CN106521712B - A kind of controllable laser type superhigh temperature graphitizing device of carbon fiber - Google Patents
A kind of controllable laser type superhigh temperature graphitizing device of carbon fiber Download PDFInfo
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- CN106521712B CN106521712B CN201611125979.0A CN201611125979A CN106521712B CN 106521712 B CN106521712 B CN 106521712B CN 201611125979 A CN201611125979 A CN 201611125979A CN 106521712 B CN106521712 B CN 106521712B
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- carbon fiber
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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
Abstract
The invention discloses a kind of controllable laser type superhigh temperature graphitizing devices of carbon fiber, main includes putting silk device, sealing device, furnace body, controllable laser, observation camera, air valve, tracheae, micro-suction pump, quartz glass window, superhigh temperature infrared radiation thermometer, purification for argon machine and receiving silk device, there are inlet seal and exit seal at sidewall of the furnace body carbon fiber entrance, inlet seal and exit seal have argon gas inlet and carbon fiber to pass through, there are also gas vent and Ar inlet, gas vents to connect air valve, tracheae, micro-suction pump for furnace body；Micro-suction pump is connected to the gas outlet of furnace body by tracheae；The laser head of controllable laser, which is fixed on, to be used to carry out superhigh temperature heating to carbon fiber on furnace body；Superhigh temperature infrared radiation thermometer can be by quartz glass window real-time measurement hot spot temperature, and transfers data to controller, the speed of controller real-time control folding and unfolding silk device and the power of controllable laser, to guarantee that the temperature of heating region keeps dynamic equilibrium.
Description
Technical field
The present invention relates to a kind of controllable laser type superhigh temperature graphitizing devices of carbon fiber, belong to carbon fiber and graphiteization processing system
Make field.
Background technique
High-performance carbon fibre (graphite fibre) be by carbon fiber under the protection of inert gas with 2000-3000 DEG C of progress stone
Prepared by inkization.In graphitizing process, carbon fiber can further remove 5% or so non-carbon element, at the same carbon atom into
The arrangement of row graphite-like structure is changed on microcosmic from two-dimensional layer graphite-structure to ordered 3 D structure, and crystalline size increases, and is taken
Increase to degree, so that the modulus of carbon fiber improves.Carbon fiber not only has the intrinsic intrinsic property of carbon material, and has both spinning
The soft machinability of textured fiber has high intensity, high-modulus, excellent heat resistance, chemical stability, the swollen property of low-heat, stone
Black self-lubrication, concussion Decay Rate, and fibre density is low, X-ray transmission is good, rub resistance, it is corrosion-resistant, antifatigue the advantages that it is wide
It is general to apply in fields such as aerospace, auto industry, mechano-electronic industry, new energy, infrastructure and leisure styles.It is preparing
In terms of high-performance carbon fibre, superhigh temperature graphitizing furnace and superhigh temperature heat treatment technics are crucial technological difficulties, fiber high-modulus
Characteristic derive from its graphite-like structure, numerous studies prove carbon fiber stretch modulus mentioned with the raising of graphitization temperature
Height, and the raising of degree of graphitization is realized by high-temperature heat treatment.
The main method in terms of industrial application is high-temperature tubular resistance indirect heating graphitizing furnace and electromagnetism sense at present
Indirect heating graphitizing furnace technology is answered, in both graphitization heating methods, carbon fiber passes through among graphite-pipe, in graphite
Pipe both ends apply direct current or so that graphite-pipe is generated direct current, the graphite when electric current passes through graphite heater by electromagnetic induction
Heater is heated as resistance, and the form that thermal current leads to heat transfer between graphite heater and carbon fiber is realized to carbon fiber
The indirect heating of dimension.The method disadvantage is that furnace body temperature need to be higher than carbon fiber temperature, and diabatic process is slow, and most of energy is dissipated
Hair falls, and the thermal efficiency is low, and energy consumption is big, and the temperature for acting on carbon fiber is difficult to control；Cavity protection constraint graphite heater is needed, is led
It causes cavity body structure complicated, height is required to cavity material, graphitizing furnace is expensive；Heater hot soak condition, by residual
The erosion of oxygen, the service life is short, and burns out rear unrepairable.Meanwhile being started distillation at 2800 DEG C by graphite heater and being limited, it is domestic
Type graphitizing furnace is only capable of operating normally at 2500 DEG C or less, cannot achieve the stabilization high temperature of 2800 DEG C of even higher temperature, graphite
Change degree is lower, cannot achieve the continuous controllable preparation of high strength high modulus carbon fiber.
Summary of the invention
It is an object of the invention to for existing graphitizing furnace equipment energy consumption is big, expensive, the service life is short, is difficult to realize
The problems such as 2500 DEG C or more of superhigh temperature graphitization, thus propose it is a kind of low energy consumption, the service life is long, it is at low cost, to carbon fiber progress
The device and method that superhigh temperature is graphitized controllability preparation.
Realizing above-mentioned purpose technical solution is: a kind of controllable laser type superhigh temperature graphitizing device of carbon fiber mainly includes
Put silk device, sealing device, furnace body, controllable laser, observation camera, air valve, tracheae, micro-suction pump, quartz glass view
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 entrance,
Sealing device includes inlet seal and exit seal, and inlet seal and exit seal have argon gas inlet and carbon fiber to pass through,
It is exchanged by the pressure blocking furnace body of argon gas with the air-flow in the external world, is to create oxygen-free environment in furnace body, is formed strictly in furnace
Inert gas shielding environment, furnace body have gas vent and Ar inlet, and at a distance of as far as possible far, gas goes out for gas vent and Ar inlet
Mouthful setting in furnace body upper end close to filament mouth, Ar inlet setting in furnace body lower end close into silk mouth, gas vent connect air valve,
Tracheae, micro-suction pump, the intracorporal argon gas of furnace recycle under the action of micro-suction pump, the argon that micro-suction pump is released
Gas enters purification for argon machine, and purified high purity argon is again from the argon gas inlet and furnace body of inlet seal and exit seal
Ar inlet inject furnace body；Carbon fiber is drawn by putting silk device and receiving silk device, and mobile with certain speed.Furnace body is placed
It is putting silk device and is receiving between silk device；Micro-suction pump is connected to the gas outlet of furnace body by tracheae, can enter furnace in argon gas
In advance to carrying out taking out air in furnace and carry out waste discharge gas disposal after argon gas reaches purity requirement before body；Controllable laser
Laser head, which is fixed on furnace body, is used to carry out carbon fiber superhigh temperature heating, and the laser head of controllable laser can be single or more
A, the laser facula of laser head transmitting is irradiated on carbon fiber wire；Superhigh temperature infrared radiation thermometer is mounted on furnace body side, passes through stone
English glass vision panel carries out thermometric；Observation camera is mounted in furnace body, can be monitored in real time to the laser facula heating process in furnace
And it records.
A kind of controllable laser type superhigh temperature graphitizing device 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.The present apparatus can be according to the need of actual process condition
Select suitable pulsed or continuous wave laser.Single or multiple laser heads can be used to swash on carbon fiber
Light heating.In order to improve carbon fiber and graphite efficiency and graphitization uniformity coefficient, generally swashed simultaneously using multiple laser heads
Light heating, carbon fibre tow circumferential position by multiple laser heads according to being angularly uniformly distributed, in carbon fibre tow
Axial make multiple laser while heating axial different location region or the axial direction in carbon fibre tow using equidistantly distributing
More laser heads are mounted in axial same plane while heating the identical band of position.It is designed according to above-mentioned apparatus, is located at axis
The carbon fibre tow of core can be brought rapidly up under the directly heating of laser beam to 2500 DEG C or more of temperature, and when extremely short
It is interior to complete graphitizing process.When carrying out high-temperature process, can be adjusted by controlling the watt level of laser
The graphitization temperature of carbon fiber makes temperature control in suitable range.It can be by installing laser additional inside the laser head of the present apparatus
Beam reshaper converts the light spot shape of output, size and energy distribution of laser, 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
It is mobile with certain speed, the graphitization time of carbon fiber is controlled by controlling the speed of folding and unfolding silk.It puts silk device and receives silk
Device can carry out some tension control to carbon fiber, make carbon fiber graphited while being taken under the action of tractive force
To and drawing-off, to improve carbon fiber and graphite degree.
A kind of controllable laser type superhigh temperature graphitizing device of carbon fiber of the present invention, in order to guarantee that carbon fiber can be realized superelevation
Temperature graphitization, avoids carbon fiber from being oxidized when heated, and the heating region of carbon fiber is needed in high-purity inert gas shielding
In be graphitized.The present apparatus is used as protection gas, argon gas after purification using the ultrapure argon after purification for argon machine is cleaned
The content control of middle impurity is 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 furnace, first using micro-suction pump in furnace
Pumping process is carried out, then ultrapure argon is inputted by copper pipe or steel pipe into furnace, until purity of argon reaches technique in furnace
After required standard, reduce the speed of evacuation of micro-suction pump, to guarantee that argon gas is steady and slowly flows in furnace, while
It can will be outside the timely grate furnace of exhaust gas；In order to make in furnace maintain ultrapure argon protection environment, sealing device is installed at furnace body both ends, every
Extraneous foreign gas enters absolutely, can be sealed using hermetic device in the present apparatus or close using device for sealing magnetic fluid
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 real-time measurement hot spot temperature, and controller is transferred data to, controller real-time control folding and unfolding silk device
The power of speed and controllable laser, to guarantee that the temperature of heating region keeps dynamic equilibrium.Observation camera is used to observe
Graphitizing process in furnace, while the property of can choose is recorded to the phenomenon that observing.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the controllable laser type superhigh temperature graphitizing device of carbon fiber of the present 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 present invention.
In figure: 1- puts silk device, and 2- is seen into wire hole, 3a inlet seal, 3b- exit seal, 4- furnace body, 5- laser head, 6-
Survey video camera, 7- venthole, 8- air valve, 9- tracheae, 10- micro-suction pump, 11- filament mouth, 12- receipts silk device, 13- quartz glass
Glass form, 14- superhigh temperature infrared radiation thermometer, 15- air inlet, 16- argon gas, 17- carbon fiber.
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 includes putting
Silk device 1, sealing device, furnace body 4, controllable laser, observation camera 6, air valve 8, tracheae 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 entrances, sealing device includes inlet seal 3a and exit seal 3b, and inlet seal 3a and exit seal 3b have argon gas
Inlet and carbon fiber 17 pass through, and exchange by the pressure blocking furnace body of argon gas with extraneous air-flow, are that anaerobic is created in furnace body
Environment, forms stringent inert gas shielding environment in furnace, and furnace body has venthole 7 and argon inlet mouth 15, venthole 7 and argon
Gas air inlet 15 is at a distance of as far as possible far, and in furnace body upper end close to filament mouth 11, argon inlet mouth 15 is arranged in furnace body the setting of venthole 7
4 lower ends are close into silk mouth 2, and venthole 7 connects air valve 8, tracheae 9, micro-suction pump 10, and the argon gas in furnace body 4 is in miniature pumping
Circulation is got up under the action of pump 10, and the argon gas that micro-suction pump 10 is released enters purification for argon machine, purified high-purity argon
Gas 16 injects furnace body from the argon inlet mouth 15 on the argon gas inlet and furnace body 4 of inlet seal 3a and exit seal 3b again；Carbon
Fiber 17 is drawn by putting silk device 1 and receiving silk device 12, and mobile with certain speed.Furnace body is placed on silk device 1 and receives
Between silk device 12；Micro-suction pump 10 is connected to the venthole 7 of furnace body 4 by tracheae 9, can be before argon gas enters furnace body first
Row to carried out in furnace take out air and after argon gas reaches purity requirement carry out waste discharge gas disposal；The laser head 5 of controllable laser
Be fixed on furnace body and be used to carry out carbon fiber 17 superhigh temperature heating, the laser head 5 of controllable laser can be it is single or multiple,
The laser facula that laser head 5 emits is irradiated on carbon fiber wire 17；Superhigh temperature infrared radiation thermometer 14 is mounted on 4 side of furnace body, leads to
It crosses quartz glass window 13 and carries out thermometric；Observation camera 6 is mounted in furnace body 4, can be to the laser facula heating process in furnace
It monitors in real time and records.
Micro-suction pump 10 carries out fast pump to furnace body 5 first at the beginning of being passed through argon gas, and the argon gas 16 by purification is logical
It crosses air inlet 15 to enter in furnace body 4, is then full of furnace body 4 at leisure, micro-suction pump 10 passes through gas outlet 7 for the gas in furnace
Furnace body 4 is constantly extracted out, when argon gas reaches the pumping speed of adjusting air valve 8 and reduction micro-suction pump 10 when technique requires in furnace
Degree, so that furnace gas be made gently to stablize, makes argon gas reach dynamic equilibrium.It is 180w, continuous type CO that power is selected in this example2Swash
Optical generator is used to carry out laser heating, issues superlaser to carbon fiber progress when argon gas reaches laser head 5 after technique requires
Heating, while superhigh temperature infrared radiation thermometer 14 starts to carry out thermometric to heating region and control, observation camera 6 can be to heating zones
Domain is observed and records, and carbon fiber 17 just completes graphitizing process after passing through exit seal 3b.
A kind of controllable laser type superhigh temperature graphitizing device of carbon fiber of the present invention, multiple 5 arragement construction of laser head such as Fig. 2,
In Fig. 2 there are three laser heads 5, three laser heads 5 are circumferential at being uniformly distributed in carbon fiber 17.It can be arranged using two kinds axial
Mode, the first is that multiple laser heads 5 are in same plane, at this time one region of more laser heads 5 while heating, second
It is in axially distinct plane by corresponding range distribution, different zones can be heated simultaneously at this time.More laser heads 5 heat simultaneously,
Heating efficiency can be improved, it is also possible that the carbon fiber and graphiteization heated is more uniform.It can inside the laser head 5 of the present apparatus
To be converted by installing laser beam reshaping device additional to the light spot shape of output, size and energy distribution of laser, to change
Heating Zone Temperature field distribution enables carbon fiber to be efficiently completed graphitizing process under suitable temperature field.
Claims (3)
1. a kind of controllable laser type superhigh temperature graphitizing device of carbon fiber, it is characterised in that: main includes putting silk device, sealing dress
It sets, furnace body, controllable laser, observation camera, air valve, tracheae, micro-suction pump, quartz glass window, the infrared survey of superhigh temperature
Wen Yi, purification for argon machine and silk device is received, has sealing device at sidewall of the furnace body carbon fiber entrance, sealing device includes entrance
Sealing and exit seal, inlet seal and exit seal have argon gas inlet and carbon fiber to pass through, by the pressure blocking of argon gas
Furnace body is exchanged with extraneous air-flow, is to create oxygen-free environment in furnace body, is formed stringent inert gas shielding environment, furnace in furnace
Body is there are also gas vent and Ar inlet, and in furnace body upper end close to filament mouth, Ar inlet is arranged in furnace body for gas vent setting
Close into silk mouth, gas vent connects air valve, tracheae, micro-suction pump, work of the intracorporal argon gas of furnace in micro-suction pump for lower end
Got up with lower circulation, the argon gas that micro-suction pump is released enters purification for argon machine, and purified high purity argon is again from entrance
Ar inlet on the argon gas inlet and furnace body of sealing and exit seal injects furnace body；Carbon fiber is by putting silk device and receiving silk dress
Traction is set, and mobile with certain speed；Furnace body is placed on silk device and receives between silk device；Micro-suction pump is connected by tracheae
It connects at the gas outlet of furnace body, it can be before argon gas enters furnace body in advance to carrying out taking out air in furnace and reach purity in argon gas and want
Waste discharge gas disposal is carried out after asking；The laser head of controllable laser, which is fixed on furnace body, to be used to carry out superhigh temperature to carbon fiber to add
The laser facula of heat, laser head transmitting is irradiated on carbon fiber wire；Superhigh temperature infrared radiation thermometer is mounted on furnace body side, passes through stone
English glass vision panel carries out thermometric to hot spot；Observation camera is mounted in furnace body, real to the laser facula heating process in furnace
When monitor and record；The laser head of controllable laser is multiple；Multiple laser heads are according to angularly carrying out being evenly distributed on carbon fiber
Tie up the circumferential position of tow；Or the laser head of multiple controllable lasers carbon fibre tow it is axial using equidistantly distribute make it is more
Shu Jiguang heats axial different location region or axial same in being axially mounted on more laser heads of carbon fibre tow simultaneously
The identical band of position is heated in plane simultaneously.
2. 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
It device and receives silk device some tension control is carried out to carbon fiber, make carbon fiber graphited while under the action of tractive force
Carry out orientation and drawing-off.
3. 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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Families Citing this family (9)
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| CN107761193B (en) * | 2017-09-21 | 2023-06-27 | 北京化工大学 | Efficient preparation device and method for gradual-change laser carbonization furnace |
| CN107973284B (en) * | 2017-11-07 | 2020-09-08 | 西安交通大学 | Preparation method of nano porous carbon material based on high repetition frequency laser graphitization |
| CN108560243B (en) * | 2018-05-12 | 2020-12-25 | 中国科学院山西煤炭化学研究所 | Carbon fiber surface treatment method and application |
| CN110042583B (en) * | 2019-04-27 | 2023-06-30 | 北京化工大学 | Carbon fiber laser graphitization sizing equipment 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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| JP2002013031A (en) * | 2000-06-28 | 2002-01-18 | Nippon Steel Corp | Method for graphitizing carbon material and apparatus therefor |
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| CN2605544Y (en) * | 2003-02-21 | 2004-03-03 | 司书珂 | Bell type inert gas-shielded fritting furnace |
| US7824495B1 (en) * | 2005-11-09 | 2010-11-02 | Ut-Battelle, Llc | System to continuously produce carbon fiber via microwave assisted plasma processing |
| CN102644132B (en) * | 2012-04-25 | 2015-04-08 | 上海联川自动化科技有限公司 | High-temperature carbide furnace for manufacturing carbon fiber by charging gas after vacuum pumping |
| 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 |
| CN206385288U (en) * | 2016-12-09 | 2017-08-08 | 北京化工大学 | A kind of controllable laser type superhigh temperature graphitizing device of carbon fiber |
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| JP2002013031A (en) * | 2000-06-28 | 2002-01-18 | Nippon Steel Corp | Method for graphitizing carbon material and apparatus therefor |
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