CN111809274A - Device and method for preparing continuous carbon nanotube fiber based on laser heating post-treatment - Google Patents
Device and method for preparing continuous carbon nanotube fiber based on laser heating post-treatment Download PDFInfo
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Abstract
The invention relates to the technical field of nano material preparation, in particular to a device and a method for preparing continuous carbon nanotube fibers based on laser heating post-treatment, which comprises a CVD reaction system, a laser post-treatment system and a control system, wherein the CVD reaction system comprises an injection port and a chemical vapor deposition reaction chamber and is used for preparing the carbon nanotube fibers; the laser post-processing system comprises a laser heating device and a temperature measuring device, the laser heating device performs irradiation heating on the carbon nanotube fiber to form a heating area, and the temperature measuring device performs real-time temperature measurement on the temperature in the heating area; the control system is respectively connected with the CVD reaction system and the laser post-processing system and is used for controlling the reaction system and the post-processing system to work coordinately. The invention adopts laser to process the carbon nanotube fiber on line, removes the redundant impurities on the carbon nanotube fiber prepared by the CVD method, leads the performance of the fiber to be higher, has good surface quality, and can produce the carbon nanotube fiber in large batch.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a device and a method for preparing continuous carbon nano tube fibers based on laser heating post-treatment.
Background
The carbon nanotube fiber is a one-dimensional macroscopic assembly of the carbon nanotube, and is widely applied to the fields of aerospace, national defense and military wearable electronic products and the like due to the unique high porosity/specific surface area, excellent mechanical/physical properties, excellent structural flexibility and novel corrosion/oxidation resistivity.
The key to realizing the application of the carbon nano tube is to prepare the carbon nano tube with excellent performance in a large scale. The CVD floating gas-phase spinning method is the most potential method for preparing carbon nano tube fibers in a large scale, and the method can be used for preparing the carbon nano tube fibers in the order of thousands of meters. However, most of the carbon nanotube fibers prepared by the existing CVD method contain more impurities and amorphous carbon particles, the tensile strength is low, the interior of the fibers is mostly of a mechanical lapping structure which is randomly distributed, and the electrical properties are poor due to large contact resistance. Impurities on the carbon nano tube fiber can be removed through laser heating, an interconnection structure is generated inside the fiber, and mechanical and electrical properties are improved.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a device and a method for preparing continuous carbon nanotube fibers based on laser heating post-treatment, which can solve the problems of impurities, poor mechanical properties and poor electrical properties of the carbon nanotube fibers prepared by a CVD method to a certain extent.
The technical scheme adopted by the invention for solving the technical problems is as follows: a device for preparing continuous carbon nano tube fiber based on laser heating post-treatment comprises a CVD reaction system, a laser post-treatment system and a control system,
the CVD reaction system is used for preparing carbon nanotube fibers and comprises an injection port, a chemical vapor deposition reaction chamber and a water tank, wherein the injection port is arranged at the upper end of the chemical vapor deposition reaction chamber, the water tank is arranged at the lower end of the chemical vapor deposition reaction chamber, and a rotating shaft is arranged in the water tank;
the laser post-processing system comprises a laser heating device for carrying out irradiation heating on the carbon nano tube fiber and a temperature measuring device for carrying out real-time temperature measurement on the temperature in a heating area;
and the control system is used for controlling the reaction system and the post-processing system to work coordinately and is respectively electrically connected with the CVD reaction system and the laser post-processing system.
Furthermore, the laser heating device comprises a laser and a laser heating head, the laser and the laser heating head are connected through an optical fiber, and the laser is an optical fiber laser which is arranged independently.
Further, still including setting up the heating platform in CVD reaction system one side, heating platform includes workstation, quartz capsule, spindle and infrared illuminator, and the quartz capsule level is placed on the workstation, and the spindle setting is kept away from CVD reaction system's one end at the workstation, and the axis and the spindle of quartz capsule are perpendicular, offer the aperture that is used for the laser heating head to stretch into on the quartz capsule for the fibrous infrared illuminator setting of stoving carbon nanotube is close to CVD reaction system's one end at the workstation.
Furthermore, the temperature measuring device is a non-contact type temperature measuring instrument and is arranged on the laser heating head.
A method for preparing continuous carbon nanotube fibers based on laser heating post-treatment comprises the following steps:
the method comprises the following steps: preparing a mixed solution comprising a carbon source, a catalyst, a promoter and water as a reaction solution;
step two: injecting the reaction liquid into a chemical vapor deposition reaction chamber through an injection port, gasifying and cracking the reaction liquid by heat, gasifying the reaction liquid, moving the gasified reaction liquid to the lower part of the quartz tube along the carrier gas to gradually generate a black cylindrical carbon nanotube film, and moving the black cylindrical carbon nanotube film to the tail end of the quartz tube under the push of airflow;
step three: then manually stretching an iron wire into the quartz tube from the water tank, pulling the black cylindrical carbon nanotube film out of the water tank, compactly shrinking the black cylindrical carbon nanotube film into carbon nanotube fibers, and then passing the fibers through a rotating shaft in the water tank to obtain the carbon nanotube fibers;
step four: after being dried by an infrared illuminator, the carbon nanotube fiber enters a quartz tube and is subjected to laser heating treatment in an argon flow protection atmosphere;
step five: setting a heating program in a control system, adjusting the defocusing amount of laser heating, positioning the position of the carbon nanotube fiber according to heating requirements, starting the heating program, emitting light by a laser, collimating and focusing laser beams by a laser heating head, irradiating and heating the carbon nanotube fiber to form a laser heating area, detecting the temperature of the fiber in the heating area in real time by a temperature measuring device, and transmitting the result to the control system;
step six: the CVD reaction system continuously generates carbon nanotube fibers, meanwhile, the laser continuously emits light, the spinning shaft at the tail end continuously collects rolls, and the three are linked to realize the on-line treatment of the carbon nanotube fibers by laser heating and the continuous change of the position of an irradiation heating area;
step seven: after the reaction is finished, the laser stops emitting light under the control of the control system, the CVD reaction system is cooled, the spinning shaft stops rotating, and the fiber roll is unloaded.
Further, the catalyst comprises a carbon source, a catalyst, an accelerant and water, and the components in percentage by mass are as follows: 92-96% of carbon source, 1.0-2.5% of catalyst, 0.6-1.5% of accelerant and 2.0-5.0% of water.
Further, the carbon source is acetone, ethanol, ethylene glycol or n-hexane, and the catalyst is a compound of iron, cobalt and nickel.
Further, the temperature of the CVD reaction system is 500-1100 ℃, and the temperature of the laser heating zone is more than 1500 ℃.
The method has the advantages that the carbon nanotube fiber prepared from the CVD reaction furnace is heated and processed on line by the laser, redundant impurities and amorphous carbon on the original carbon nanotube fiber are gasified or ablated and removed, meanwhile, the surface of the fiber has certain orientation, a cross-linking structure can be generated inside the carbon nanotube fiber, and the trouble that the carbon nanotube fiber needs to be processed firstly when used subsequently is avoided. The carbon nano tube fiber prepared by the method has few impurities and amorphous carbon particles on the surface, the carbon nano tubes are combined more tightly, and the orientation is obviously improved, so that the mechanical and electrical properties are improved.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic diagram of the apparatus of the present invention;
FIG. 2 is an SEM image of carbon nanotube fibers prepared in example 1;
FIG. 3 is a photomicrograph of the carbon nanotube fiber prepared in example 1;
fig. 4 is a comparison graph of raman spectra of the original carbon nanotube fiber prepared in example 1.
In the figure, 1, an injection port, 2, a chemical vapor deposition reaction chamber, 3, a water tank, 4, a rotating shaft, 5, a temperature measuring device, 6, a laser, 7, a laser heating head, 8, an optical fiber, 9, a workbench, 10, a quartz tube, 11, a spinning shaft, 12, an infrared light lamp and 13, a carbon nano tube fiber are arranged.
Detailed Description
As shown in fig. 1, which is a schematic structural diagram of the present invention, an apparatus for preparing continuous carbon nanotube fibers based on laser heating post-treatment includes a CVD reaction system, a laser post-treatment system and a control system, the CVD reaction system, which is used for preparing carbon nanotube fibers 13, includes an injection port 1, a chemical vapor deposition reaction chamber 2 and a water tank 3, the upper end of the chemical vapor deposition reaction chamber 2 is provided with the injection port 1, the lower end of the chemical vapor deposition reaction chamber 2 is provided with the water tank 3, a rotating shaft 4 is arranged inside the water tank 3, and the water tank 3 is used for compacting a cylindrical carbon nanotube film formed inside the reaction chamber by water to obtain the continuous carbon nanotube fibers 13;
the laser post-processing system comprises a laser heating device for carrying out irradiation heating on the carbon nanotube fiber 13 and a temperature measuring device 5 for carrying out real-time temperature measurement on the temperature in a heating area, wherein the temperature measuring device 5 is a non-contact type temperature measuring instrument, the temperature measuring device 5 is arranged on a laser heating head 7, non-contact type temperature detection is carried out on the heating area, the result is input into a control system, and the control system and a laser 6 or a heating platform carry out information interaction to realize closed-loop control of the heating temperature;
the laser heating device comprises a laser 6 and a laser heating head 7, the laser 6 is connected with the laser heating head 7 through an optical fiber 8, the laser 6 is an independently arranged optical fiber laser, and the laser heating head 7 is used for collimating and focusing laser so that the laser output by the laser 6 can meet the heating requirement of a material with a certain width;
and the control system is used for controlling the reaction system and the post-processing system to work coordinately and is respectively electrically connected with the CVD reaction system and the laser post-processing system.
Still including setting up the heating platform in CVD reaction system one side, heating platform includes workstation 9, quartz capsule 10, spindle 11 and infrared illuminator 12, quartz capsule 10 level is placed on workstation 9, spindle 11 sets up the one end of keeping away from CVD reaction system at workstation 9, the axis of quartz capsule 10 is perpendicular with spindle 11, set up the aperture that is used for laser heating head 7 to stretch into on the quartz capsule 10, an infrared illuminator 12 setting for drying carbon nanotube fibre 13 is close to CVD reaction system's one end at workstation 9.
The laser heating system comprises a gas path pipe, an infrared illuminator 12, carbon nanotube fibers 13, a quartz tube 10, a spindle 11, a laser heating head 7, a temperature measuring device 5, an optical fiber 8 and a laser 6, wherein the laser 6 is an optical fiber laser, and the laser heating head 7 is connected with the laser 6 through the optical fiber 8; the quartz tube 10 is fixed on the laser heating workbench 9, the left end of the quartz tube 10 is connected with the CVD reaction system through an air path tube, meanwhile, the left end is provided with an infrared illuminator 12 for drying carbon nanotube fibers 13 pulled out from water, the right end of the quartz tube 10 is provided with a spindle 11 for collecting the finally prepared carbon nanotube fibers 13, and the axis of the quartz tube 10 is vertical to the spindle 11; the temperature measuring device 5 is arranged on the laser heating head 7 through a magnetic clamp, and the temperature measuring device 5 is detected by adopting a non-contact temperature measuring device; the input end of the laser 6 and the output end of the temperature measuring device 5 are respectively electrically connected with the output end and the input end of the control system.
A method for preparing continuous carbon nanotube fibers based on laser heating post-treatment comprises the following specific implementation steps: after the reaction liquid is prepared, the reaction liquid enters the reaction chamber from the injection port 1, is gasified and cracked under heat, and moves to the lower part of the quartz tube 10 along the carrier gas after being gasified to gradually generate a black cylindrical carbon nanotube film and moves to the tail end of the quartz tube 10 under the push of airflow; then manually stretching an iron wire into the quartz tube 10 from the water tank 3, and after pulling the black cylindrical carbon nanotube film out of the water tank 3, compactly shrinking the black cylindrical carbon nanotube film into carbon nanotube fibers; then the fiber passes through a rotating shaft 4 in the water tank 3 to obtain carbon nanotube fiber 13; then, the carbon nanotube fiber 13 is dried by an infrared illuminator 12, enters a quartz tube 10, and is subjected to laser heating treatment in an argon gas flow protection atmosphere; setting a heating program in a control device, and adjusting the defocusing amount of laser heating; positioning the carbon nanotube fiber 13 according to the heating requirement; starting a heating program, enabling the laser 6 to emit light, collimating and focusing laser beams through the laser heating head 7, irradiating and heating the carbon nanotube fibers 13 to form a laser heating area, and enabling the laser output by the laser 6 to meet the heating requirement at a certain temperature; the reaction system continuously generates carbon nanotube fibers 13, meanwhile, the laser 6 continuously emits light, the tail spinning shaft 11 continuously collects the rolls, the carbon nanotube fibers 13 are subjected to laser heating on line through linkage of the three, and the positions of the irradiation heating areas continuously change. The temperature measuring device 5 detects the temperature of the fiber in the heating area in real time, transmits the result to the control system, and conveniently and timely adjusts the output power of the laser 6 when the temperature deviates from the temperature required by heating, so as to realize the adjustment of the temperature of the heating area; after the reaction is finished, under the control of the control system, the laser 6 stops emitting light, the reaction system cools down, the spinning shaft 11 stops rotating, and the fiber roll is unloaded.
Example 1
0.5g of water is introduced into a solution containing 0.25g of ferrocene, 25g of ethanol and 0.15g of thiophene to prepare a mixed solution, and the mixed solution is injected into an injection port with the diameter of 1mm and enters 900sccm H2Airflow quartzIn the tube, the upper temperature of the resistance furnace is set to be 500 ℃, the middle temperature and the lower temperature are set to be 1100 ℃, the reaction can continuously obtain the cylindrical carbon nano tube aerogel, and the cylindrical carbon nano tube aerogel is compacted by water and then mechanically wound to obtain the continuous carbon nano tube fiber. Then enter 700sccm Ar2In the airflow quartz tube, the laser power is set to be 6-8W, the scanning speed is set to be 200mm/s, the diameter of a light spot is about 30 mu m, a T-shaped interconnected topography can be obtained under the action of laser, and the connection part is smooth.
The preparation process comprises the following steps:
(1) checking the air tightness of the device, setting the upper temperature of the resistance furnace to be 500 ℃, setting the middle and lower temperatures to be 1100 ℃, and introducing hydrogen into a quartz tube at the flow rate of 900 sccm;
(2) 0.25g of ferrocene, 25g of ethanol, 0.15g of thiophene and 0.5g of water are sequentially added into a beaker, mixed until the solution is clear, and the solution is injected into a reaction furnace through an injection port 1.
(3) The reaction liquid on the upper part of the quartz tube is subjected to gasification cracking (the temperature is higher than 400 ℃) to generate white aerogel-like substances, the white aerogel-like substances reach the middle part of the quartz tube to generate black cylindrical carbon nanotube films (the temperature is about 1100 ℃), when the generated cylindrical carbon nanotube films are driven by hydrogen to reach the bottom end of the quartz tube to be close to the water tank sealing cover, the cylindrical carbon nanotube films are manually pulled by iron wires to pass through water and shrink into filaments, and the filaments bypass the rotating shaft in the water tank to change the direction and reach an external spindle, are dried by the infrared illuminator 11 and then are.
(4) The power of the laser is set through the control device, the laser heating head emits light, the position of the carbon nanotube fiber is well adjusted, and the carbon nanotube fiber with good performance is obtained by collecting the carbon nanotube fiber through an external spindle after the carbon nanotube fiber is subjected to online post-treatment through laser heating.
The average diameter of the obtained fiber is about 140 μm, as shown in FIGS. 2 and 3.
The tensile strength of the fiber is about 120-140 MPa, and the linear density is about 0.7 tex.
The resistance of the fiber was measured to be about 300 Ω at a length of 2 cm.
As can be seen from the raman spectrum of fig. 4, the limiting D peak prepared in this example is decreased, the G peak is increased, and the ratio ID/IG is decreased, which indicates that the impurities are decreased, and is in accordance with the expectation.
The carbon nano tube fiber prepared by the method has few impurities and amorphous carbon particles on the surface, the carbon nano tubes are combined more tightly, and the orientation is obviously improved, so that the mechanical and electrical properties are improved.
The foregoing description is intended to be illustrative rather than limiting, and it will be appreciated by those skilled in the art that many modifications, variations or equivalents may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. A device for preparing continuous carbon nano tube fiber based on laser heating post-treatment is characterized by comprising a CVD reaction system, a laser post-treatment system and a control system,
the CVD reaction system is used for preparing carbon nanotube fibers (13) and comprises an injection port (1), a chemical vapor deposition reaction chamber (2) and a water tank (3), wherein the injection port (1) is arranged at the upper end of the chemical vapor deposition reaction chamber (2), the water tank (3) is arranged at the lower end of the chemical vapor deposition reaction chamber (2), and a rotating shaft (4) is arranged in the water tank (3);
the laser post-processing system comprises a laser heating device for carrying out irradiation heating on the carbon nano tube fiber (13) and a temperature measuring device (5) for carrying out real-time temperature measurement on the temperature in a heating area;
and the control system is used for controlling the reaction system and the post-processing system to work coordinately and is respectively electrically connected with the CVD reaction system and the laser post-processing system.
2. The apparatus for manufacturing continuous carbon nanotube fiber based on laser heating post-treatment according to claim 1, wherein the laser heating apparatus comprises a laser (6) and a laser heating head (7), the laser (6) and the laser heating head (7) are connected by an optical fiber (8), and the laser (6) is a separately installed fiber laser.
3. The device for preparing the continuous carbon nanotube fiber based on the laser heating post-treatment as claimed in claim 1, further comprising a heating platform arranged on one side of the CVD reaction system, wherein the heating platform comprises a workbench (9), a quartz tube (10), a spindle (11) and an infrared illuminator (12), the quartz tube (10) is horizontally arranged on the workbench (9), the spindle (11) is arranged at one end of the workbench (9) far away from the CVD reaction system, the axis of the quartz tube (10) is perpendicular to the spindle (11), a small hole for the laser heating head (7) to extend into is arranged on the quartz tube (10), and the infrared illuminator (12) for drying the carbon nanotube fiber is arranged at one end of the workbench (9) close to the CVD reaction system.
4. The apparatus for manufacturing continuous carbon nanotube fiber based on laser heating post-treatment according to claim 1, wherein the temperature measuring device (5) is a non-contact type temperature measuring instrument, and the temperature measuring device (5) is disposed on the laser heating head (7).
5. A method for preparing continuous carbon nanotube fibers based on laser heating post-treatment is characterized by comprising the following steps:
the method comprises the following steps: preparing a mixed solution comprising a carbon source, a catalyst, a promoter and water as a reaction solution;
step two: injecting the reaction liquid into a chemical vapor deposition reaction chamber (2) through an injection port (1), gasifying and cracking the reaction liquid under heat, gasifying the reaction liquid, moving the gasified reaction liquid to the lower part of a quartz tube (10) along a carrier gas to gradually generate a black cylindrical carbon nanotube film, and moving the black cylindrical carbon nanotube film to the tail end of the quartz tube (10) under the push of airflow;
step three: then manually stretching an iron wire into the quartz tube (10) from the water tank, drawing the black cylindrical carbon nanotube film out of the water tank (3), compactly shrinking the black cylindrical carbon nanotube film into carbon nanotube fibers (13), and then passing the fibers through a rotating shaft (4) in the water tank (3) to obtain the carbon nanotube fibers (13);
step four: after being dried by an infrared illuminator (12), the carbon nano tube fiber enters a quartz tube (10) and is subjected to laser heating treatment in an argon flow protective atmosphere;
step five: setting a heating program in a control system, adjusting the defocusing amount of laser heating, positioning the position of the carbon nanotube fiber (13) according to heating requirements, starting the heating program, emitting light by a laser (6), collimating and focusing laser beams through a laser heating head (7), irradiating and heating the carbon nanotube fiber (13) to form a laser heating area, detecting the temperature of the fiber in the heating area in real time through a temperature measuring device (5), and transmitting the result to the control system;
step six: the CVD reaction system continuously generates carbon nanotube fibers (13), meanwhile, the laser (6) continuously emits light, the tail end spinning shaft (11) continuously collects rolls, the three are linked, the carbon nanotube fibers (13) are processed on line by laser heating, and the positions of irradiation heating areas are continuously changed;
step seven: after the reaction is finished, the laser (6) stops emitting light under the control of the control system, the CVD reaction system is cooled, the spinning shaft (11) stops rotating, and the fiber roll is unloaded.
6. The method for preparing continuous carbon nanotube fiber based on laser heating post-treatment as claimed in claim 5, wherein the carbon source, the catalyst, the promoter and the water comprise the following components by mass percent: 92-96% of carbon source, 1.0-2.5% of catalyst, 0.6-1.5% of accelerant and 2.0-5.0% of water.
7. The method for preparing continuous carbon nanotube fiber based on laser heating post-treatment as claimed in claim 6, wherein the carbon source is acetone, ethanol, ethylene glycol or n-hexane, and the catalyst is a compound of iron, cobalt or nickel.
8. The method of claim 5, wherein the CVD reaction system temperature is 500-1100 ℃ and the laser heating zone temperature is above 1500 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112941680A (en) * | 2021-01-28 | 2021-06-11 | 华侨大学 | Preparation method of carbon nanotube fiber-loaded nano iron oxide composite material |
| CN115466918A (en) * | 2022-09-06 | 2022-12-13 | 哈尔滨工程大学 | Modification method of whisker/fiber surface textured nano bump structure and strengthening and toughening application thereof |
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- 2020-08-25 CN CN202010863188.8A patent/CN111809274A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112941680A (en) * | 2021-01-28 | 2021-06-11 | 华侨大学 | Preparation method of carbon nanotube fiber-loaded nano iron oxide composite material |
| CN115466918A (en) * | 2022-09-06 | 2022-12-13 | 哈尔滨工程大学 | Modification method of whisker/fiber surface textured nano bump structure and strengthening and toughening application thereof |
| CN115466918B (en) * | 2022-09-06 | 2024-04-16 | 哈尔滨工程大学 | Whisker/fiber surface texturing nano bump structure modification method and toughening application thereof |
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