of argon is passed through first, and the argon 16 through purifying leads to Air inlet 15 is crossed in body of heater 4, body of heater 4 is then full of at leisure, micro-suction pump 10 passes through gas outlet 7 by the gas in stove Body of heater 4 is extracted out constantly, the pumping speed of adjusting air valve 8 and reduction micro-suction pump 10 when argon reaches technological requirement in stove Degree, so that furnace gas is gently stable, makes argon reach dynamic equilibrium.Power is selected in this example for 180w, continuouss CO2Swash Optical generator is used for carrying out LASER HEATING, and after argon reaches technological requirement, laser head 5 sends superlaser and carbon fiber is carried out Heating, while superhigh temperature infrared radiation thermometer 14 starts to carry out heating region thermometric and control, observation camera 6 can be to the thermal treatment zone Domain is observed and records, and carbon fiber 17 just completes graphitizing process after exit seal 3b.
A kind of controllable laser type superhigh temperature graphitizing device of carbon fiber of the present invention, multiple laser heads 5 arrangement such as Fig. 2, In Fig. 2, laser head 5 has three, and three laser heads 5 are circumferentially uniformly distributed in carbon fiber 17.Axially can arranged using two kinds Mode, the first is that multiple laser heads 5 are in same plane, and now many laser heads 5 heat a region simultaneously, second It is, by corresponding range distribution, now can to heat zones of different simultaneously in axially distinct plane.Many laser heads 5 are heated simultaneously, The efficiency of heating surface can be improved, it is also possible to which the carbon fiber and graphiteization for allowing to carry out heating is more uniform.Can inside the laser head 5 of this device To enter line translation by installing light spot shape, size and energy distribution of laser of the laser beam reshaping device to exporting additional, so as to change Heating Zone Temperature field distribution enables carbon fiber to be efficiently completed graphitizing process under suitable temperature field.

Claims (6)

1. the controllable laser type superhigh temperature graphitizing device of a kind of carbon fiber, it is characterised in that:It is main to include putting silk device, sealing dress Put, body of heater, controllable laser instrument, observation camera, air valve, trachea, micro-suction pump, quartz glass window, the infrared survey of superhigh temperature Wen Yi, purification for argon machine and receipts silk device, sidewall of the furnace body carbon fiber have sealing device at gateway, and sealing device includes entrance Sealing and exit seal, inlet seal and exit seal have argon inlet and carbon fiber to pass through, by the pressure blocking of argon Body of heater is exchanged with the air-flow in the external world, is that oxygen-free environment is created in body of heater, strict inert gas shielding environment, stove are formed in stove Body also has gas outlet and Ar inlet, and gas outlet is arranged on body of heater upper end near filament mouth, and Ar inlet is arranged on body of heater Lower end connects air valve, trachea, micro-suction pump, work of the argon in body of heater in micro-suction pump near silk mouth, gas outlet is entered Got up with lower circulation, the argon that micro-suction pump is released enters purification for argon machine, and the high purity argon after purification is again from entrance Ar inlet injection body of heater on the argon inlet and body of heater of sealing and exit seal;Carbon fiber is filled by silk device and receipts silk is put Traction is put, and is moved with certain speed;Body of heater is placed on silk device and receives between silk device;Micro-suction pump is connected by trachea Be connected at the gas outlet of body of heater, can argon into before body of heater in advance to stove in carry out taking out air and reach purity in argon will Waste discharge gas disposal is carried out after asking;The laser head of controllable laser instrument is fixed on body of heater and adds for carrying out superhigh temperature to carbon fiber Heat, the laser facula of laser head transmitting are irradiated on carbon fiber wire;Superhigh temperature infrared radiation thermometer is arranged on body of heater side, by stone English glass vision panel carries out thermometric;Observation camera is arranged in body of heater, to the laser facula heating process monitor in real time in stove simultaneously Record.
2. the controllable laser type superhigh temperature graphitizing device of a kind of carbon fiber according to claim 1, it is characterised in that:It is controllable The laser head of laser instrument is single or multiple.
3. the controllable laser type superhigh temperature graphitizing device of a kind of carbon fiber according to claim 2, it is characterised in that:It is multiple Laser head is according to angularly carrying out being evenly distributed on the circumferential position of carbon fibre tow.
4. the controllable laser type superhigh temperature graphitizing device of a kind of carbon fiber according to claim 2, it is characterised in that:It is multiple The laser head of controllable laser instrument adopts to equidistantly distribute in the axial direction of carbon fibre tow makes multiple laser while heating axially distinct Identical position is heated simultaneously in being axially arranged on many laser heads in axial same plane for carbon fibre tow in the band of position Put region.
5. the controllable laser type superhigh temperature graphitizing device of a kind of carbon fiber according to claim 1, it is characterised in that:Put silk Device and receipts silk device carry out some tension control to carbon fiber, make carbon fiber graphited while in the presence of pull strength It is orientated and drawing-off.
6. the controllable laser type superhigh temperature graphitizing device of a kind of carbon fiber according to claim 1, it is characterised in that:Entrance Sealing and exit seal are sealed using device for sealing magnetic fluid.
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Cited By (9)

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CN107761193A (en) * 2017-09-21 2018-03-06 北京化工大学 One kind can the efficient preparation facilities of gradual change integrating laser carbonization stove and method
CN107973284A (en) * 2017-11-07 2018-05-01 西安交通大学 A kind of preparation method of the nanoporous carbon materials based on Gao Zhongying laser graphite
CN108560243A (en) * 2018-05-12 2018-09-21 中国科学院山西煤炭化学研究所 A kind of method of surface treatment of carbon fibers and application
CN110042583A (en) * 2019-04-27 2019-07-23 北京化工大学 A kind of carbon fiber laser graphite device for sizing and method
CN110257960A (en) * 2019-07-15 2019-09-20 中国科学院合肥物质科学研究院 A kind of microwave heating cavity for carbon fiber and graphite
CN110524905A (en) * 2019-08-21 2019-12-03 大同新成新材料股份有限公司 A kind of carbon carbon composite mould pressing method
CN114351291A (en) * 2022-01-19 2022-04-15 苏州光兴智能科技有限公司 Special fiber laser tunnel preparation method and device
CN114672900A (en) * 2022-04-28 2022-06-28 南通普朗克石墨烯科技有限公司 Preparation method of carbon fiber with high graphitization degree
CN114892388A (en) * 2022-06-08 2022-08-12 途格科技(广东)有限公司 Carbon fiber laser graphitization tunnel preparation method and device

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CN104294407A (en) * 2014-10-15 2015-01-21 北京化工大学 Shaft core focused carbon fiber graphitization furnace through laser tunnel reflection method
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CN2605544Y (en) * 2003-02-21 2004-03-03 司书珂 Bell type inert gas-shielded fritting furnace
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CN107761193A (en) * 2017-09-21 2018-03-06 北京化工大学 One kind can the efficient preparation facilities of gradual change integrating laser carbonization stove and method
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CN110257960A (en) * 2019-07-15 2019-09-20 中国科学院合肥物质科学研究院 A kind of microwave heating cavity for carbon fiber and graphite
CN110524905A (en) * 2019-08-21 2019-12-03 大同新成新材料股份有限公司 A kind of carbon carbon composite mould pressing method
CN114351291A (en) * 2022-01-19 2022-04-15 苏州光兴智能科技有限公司 Special fiber laser tunnel preparation method and device
CN114672900A (en) * 2022-04-28 2022-06-28 南通普朗克石墨烯科技有限公司 Preparation method of carbon fiber with high graphitization degree
CN114892388A (en) * 2022-06-08 2022-08-12 途格科技(广东)有限公司 Carbon fiber laser graphitization tunnel preparation method and device

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