CN102168324B - Carbonization device for electrostatically spinning nanometer tows and preparation method of carbon nanofibers - Google Patents
Carbonization device for electrostatically spinning nanometer tows and preparation method of carbon nanofibers Download PDFInfo
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- CN102168324B CN102168324B CN2011100544204A CN201110054420A CN102168324B CN 102168324 B CN102168324 B CN 102168324B CN 2011100544204 A CN2011100544204 A CN 2011100544204A CN 201110054420 A CN201110054420 A CN 201110054420A CN 102168324 B CN102168324 B CN 102168324B
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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
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- 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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
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Abstract
The invention discloses a carbonization device for electrostatically spinning nanometer tows. The periphery of a corundum tube is provided with a silicon carbide spiral tube heating element; the temperature of an atmosphere cavity formed in the corundum tube is controlled by an operation panel; two ends of the corundum tube are respectively and fixedly connected with an inlet stainless steel flange and an outlet stainless steel flange; the surface of the inlet stainless steel flange is embedded with an air inlet and a tow inlet; when in pre-oxidation, the air inlet is connected with an air cylinder through an inlet air-guide tube; when in carbonization, the air inlet is connected with a nitrogen cylinder; corresponding to the two inlet, an inlet guide pulley and an inlet clamping mechanism are arranged in sequence; the surface of the outlet stainless steel flange is embedded with an air outlet and a tow outlet; the air outlet is connected with an outlet air-guide tube; the other end of the outlet air-guide tube is led into a water tank; and corresponding to the tow outlet, an outlet guide pulley and a tension adjusting mechanism are arranged in sequence. By the processes of setting the temperature of pre-oxidation, the final temperature of pre-oxidation and short-time constant temperature stage, and the temperature of carbonization, carbon nanofibers can be prepared.
Description
Technical field
The invention belongs to the high temperature thermal treatment technical field, relate to a kind of carbonizing plant, be specifically related to the carbonizing plant that a kind of static spins the nanometer tow, the invention still further relates to and utilize this device to prepare the method for carbon nano-fiber.
Background technology
Along with CNT in the development of discovery in 1991 and nanometer technology in fiber art, carbon nano-fiber has caused more and more researchers' attention gradually.Because high length-diameter ratio, high-specific surface area, heat-resisting quantity and good performances such as electricity/thermal conductivity that carbon nano-fiber had; Carbon nano-fiber can be widely used in multiple field, comprises that supporting material, nanotube prepare template, high temperature filtration, high-temperature catalytic matrix material and super capacitor etc.Traditional method for preparing carbon nano-fiber comprises matrix method, spray process, vapor growth method and plasma enhanced chemical vapor deposition method etc., and these method relative complex and cost are higher.Therefore, in the past 10 years, a kind of simple and relatively inexpensive static spinning process just progressively is considered to prepare the optimised process of continuous carbon nano-fiber.
Because higher carbonization yield and simple relatively carbonization technique, commercial polypropylene nitrile (PAN) base carbon fibre accounts for 90% of the whole carbon fiber output in the world.Therefore, the researcher utilizes PAN/ dimethyl formamide (DMF) solution mostly, is equipped with carbon nano-fiber through electro-spinning.In addition, also see in document other precursor (such as pitch, polyimides, polyvinyl alcohol and polybenzimidazoles etc.) report is arranged by base nano carbon fibre.
When the nanometer tow that utilizes static to spin acquisition prepares carbon nano-fiber as precursor, must be in pre-oxidation and carbonisation fiber be applied tension force to prevent the contraction of macromolecular disorientation and controlling fiber in the high-temperature process.And, need feed hot-air during pre-oxidation and react required oxygen and take away reaction heat, and can take away byproduct of reaction so that pre-oxidation to be provided, promote the carrying out of pre-oxidation reaction.In the carbonisation, for fear of oxidation, carbonization need be carried out in inert atmosphere (such as nitrogen or helium) or vacuum.And traditional high temperature process furnances is not taken all factors into consideration these three aspects.
Summary of the invention
The purpose of this invention is to provide the carbonizing plant that a kind of static spins the nanometer tow; Be provided with special mobile hot-air and nitrogen device for supplying and Necessary Tensility applying mechanism; Solved when adopting traditional high temperature process furnances to prepare carbon nano-fiber the problem of pre-oxidation and carbonization poor effect.
Another object of the present invention provides the method for utilizing said apparatus to prepare carbon nano-fiber.
The technical scheme that the present invention adopted is; Static spins the carbonizing plant of nanometer tow; Comprise alundum tube, the outer periphery of alundum tube is equipped with carborundum helix tube heating element heater, and carborundum helix tube heating element heater is wrapped in the glass wool; The temperature in the atmosphere chamber that forms in the alundum tube is controlled by guidance panel; The two ends of alundum tube are fixedly connected with the outlet steel flange with the import steel flange respectively, and import steel flange surface studs with suction nozzle and tow import mouth, and suction nozzle is connected with air bottle through the import wireway when pre-oxidation; Suction nozzle is connected with nitrogen cylinder and corresponding inlet guide pulley and the inlet clamping body of being disposed with of tow import mouth through the import wireway when carbonization; Outlet steel flange surface studs with outlet nozzle and tow outlet mouth, and outlet nozzle is connected with the outlet wireway, and the other end of outlet wireway imports in the tank and tow outlet mouth correspondence is disposed with export orientation pulley and governing mechanism of tension.
Another technical scheme that the present invention adopted is; The method for preparing carbon nano-fiber adopts static to spin the carbonizing plant of nanometer tow, and the structure of this device is: comprise alundum tube; The outer periphery of alundum tube is equipped with carborundum helix tube heating element heater; Carborundum helix tube heating element heater is wrapped in the glass wool, and the temperature in the atmosphere chamber that forms in the alundum tube is controlled by guidance panel, and the two ends of alundum tube are fixedly connected with the outlet steel flange with the import steel flange respectively; Import steel flange surface studs with suction nozzle and tow import mouth; Suction nozzle is connected with air bottle through the import wireway when pre-oxidation, and suction nozzle is connected with nitrogen cylinder and corresponding inlet guide pulley and the inlet clamping body of being disposed with of tow import mouth through the import wireway when carbonization; Outlet steel flange surface studs with outlet nozzle and tow outlet mouth, and outlet nozzle is connected with the outlet wireway, and the other end of outlet wireway imports in the tank and tow outlet mouth correspondence is disposed with export orientation pulley and governing mechanism of tension.
Specifically implement according to following steps:
Step 1: adopt conventional static spinning method to prepare the nanometer tow;
Step 2: nanometer tow one end that step 1 obtains is fixed through the inlet clamping body; Through inlet guide pulley and tow import mouth; Through the atmosphere chamber in the alundum tube; Through tow outlet mouth and export orientation pulley, finally be connected with governing mechanism of tension at the other end, applying tension force through the governing mechanism of tension setting is 0.04～0.26 cN/dtex; Simultaneously, heating schedule is set, comprises pre-oxidation temperature programming, pre-oxidation final temperature short time constant temperature zone program and carbonation reaction temperature program through control panel;
Step 3: air bottle is connected with suction nozzle through the import wireway; Open the air bottle valve; Open carborundum helix tube heating element heater, the pre-oxidation temperature programming of setting according to step 2 carries out the pre-oxidation reaction, after reaction finishes; Close the air bottle valve, air bottle and import wireway are broken away from;
Step 4: nitrogen cylinder is connected with suction nozzle through the import wireway; Open the nitrogen cylinder valve; Add tension range at 0.005～0.12 cN/dtex through the governing mechanism of tension adjusting; Pre-oxidation final temperature short time constant temperature zone program according to step 2 is set is carried out isothermal reaction, and the carbonation reaction temperature program of setting according to step 2 is then carried out carburizing reagent, prepares carbon nano-fiber.
Characteristics of the present invention also are,
Governing mechanism of tension wherein is provided with scale.
Pre-oxidation temperature programming wherein, temperature is raised to 300 ° of C from room temperature, and programming rate is 0.2～2 ° of C/min.
Pre-oxidation final temperature short time constant temperature zone program wherein, temperature is 280～300 ° of C, the retention time is 3～20min.
Carbonation reaction temperature program wherein, temperature is raised to 1600 ° of C from 280 ° of C, and programming rate is 5～35 ° of C/min.
The preparation method of preparatory carbonizing plant of the present invention and carbon nano-fiber has following advantage:
(1) temperature control system adopts temperature programmed control, can carry out temperature programmed control to the nanofiber precursor, is beneficial to different ceiling temperatures of research and programming rate condition to the carbon nano-fiber Effect on Performance.
(2) special mobile hot-air and import and export of nitrogen are set; Be beneficial to the preparatory oxygen silk of nanofiber in high-temperature process effective protection and discharge the waste gas in the course of reaction; The gas outlet is connected with tank through wireway; Can effectively remove waste gas such as hydrogen cyanide first, second can reduce the air consumption of high purity nitrogen.
(3) special governing mechanism of tension is set, is beneficial in pre-oxidation and carbonisation fiber is applied Necessary Tensility, prevent the contraction of macromolecular disorientation and controlling fiber in the high-temperature process.
It is heating element heater that the furnace body of carbonizing plant adopts the carborundum helix tube, has that durable temperature is high, programming rate is fast and advantage such as long service life.Place alundum tube in the boiler tube as the atmosphere chamber, the alundum tube two ends have steel flange, turnover valve and yarn turnover mouth respectively.Temperature control system can temperature programmed control, is beneficial to the nanofiber precursor and carries out segmentation heat treatment.Tensioner by the inlet clamping body, import and export leading block, governing mechanism of tension, scale and heat resisting steel guide rod etc. and form, the fixing and expansion and contraction of stove of wearing that is used to accomplish precursor is measured.Tension force pre-oxidation response procedures, pre-oxidation final temperature short time constant temperature zone and tension force carburizing reagent program that the present invention is provided with; Can make fiber under the situation that heat endurance improves constantly, make fiber reach desired pre-oxidation degree; And make side reactions such as cracking be controlled at bottom line; And two phasic properties that skin-core structure brings to carbon fiber structural have effectively been prevented; When pre-oxidation tension force that the stage executes can guarantee to suppress the fibrous physics contraction, provide cyclization required chemical shrinkage amount.Simultaneously, tension force that carbonation stage is executed can keep and improve the orientation texture of pre-oxidation stage foundation.
Description of drawings
Fig. 1 is the structural representation that static of the present invention spins the carbonizing plant of nanometer tow.
Among the figure, clamping body, 2. nanometer tow, 3. inlet guide pulley, 4. tow import mouth, 5. suction nozzle 1. enter the mouth; 6. import steel flange, 7. glass wool, 8. carborundum helix tube heating element heater, 9. alundum tube, 10. outlet steel flange, 11. outlet nozzles; 12. the tow outlet mouth, 13. export orientation pulleys, 14. governing mechanism of tension, 15. scales, 16. guidance panels; 17. nitrogen cylinder, 18. import wireways, 19. outlet wireways, 20. tanks, 21. air bottles.
The specific embodiment
Below in conjunction with the accompanying drawing and the specific embodiment the present invention is elaborated.
Static of the present invention spins the structure of a kind of embodiment of carbonizing plant of nanometer tow, and is as shown in Figure 1, comprises alundum tube 9, and the outer periphery of alundum tube 9 is equipped with carborundum helix tube heating element heater 8, and carborundum helix tube heating element heater 8 is wrapped in the glass wool 7.The temperature in the atmosphere chamber that forms in the alundum tube 9 is by guidance panel 16 controls.The two ends of alundum tube 9 utilize fluid sealant to be fixedly connected with import steel flange 6 with outlet steel flange 10 respectively; Import steel flange 6 surfaces stud with suction nozzle 5 and tow import mouth 4; Suction nozzle 5 is connected with air bottle 21 through import wireway 18 when pre-oxidation; When carbonization, be connected and tow import mouth 4 corresponding inlet guide pulley 3 and the inlet clamping bodies 1 of being disposed with nitrogen cylinder 17; Outlet steel flange 10 surfaces stud with outlet nozzle 11 and tow outlet mouth 12; Outlet nozzle 11 is connected with outlet wireway 19, and the other end of outlet wireway 19 imports in the tank 20 and tow outlet mouth 12 correspondences are disposed with export orientation pulley 13 and governing mechanism of tension 14; Governing mechanism of tension 14 is provided with scale 15; Nanometer tow 2 one end utilizations inlet clamping body 1 is fixing, through inlet guide pulley 3 and tow import mouth 4, through the atmosphere chamber in the alundum tube 9; Through tow outlet mouth 12 and export orientation pulley 13, and finally be connected with governing mechanism of tension 14 at the other end.The variation of nanometer tow 2 expansion and contractions is confirmed by scale 15.
The carbonizing plant that utilizes above-mentioned static to spin the nanometer tow prepares the method for carbon nano-fiber, specifically implements according to following steps:
Step 1: adopting mass concentration is the PAN/DMF solution of 15wt%, and flow velocity is 0.3mL/h; The No.1 number of pin is 12 #, adjustment receiving range, applied voltage and the spinning time, utilizes the plane aluminium sheet to spin as receiving system acquisition static and aligns nanometer tow 2.
Step 2: the atmosphere chamber that utilizes the stainless steel guide rod that nanometer tow 2 is introduced in the alundum tube 9; Nanometer tow 2 one ends are fixed in inlet clamping body 1; The other end utilizes governing mechanism of tension 14 to apply suitable tension force according to the line density of nanometer tow 2, and it is adjustable at 0.04～0.26cN/dtex to apply tension range.
Through control panel 16 heating schedule is set, comprises pre-oxidation temperature programming, pre-oxidation final temperature short time constant temperature zone and carbonation reaction temperature program.In the pre-oxidation stage, programming rate should remain on than low value, and such as 0.2～2 ° of C/min, temperature is raised to 300 ° of C from room temperature.Suitable rate of heat release can reduce the local thermal accumlation and the coking of fibre bundle, otherwise the concentrated heat release meeting that bigger reaction rate is brought makes big molecular disorientation and polymer fusion.The purpose that pre-oxidation final temperature short time constant temperature zone is set is before carburizing reagent is carried out, to make nitrogen be full of whole atmosphere chamber in order to guarantee, to accomplish adequately protecting to the nanometer tow.The constant temperature zone temperature is 280～300 ° of C, and the retention time is 3～20min.Carbonation stage can be selected bigger programming rate, and such as 5～35 ° of C/min, temperature is raised to 1600 ° of C from 280 ° of C.Because PAN nanofiber precursor has been converted into heat-resisting hexatomic ring trapezium structure after pre-oxidation treatment, the oxygen silk finally is converted into the carbon nano-fiber with random graphits structure through low-temperature carbonization (300～1000 ° of C) and high temperature cabonization (1100～1600 ° of C) more in advance.
Step 3: air bottle 21 is connected with suction nozzle 5 through import wireway 18; Open air bottle 21 valves; Open the predetermined heating schedule of carborundum helix tube heating element heater 8 operations, carry out the pre-oxidation reaction, treat pre-oxidation temperature programming end of run after; Close air bottle 21 valves, itself and import wireway 18 are broken away from.
Step 4: nitrogen cylinder 17 is connected with suction nozzle 5 through import wireway 18, opens nitrogen cylinder 17 valves, guarantee that nitrogen can be full of whole atmosphere chamber during constant temperature zone, in carbonisation so that nitrogen adequately protects to nanometer tow 2.Simultaneously, the line density according to preparatory oxygen tow during constant temperature zone utilizes governing mechanism of tension 14 adjustings to add tension force, and it is adjustable at 0.005～0.12cN/dtex to apply tension range.After treating the carbonation reaction temperature EP (end of program), prepare carbon nano-fiber.
Embodiment 1
In solution concentration is 15wt%; Flow velocity is 0.3mL/h; Receiving range is 11cm; Applied voltage is 11kV; The No.1 number of pin is 12#; The spinning time is under the spinning process condition of 20～40min, and the static that utilizes the plane aluminium sheet to obtain as receiving system spins and aligns the nanometer tow as nanometer tow 2.Utilize the stainless steel guide rod that nanometer tow 2 is introduced the atmosphere chamber; Nanometer tow 2 one ends are fixed in inlet clamping body 1; The other end applies the tension force that adds of 0.01～0.08cN/dtex according to the line density of nanometer tow 2; Suction nozzle 5 is connected with air bottle 21 through import wireway 18, and outlet nozzle 11 imports tank 20 through outlet wireway 19.Through guidance panel 16 heating schedule is set, comprises pre-oxidation temperature programming (25～283 ° of C; 0.2 short time constant temperature zone (283 ° of C～2 ° of C/min); 5～15min) and carbonation reaction temperature program (283～400 ° of C; 5～35 ° of C/min).Open air bottle 21 valves, open carborundum helix tube heating element heater 8 operation heating schedules, treat pre-oxidation temperature programming end of run after, close air bottle 21 valves, and with itself and suction nozzle 5 disengagings.Simultaneously nitrogen cylinder 17 is connected with suction nozzle 5 through import wireway 18; Open nitrogen cylinder 17 valves; Carbonation stage adds tension force 0.005～0.06cN/dtex; The Young's modulus of the carbon nano-fiber of preparing at last is 15～50cN/dtex, and elongation at break is 2～9%, and electrical conductivity is 0.002～0.045S/cm.
Embodiment 2
In solution concentration is 15wt%; Flow velocity is 0.3mL/h; Receiving range is 12cm; Applied voltage is 12kV; The No.1 number of pin is 12#; The spinning time is under the spinning process condition of 50～70min, and the static that utilizes the plane aluminium sheet to obtain as receiving system spins and aligns the nanometer tow as nanometer tow 2.Utilize the stainless steel guide rod that nanometer tow 2 is introduced the atmosphere chamber; Nanometer tow 2 one ends are fixed in inlet clamping body 1; The other end applies the tension force that adds of 0.03～0.12cN/dtex according to the line density of nanometer tow 2; Suction nozzle 5 is connected with air bottle 21 through import wireway 18, and outlet nozzle 11 imports tank 20 through outlet wireway 19.Through guidance panel 16 heating schedule is set, comprises pre-oxidation temperature programming (25～283 ° of C; 0.2 short time constant temperature zone (283 ° of C～2 ° of C/min); 5～15min) and carbonation reaction temperature program (283～700 ° of C; 5～35 ° of C/min).Open air bottle 21 valves, open carborundum helix tube heating element heater 8 operation heating schedules, treat pre-oxidation temperature programming end of run after, close air bottle 21 valves, and with itself and suction nozzle 5 disengagings.Simultaneously nitrogen cylinder 17 is connected with suction nozzle 5 through import wireway 18; Open nitrogen cylinder 17 valves; Carbonation stage adds tension force 0.01～0.08 cN/dtex; The Young's modulus of the carbon nano-fiber of preparing at last is 150～400cN/dtex, and elongation at break is 0.2～1.5%, and electrical conductivity is 0.003～0.062S/cm.
Embodiment 3
In solution concentration is 15wt%; Flow velocity is 0.3mL/h; Receiving range is 13cm; Applied voltage is 13kV; The No.1 number of pin is 12#; The spinning time is under the spinning process condition of 80～100min, and the static that utilizes the plane aluminium sheet to obtain as receiving system spins and aligns the nanometer tow as nanometer tow 2.Utilize the stainless steel guide rod that nanometer tow 2 is introduced the atmosphere chamber; Nanometer tow 2 one ends are fixed in inlet clamping body 1; The other end applies the tension force that adds of 0.04～0.14cN/dtex according to the line density of nanometer tow 2; Suction nozzle 5 is connected with air bottle 21 through import wireway 18, and outlet nozzle 11 imports tank 20 through outlet wireway 19.Through guidance panel 16 heating schedule is set, comprises pre-oxidation temperature programming (25～283 ° of C; 0.2 short time constant temperature zone (283 ° of C～2 ° of C/min); 5～15min) and carbonation reaction temperature program (283～1000 ° of C; 5～35 ° of C/min).Open air bottle 21 valves, open carborundum helix tube heating element heater 8 operation heating schedules, treat pre-oxidation temperature programming end of run after, close air bottle 21 valves, and with itself and suction nozzle 5 disengagings.Simultaneously nitrogen cylinder 17 is connected with suction nozzle 5 through import wireway 18; Open nitrogen cylinder 17 valves; Carbonation stage adds tension force 0.02～0.12cN/dtex; The Young's modulus of the carbon nano-fiber of preparing at last is 200～550cN/dtex, and elongation at break is 0.1～1.3%, and electrical conductivity is 50～500S/cm.
Claims (5)
1. the method for preparing carbon nano-fiber; It is characterized in that; Adopt static to spin the carbonizing plant of nanometer tow; The structure of this device is: comprise alundum tube (9), the outer periphery of alundum tube (9) is equipped with carborundum helix tube heating element heater (8), and carborundum helix tube heating element heater (8) is wrapped in the glass wool (7); The temperature in the atmosphere chamber that forms in the alundum tube (9) is controlled by guidance panel (16); The two ends of alundum tube (9) are fixedly connected with outlet steel flange (10) with import steel flange (6) respectively, and described import steel flange (6) surface studs with suction nozzle (5) and tow import mouth (4), and suction nozzle (5) is connected with air bottle (21) through import wireway (18) when pre-oxidation; Suction nozzle (5) is connected with nitrogen cylinder (17) and corresponding inlet guide pulley (3) and the inlet clamping body (1) of being disposed with of described tow import mouth (4) through import wireway (18) when carbonization; Described outlet steel flange (10) surface studs with outlet nozzle (11) and tow outlet mouth (12); Outlet nozzle (11) is connected with outlet wireway (19); The other end of outlet wireway (19) imports in the tank (20); Be disposed with export orientation pulley (13) and governing mechanism of tension (14) with described tow outlet mouth (12) correspondence
Specifically implement according to following steps:
Step 1: adopt conventional static spinning method to prepare nanometer tow (2);
Step 2: nanometer tow (2) one ends that step 1 obtains are fixing through inlet clamping body (1); Through inlet guide pulley (3) and tow import mouth (4); Through the atmosphere chamber in the alundum tube (9); Through tow outlet mouth (12) and export orientation pulley (13), finally be connected with governing mechanism of tension (14) at the other end, applying tension force through governing mechanism of tension (14) setting is 0.04～0.26 cN/dtex; Simultaneously, heating schedule is set, comprises pre-oxidation temperature programming, pre-oxidation final temperature short time constant temperature zone program and carbonation reaction temperature program through guidance panel (16);
Step 3: air bottle (21) is connected with suction nozzle (5) through import wireway (18); Open air bottle (21) valve; Open carborundum helix tube heating element heater (8), the pre-oxidation temperature programming of setting according to step 2 carries out the pre-oxidation reaction, after reaction finishes; Close air bottle (21) valve, air bottle (21) and import wireway (18) are broken away from;
Step 4: nitrogen cylinder (17) is connected with suction nozzle (5) through import wireway (18); Open nitrogen cylinder (17) valve; Add tension range at 0.005～0.12 cN/dtex through governing mechanism of tension (14) adjusting; Pre-oxidation final temperature short time constant temperature zone program according to step 2 is set is carried out isothermal reaction, and the carbonation reaction temperature program of setting according to step 2 is then carried out carburizing reagent, prepares carbon nano-fiber.
2. the method for preparing carbon nano-fiber according to claim 1 is characterized in that, described governing mechanism of tension (14) is provided with scale (15).
3. the method for preparing carbon nano-fiber according to claim 1 is characterized in that, described pre-oxidation temperature programming, and temperature is raised to 300 ° of C from room temperature, and programming rate is 0.2～2 ° of C/min.
4. the method for preparing carbon nano-fiber according to claim 1 is characterized in that, described pre-oxidation final temperature short time constant temperature zone program, and temperature is 280～300 ° of C, the retention time is 3～20min.
5. the method for preparing carbon nano-fiber according to claim 1 is characterized in that, described carbonation reaction temperature program, and temperature is raised to 1600 ° of C from 280 ° of C, and programming rate is 5～35 ° of C/min.
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| CN102560890A (en) * | 2011-12-15 | 2012-07-11 | 东华大学 | Carbon nanofiber/zinc titanate composite for personal protection and production method of carbon nanofiber/zinc titanate composite for personal protection |
| CN102560889B (en) * | 2012-01-05 | 2014-04-02 | 黑龙江大学 | Method for producing bead-stringed PAN (polyacrylonitrile)-based carbon fiber electrode materials by electrostatic spinning |
| CN102936763B (en) * | 2012-10-12 | 2015-03-18 | 福建师范大学 | Glass carbon nanometer fiber preparation method |
| CN105859293B (en) * | 2014-11-10 | 2018-06-29 | 叶青 | Vitreous carbon and its manufactured artificial trachea for artificial trachea |
| CN110184684B (en) * | 2019-05-21 | 2021-02-02 | 江西先材纳米纤维科技有限公司 | Preparation method of high-dispersity electrospun polyacrylonitrile-based carbon nano ultrashort fiber |
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| CN1861851A (en) * | 2006-02-10 | 2006-11-15 | 肖忠渊 | Apparatus of automatically cleaning deposit for producing carbon fibre carbonizing equipment |
| CN201738045U (en) * | 2010-07-09 | 2011-02-09 | 东华大学 | Simple preoxidation and carbonization integral device |
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| JP2007084953A (en) * | 2005-09-22 | 2007-04-05 | Toho Tenax Co Ltd | Heat treating furnace and method of heat treatment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1861851A (en) * | 2006-02-10 | 2006-11-15 | 肖忠渊 | Apparatus of automatically cleaning deposit for producing carbon fibre carbonizing equipment |
| CN201738045U (en) * | 2010-07-09 | 2011-02-09 | 东华大学 | Simple preoxidation and carbonization integral device |
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