CN111778586A - Preparation method of twist-controllable graphene fiber - Google Patents
Preparation method of twist-controllable graphene fiber Download PDFInfo
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- CN111778586A CN111778586A CN202010651810.9A CN202010651810A CN111778586A CN 111778586 A CN111778586 A CN 111778586A CN 202010651810 A CN202010651810 A CN 202010651810A CN 111778586 A CN111778586 A CN 111778586A
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Abstract
The invention provides a preparation method of a twist-controllable graphene fiber, which comprises the following steps: conveying the graphene oxide spinning solution into a spinning channel from the upper part of the spinning channel at a certain speed; carrying out hot air solidification, traction and twisting on the spinning solution in turn from top to bottom in a spinning channel to obtain graphene oxide fibers, wherein a twisting collecting device is arranged below the spinning channel, and twisting with different twists is carried out on the drawn fibers by controlling the rotation of the twisting collecting device; and chemically reducing the graphene oxide fiber to obtain the graphene fiber. The graphene fiber prepared by the method has a controllable and adjustable structure, mechanical properties and electrochemical properties.
Description
Technical Field
The invention relates to the field of graphene fiber preparation, in particular to a preparation method of a twist-controllable graphene fiber, and especially relates to a preparation method of a twist-controllable graphene fiber with a single-fiber twisting structure.
Background
Graphene is a two-dimensional carbon nanomaterial which is composed of carbon atoms in a hexagonal honeycomb lattice by using SP2 hybrid orbitals, is the thinnest and highest-strength material in the world at present, has excellent mechanical, electrical, thermal, optical and other properties, is spotlighted and is a hot spot for research in the scientific and material fields. Macroscopic materials formed by assembling graphene, such as one-dimensional fibers, two-dimensional films, three-dimensional porous aerogels and the like, show good performance and potential application prospects. The one-dimensional graphene fiber material has excellent performance and wide application prospect in the aspects of flexible electrodes, supercapacitors, sensors, intelligent wearable devices and the like. Due to the strong acting force between graphene sheets, agglomeration and stacking are easy to occur, and the graphene sheets are insoluble in most solvents, so that the macroscopic graphene fiber material is difficult to construct through graphene assembly. Graphene oxide as a graphene derivative has rich oxygen-containing functional groups, such as hydroxyl, carboxyl, epoxy, and the like, so that graphene oxide is soluble in most solvents, and graphene can be obtained through chemical reduction or thermal reduction, which is a good choice for preparing macroscopic graphene functional materials.
At present, graphene oxide is mainly used as a raw material for preparing graphene fibers through a wet spinning process, so that the limitation of a template method, a film shrinkage method, an electrophoresis assembly method and the like on the aspects of molding size, preparation efficiency, mechanical properties and the like is broken through, graphene fiber filaments with better performance can be continuously prepared, and the method is a good technology capable of industrial production. However, in the wet spinning forming technology, a coagulation bath plays a decisive role, and the nascent graphene oxide fiber is shrunk, coagulated, solidified and formed in the coagulation bath, and then dried and washed to obtain the graphene oxide fiber. Common coagulating baths are organic and inorganic salt solutions, such as ethanol, DMF, CTAB, calcium chloride, potassium hydroxide, and the like. In a coagulation bath, the nascent graphene oxide fibers can absorb coagulants in the process of coagulation shrinkage, and the coagulants are difficult to clean in the subsequent washing and drying processes and become impurities in the fibers to influence the fiber performance. In addition, the nascent fiber needs a certain time to be coagulated in a coagulation bath to form fiber, so the efficiency of wet spinning still needs to be improved.
The dry spinning technology is a spinning technology which takes a high-concentration graphene oxide solution as a raw material, enables a solvent in a spinning solution to be rapidly volatilized through high-temperature hot air flow in a spinning channel, and dries and forms fibers. Compared with wet spinning, the method has the most outstanding advantages that no coagulating bath is needed, the fiber is not required to stay in the coagulating bath in the preparation process, and repeated washing is not required in the subsequent process to remove residual coagulating agent. Therefore, the process of preparing the graphene fiber by dry spinning is shorter and more convenient, and the fiber is purer. The invention patent application 'an ultra-high flexible graphene fiber prepared by dry spinning and a preparation method thereof' (201810012261.3) discloses a dry spinning technology of graphene fiber. However, in the dry spinning process, the outer surface layer of the fiber is firstly dried, cured and molded to form a skin layer structure, which easily causes the graphene oxide in the core layer to be dried slowly, and the cured structure of the skin layer makes the stacking of the graphene oxide sheets in the core layer not compact enough, thereby affecting the mechanical property, the electrochemical property and the like of the fiber. In the patent application for invention
(201810011288.0) adjusting the angle of hot air flow, and obtaining graphene fibers with a certain twist structure by utilizing the rotation of air flow in a spinning channel, wherein the densification degree among graphene sheets in the fibers can be improved by single-fiber spinning twisting. But the twisting effect of hot air flow is limited, and the mechanical and other related properties of the fiber are not improved enough. Therefore, the dry spinning process of the graphene oxide fiber is further optimized and upgraded, the single-fiber twist structure of the graphene fiber is regulated and controlled through related technologies, the internal structure of the fiber can be effectively controlled, and the graphene fiber with different corresponding optimized performances is obtained.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention discloses a preparation method of a graphene fiber with controllable twist. The specific technical scheme is as follows:
the invention provides a preparation method of a twist-controllable graphene fiber, which comprises the following steps:
conveying the graphene oxide spinning solution into a spinning channel from the upper part of the spinning channel at a certain speed;
carrying out hot air solidification, traction and twisting on the spinning solution in turn from top to bottom in a spinning channel to obtain graphene oxide fibers, wherein a twisting collecting device is arranged below the spinning channel, and twisting with different twists is carried out on the drawn fibers by controlling the rotation of the twisting collecting device;
and chemically reducing the graphene oxide fiber to obtain the graphene fiber.
Further, in step S1, the graphene spinning solution is prepared as follows:
s11, preparing a graphene oxide aqueous solution by an improved Hummers method, wherein the concentration of the graphene oxide aqueous solution is 5-30 mg/ml;
s12, stirring the graphene oxide aqueous solution at 40-100 ℃ for 12-48 hours to obtain a graphene spinning solution, wherein the stirring speed is 200-1000 r/min, and the concentration of the obtained graphene spinning solution is 40-60 mg/ml;
s13, adding the graphene oxide spinning solution into a spinning container, and spinning the graphene oxide spinning solution into an inner cavity of a spinning channel through a spinning hole in the upper end of the spinning channel at a certain spinning speed by using a metering pump, wherein the inner diameter of the spinning hole is 0.1-5 mm; the spinning speed is 0.1-10 ml/h.
Further, step S2 specifically includes,
s21, blowing hot air from the upper end of the spinning channel into the inner cavity of the spinning channel obliquely towards the spinning solution through a hot air conveying device to solidify the spinning solution, and obtaining solidified fibers, wherein the included angle between the hot air spraying direction of the hot air conveying device and the central axis of a spinning hole is 0-60 degrees, the temperature of the hot air is 100-500 ℃, and the flow rate of the hot air in the inner cavity of the spinning channel is 3-50L/min;
s22, drawing and outputting the solidified fibers through a drawing roller, wherein the central shaft of the drawing roller is vertical to the central shaft of the spinning hole, and the drawing speed of the drawing roller is consistent with the filament outlet speed of the spinning hole;
and S23, carrying out first rotation below the spinning channel by controlling the twisting collecting device, twisting the fibers output by traction in the step S22 with different twists, and simultaneously controlling the twisting collecting device to carry out second rotation to collect the twisted graphene oxide fibers.
Further, in step S21, the length of the spinning shaft is 30-50 cm, and the diameter is 2-5 cm;
in the step S22, the distance between the traction roller and the spinning hole is 10-20 cm;
in step S23, the first rotating twisting speed of the twisting collecting device is 50 to 500r/min, and the second rotating linear speed is consistent with the yarn outlet speed of the spinning hole.
Further, step S3 specifically includes:
and reducing the graphene oxide fibers with different twists in a reducing agent for 4-10 hours at the temperature of 60-200 ℃, and washing and drying to obtain the graphene fibers with different twists, wherein the reducing agent is one or more of hydriodic acid, hydrazine hydrate, sodium borohydride and ascorbic acid.
Furthermore, the device of the method comprises a spinning channel, a spinning pipe, a metering pump, a hot air conveying device, a traction roller and a twisting collecting device,
the spinning channel is vertically arranged in a cylindrical shape and is provided with an inner cavity;
one end of the spinning pipe is communicated with the metering pump, a spinning hole is formed in the other end of the spinning pipe, the spinning pipe is communicated with the spinning channel from the upper end of the spinning channel through the spinning hole, and the metering pump is configured to spray spinning liquid into an inner cavity of the spinning channel through the spinning hole of the spinning pipe;
the hot air conveying device is arranged on one side of the spinning channel and is configured to eject hot air from the upper end of the spinning channel obliquely towards the inner cavity of the spinning channel to solidify spinning solution to form solidified fibers;
the traction roller is positioned in the inner cavity of the spinning channel, and is configured to hold and pull downwards to convey solidified fibers;
the twisting collecting device is arranged below the spinning channel, the free end of the fiber is dragged and output by the twisting collecting device in a supporting mode and rotates around the vertical axial direction to twist the fiber, and meanwhile the twisting collecting device is also arranged to rotate around the horizontal axial direction to wind and collect the twisted fiber.
Further, the device also comprises a spinning container which is communicated with a spinning pipe, the metering pump is configured to extrude spinning solution in the spinning container out of the spinning pipe and spray the spinning solution into an inner cavity of the spinning shaft from the upper part of the spinning shaft through a spinning hole,
the lower end of the spinning channel is provided with an opening for twisted fibers to pass through, and the central axis of the spinning channel is superposed with the central axis of the spinning pipe;
the hot air conveying device is an air-blast electric heating gun, the air-blast electric heating gun comprises a spray head and a control device electrically connected with the spray head, the spray head obliquely extends into the inner cavity of the spinning channel from the upper part of the spinning channel, the spray head is configured to generate hot air to solidify spinning liquid to obtain solidified fibers under the control of the control device, and the flow and the temperature of the sprayed hot air are controlled by the control device;
the traction roller comprises a first roller and a second roller, the first roller and the second roller are arranged in parallel and adjacent to each other, a gap for solidified fibers to pass through is formed between the first roller and the second roller, the fibers are prevented from being extruded and deformed, the fibers are held at the same time, the fibers at a yarn outlet hole are prevented from being broken due to twisting, and central shafts of the first roller and the second roller are respectively vertical to a central shaft of the spinning channel;
the twisting collecting device comprises a rotating platform, a winding roller arranged on the rotating platform, a driving device for respectively driving the rotating platform and the winding roller to rotate and a controller electrically connected with the driving device, wherein the rotating platform is configured to be twisted by the driving device to rotate around the vertical axial direction to the drawn fiber, and the winding roller is configured to be wound and collected by the driving device to rotate around the horizontal axial direction to the twisted fiber.
The blowing electric heating gun further comprises a support, the nozzle comprises a nozzle, a heating device, a blowing device and a handle, the heating device and the blowing device are both located in the handle, the handle is erected on the support, one end of the handle is connected with the nozzle, the other end of the handle is electrically connected with a control device, the nozzle obliquely extends into an inner cavity of the spinning channel from the upper part of the spinning channel, the heating device is configured to generate hot air under the control of the control device, and the blowing device is configured to control the flow of the blown hot air under the control of the control device;
the first roller and the second roller are respectively fixed at one end of a fixed shaft, the other end of the fixed shaft is connected with a motor, the motor is electrically connected with a controller, the controller controls the motor to rotate, and the motor drives the fixed shaft to drive the first roller and the second roller to rotate;
the twisting and collecting device further comprises a translation table arranged on the rotating table, and the translation table is configured to drive the winding roller to perform reciprocating translation by the driving device so as to collect the twisted fibers.
Furthermore, the included angle between the central axis of the nozzle and the central axis of the spinning hole is 0-60 degrees, the central axis of the spinning hole is overlapped with the central axis of the spinning channel, and the inner diameter of the spinning hole is 0.1-5 mm;
the length of the spinning channel is 30-50 cm, the diameter of the spinning channel is 2-5 cm, and the distance between the traction roller and the spinning hole is 10-20 cm.
Furthermore, the spinning container is a glass injector, the injector is communicated with the spinning pipe, the spinning pipe is a stainless steel metal pipe, and the spinning channel is a quartz pipe.
The invention has the following beneficial effects:
(1) according to the invention, the structural order and regularity of graphene sheets in the fiber can be effectively adjusted through monofilament twisting, so that the graphene sheets in the fiber can be orderly arranged in a certain direction, and the performance of the fiber is improved; by controlling the twisting speed, the spinning speed, the hot air temperature and the flow, the twisting structure in the formed fiber can be effectively adjusted, so that the mechanical property and the electrochemical property of the formed fiber can be adjusted and controlled.
(2) According to the invention, hot air solidification, traction and twisting are sequentially completed in the same spinning channel, and graphene sheets in the fiber can be rapidly stacked, solidified and formed while an external skin layer is formed by external twisting and extrusion in the spinning forming process, so that the graphene structure finished by the fiber is more densified, and the fiber performance is improved.
(3) According to the invention, the structure regulation and control of the fiber and the spinning are carried out synchronously, the structure of the prepared graphene fiber with a certain twist structure is formed in a spinning channel, the shaping effect at high temperature is obvious, the structure is stable, the untwisting phenomenon is avoided, the secondary processing is avoided, the process is convenient and fast, the flow is short, and the large-scale production can be realized.
(4) The outer surface of the fiber twisted by the method is more regular, the subsequent processing and use are facilitated, the prepared fiber is better in flexibility, the elongation is increased, and the fiber is more widely applied to flexible electronic devices, wearable intelligent textiles and the like, for example, the elongation of the graphene fiber with the twist of 130r/10cm is 15.2%, the elongation of the graphene fiber with the twist of 1000r/10cm is 19.3%, and the elongation can reach 2 times of that of common dry spinning and 4 times of that of wet spinning.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic view of the structure of a production apparatus of the present invention;
FIG. 2 is a schematic view of the construction of the pulling roll of FIG. 1;
FIG. 3 is a schematic view of the twisting and collecting device of FIG. 1;
FIG. 4 is a scanning electron microscope image of graphene fibers with 130r/10cm twist prepared in example 1 of the present invention;
FIG. 5 is a scanning electron microscope image of graphene fibers with a twist of 1000r/10cm prepared in example 2 of the present invention;
FIG. 6 is a stress-strain curve of graphene fibers with twists of 130r/10cm and 1000r/10cm, respectively.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise. In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or may be connected through the interior of two elements or in interactive relation with one another. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Referring to fig. 1 to 3, fig. 1 is a schematic structural diagram of a manufacturing apparatus according to the present invention; FIG. 2 is a schematic view of the construction of the pulling roll of FIG. 1; FIG. 3 is a schematic view of the twisting and collecting device shown in FIG. 1.
As shown in fig. 1 to 3, the preparation apparatus for graphene fiber with controllable twist according to the present invention includes a spinning shaft 5, a spinning tube 10, a spinning container 2, a metering pump 1, a hot air delivery device 3, a traction roller 6, and a twisting collection device 8.
The spinning channel 5 is vertically arranged in a cylindrical shape, and the spinning channel 5 is provided with an inner cavity 52. The upper end of the spinning channel 5 is provided with an opening 51 for the spinning tube to pass through, the spinning hole of the spinning tube 10 is connected to the opening, the spinning tube 10 is communicated with the spinning channel 5 through the opening, the lower end of the spinning channel 5 is provided with an opening for the twisted fiber to pass through, and the central shaft of the spinning channel 5 coincides with the central shaft of the spinning tube 10. The spinning channel 5 is a high-temperature-resistant quartz tube.
One end of the spinning tube 10 is communicated with the metering pump 1, the other end of the spinning tube forms a spinning hole, the spinning tube is communicated with the spinning channel 5 from the upper end of the spinning channel 5 through the spinning hole, and the metering pump 1 is configured to spray spinning solution into an inner cavity 52 of the spinning channel 5 through the spinning hole of the spinning tube 10.
The central axis of the spinning hole coincides with the central axis of the spinning channel 5, and the inner diameter of the spinning hole 51 is 0.1-5 mm. The length of the spinning channel 5 is 30-50 cm, the diameter of the spinning channel 5 is 2-5 cm, and the distance between the traction roller 6 and the spinning hole is 10-20 cm.
The spinning container 2 is communicated with a spinning pipe 10, and the metering pump 1 is configured to extrude the spinning solution in the spinning container 2 from the spinning pipe 10 and spray the spinning solution into the spinning duct 5 from the upper part of the spinning duct 5 through a spinning hole. In one embodiment, the spinning vessel is an injector, and the injector is a glass injector. The injector is communicated with a spinning pipe 10, and the spinning pipe is a stainless steel metal pipe.
The hot air conveying device 3 is arranged on one side of the spinning duct 5, and the hot air conveying device 3 is configured to eject hot air from the upper end of the spinning duct 5 obliquely towards the inner cavity of the spinning duct 5. The hot air conveying device 3 is an air-blast electric heating gun, the air-blast electric heating gun comprises a spray head 31 and a control device 4 electrically connected with the spray head 31, the spray head 31 obliquely extends into the inner cavity 52 of the spinning duct from the upper part of the spinning duct 5, the temperature of hot air generated by the spray head 31 is controlled by the control device 4, and the flow and the temperature of the sprayed hot air are controlled by the control device 4 of the spray head 31.
The air-blast electric heating gun further comprises a bracket 11, the nozzle 31 comprises a nozzle 311, a heating device (not shown), an air blowing device (not shown) and a handle 312, the heating device and the air blowing device are both positioned in the handle 312, the handle 312 is erected on the bracket 11, one end of the handle 312 is connected with the nozzle 311, the other end of the handle 312 is electrically connected with the control device 4, the nozzle 311 obliquely extends into the inner cavity 52 of the spinning duct 5 from the upper part of the spinning duct, the heating device is configured to generate hot air under the control of the control device 4, and the air blowing device is configured to control the flow of the hot air sprayed out under the control of the control device 4. The included angle between the central axis of the nozzle 311 and the central axis of the spinning hole 51 is 0-60 degrees. Preferably, the central axis of the nozzle 311 is at an angle of 45 ° to the central axis of the spinning hole 51.
The control device 4 comprises a speed regulating button and a temperature regulating button, the hot air ejection flow of the nozzle 31 is controlled by regulating the speed regulating button, and the temperature of the hot air is controlled by regulating the temperature regulating button.
The drawing drum 6 is located in the inner cavity of the spinning shaft and is configured to hold and draw down the hot air-cured fibers. The traction roller comprises a first roller 61 and a second roller 62, the first roller 61 and the second roller 62 are arranged in parallel and adjacent, a gap for solidified fibers to pass through is arranged between the first roller 61 and the second roller 62, the fibers are prevented from being extruded and deformed, the fibers are held, the fibers are prevented from being broken at a yarn outlet due to twisting, and the central axes of the first roller 61 and the second roller 62 are respectively vertical to the central axis of the spinning channel 5. The traction roller 6 is configured to be controlled by the controller 9 to rotate so as to carry out traction output on twisted fibers. In one embodiment, the first roller 61 and the second roller 62 are respectively fixed at one end of a fixed shaft 12, the other end of the fixed shaft 12 extends out of the spinning duct 5 and is connected with a motor (not shown), the controller 9 controls the motor to rotate, the motor drives the fixed shaft 12 to rotate, and the fixed shaft 12 drives the first roller 61 and the second roller 62 to rotate. In one embodiment, the controller is connected to the motor by a wire 13.
The twisting collecting device 8 is located below the spinning duct 5, and the twisting collecting device 8 includes a rotating platform 81, a winding drum 7 disposed on the rotating platform 81, a driving device (not shown) for respectively driving the rotating platform 81 and the winding drum 7 to rotate, and a controller 9 electrically connected to the driving device. Controller 9 control drive arrangement rotates, drive arrangement drives revolving stage 81 rotates around vertical axial to the realization twists to the fibre after pulling, simultaneously, controller 9 control drive arrangement rotates, drive arrangement drives the cylinder 7 that convolutes rotates around horizontal axial emergence, thereby realizes collecting the fibre after the twisting. In one embodiment, the driving device is a motor which simultaneously drives the rotating table and the winding drum to rotate. In another embodiment, the driving device is two motors, and the two motors respectively drive the rotating table and the winding drum to rotate. The rotating speed of the winding drum 7 of the present invention is the same as the spinning speed of the spinning hole 51. In one embodiment, the speed regulating range of the motor is 30-466r/min, and the controller is an intelligent digital display speed regulator.
Twisting collection device 8 still including set up in translation platform (not shown) on the revolving stage, the controller control drive arrangement rotates, drive arrangement drives translation platform takes place the translation, translation platform drives the coiling cylinder takes place to reciprocate the translation to make the fibre regularly distribute in the coiling cylinder. In this embodiment, the driving device may be a single motor.
The preparation method of the twist-controllable graphene fiber according to the present invention is described below with reference to fig. 1 to 3.
Example 1
The invention relates to a preparation method of a twist-controllable graphene fiber, which comprises the following steps:
s1, conveying the graphene oxide spinning solution into the spinning channel from the upper part of the spinning channel at a certain speed, wherein the method specifically comprises the following steps:
a graphene oxide aqueous solution with the concentration of 17mg/ml is prepared by a modified Hummers method, and is stirred at the speed of 500r/min for 36h at the temperature of 60 ℃ to obtain a spinning solution with the concentration of 50 mg/ml. Adding the spinning solution into a spinning container, and spinning the graphene oxide spinning solution into a spinning channel from the upper end of the spinning channel through a spinning hole with the inner diameter of 0.5mm by using a metering pump at the spinning speed of 0.5 ml/h.
S2, in the spinning channel from top to bottom in proper order the spinning solution carries out hot air precuring, traction and twisting, obtains graphene oxide fiber, wherein, the below of spinning channel is provided with twisting collection device, through control twisting collection device' S rotation carries out the twisting of different twists to the fibre after pulling, leads to simultaneously to collect the fibre of twisting, obtains graphene oxide fiber, specifically includes:
after the spinning solution enters a spinning channel through spinning holes of a spinning pipe, hot air is sprayed out from the upper end of the spinning channel into an inner cavity of the spinning channel obliquely towards the spinning solution by using a hot air conveying device, so that the spinning solution is solidified into fibers, and solidified fibers are obtained. The axial included angle between the nozzle of the hot air conveying device and the spinning hole is 45 degrees, the temperature of the hot air is 250 ℃, and the flow of the hot air in the inner cavity of the spinning shaft is 20L/min. The distance between the traction roller and the spinning hole is 15cm, the length of the spinning channel is 40cm, and the diameter is 4 cm. And then, traction output of the solidified fibers is connected to a twisting and collecting device with controllable speed through a traction roller, the twisting and collecting device is controlled to rotate firstly below the spinning channel, twisting with different twists is carried out on the fibers output by traction, meanwhile, the twisting and collecting device is controlled to rotate secondly, the twisted fibers are collected, and the graphene oxide fibers with certain twist structures are prepared. And the twisting rotating speed of the first rotation is 100r/min, and the linear speed of the second rotation is consistent with the filament outlet speed of the spinning hole.
S3, carrying out chemical reduction on the graphene oxide fibers to obtain graphene fibers. The method specifically comprises the following steps:
and (2) reducing the graphene oxide fibers with different twists in a reducing agent by using hydroiodic acid as the reducing agent at 80 ℃ for 8h, sequentially washing with deionized water and absolute ethyl alcohol for three times respectively, and drying at 60 ℃ to obtain the graphene fibers with a certain twist structure.
Example 2
The invention relates to a preparation method of a twist-controllable graphene fiber, which comprises the following steps:
s1, conveying the graphene oxide spinning solution into the spinning channel from the upper part of the spinning channel at a certain speed, wherein the method specifically comprises the following steps:
a graphene oxide aqueous solution with the concentration of 17mg/ml is prepared by a modified Hummers method, and is stirred at the speed of 500r/min for 36h at the temperature of 60 ℃ to obtain a spinning solution with the concentration of 50 mg/ml. Adding the spinning solution into a spinning container, and spinning the graphene oxide spinning solution into a spinning channel from the upper end of the spinning channel through a spinning hole with the inner diameter of 0.5mm by using a metering pump at the speed of 0.5 ml/h.
S2, in the spinning channel from top to bottom in proper order the spinning solution carries out hot air precuring, traction and twisting, obtains graphene oxide fiber, wherein, the below of spinning channel is provided with twisting collection device, through control twisting collection device' S rotation carries out the twisting of different twists to the fibre after pulling, leads to simultaneously to collect the fibre of twisting, obtains graphene oxide fiber, specifically includes:
after the spinning solution enters a spinning channel through spinning holes of a spinning pipe, hot air is sprayed out from the upper end of the spinning channel into an inner cavity of the spinning channel obliquely towards the spinning solution by using a hot air conveying device, so that the spinning solution is solidified into fibers, and solidified fibers are obtained. The axial included angle between the nozzle of the hot air conveying device and the spinning hole is 45 degrees, the temperature of the hot air is 250 ℃, and the flow of the hot air in the inner cavity of the spinning shaft is 20L/min. The distance between the traction roller and the spinning hole is 15cm, the length of the spinning channel is 40cm, and the diameter is 4 cm. And then, traction output of the solidified fibers is connected to a twisting and collecting device with controllable speed through a traction roller, the twisting and collecting device is controlled to rotate firstly below the spinning channel, twisting with different twists is carried out on the fibers output by traction, meanwhile, the twisting and collecting device is controlled to rotate secondly, the twisted fibers are collected, and the graphene oxide fibers with certain twist structures are prepared. And the twisting rotating speed of the first rotation is 200r/min, and the linear speed of the second rotation is consistent with the filament outlet speed of the spinning hole.
S3, carrying out chemical reduction on the graphene oxide fibers to obtain graphene fibers. The method specifically comprises the following steps:
and (2) reducing the graphene oxide fibers with different twists in a reducing agent by using hydroiodic acid as the reducing agent at 80 ℃ for 8h, sequentially washing with deionized water and absolute ethyl alcohol for three times respectively, and drying at 60 ℃ to obtain the graphene fibers with a certain twist structure.
Example 3
The invention relates to a preparation method of a twist-controllable graphene fiber, which comprises the following steps:
s1, conveying the graphene oxide spinning solution into the spinning channel from the upper part of the spinning channel at a certain speed, wherein the method specifically comprises the following steps:
a graphene oxide aqueous solution with the concentration of 17mg/ml is prepared by a modified Hummers method, and is stirred at the speed of 500r/min for 36h at the temperature of 60 ℃ to obtain a spinning solution with the concentration of 50 mg/ml. Adding the spinning solution into a spinning container, and spinning the graphene oxide spinning solution into a spinning channel from the upper end of the spinning channel through a spinning hole with the inner diameter of 0.7mm by using a metering pump at the speed of 1 ml/h.
S2, in the spinning channel from top to bottom in proper order the spinning solution carries out hot air precuring, traction and twisting, obtains graphene oxide fiber, wherein, the below of spinning channel is provided with twisting collection device, through control twisting collection device' S rotation carries out the twisting of different twists to the fibre after pulling, leads to simultaneously to collect the fibre of twisting, obtains graphene oxide fiber, specifically includes:
after the spinning solution enters the spinning channel through the spinning holes of the spinning pipe, hot air is sprayed out from the upper end of the spinning channel into the inner cavity of the spinning channel obliquely towards the spinning solution by using a hot air conveying device, so that the spinning solution is solidified into fibers. The axial included angle between the nozzle of the hot air conveying device and the spinning hole is 45 degrees, the temperature of the hot air is 300 ℃, and the flow of the hot air in the inner cavity of the spinning channel is 20L/min. The distance between the traction roller and the spinning hole is 15cm, the length of the spinning channel is 40cm, and the diameter is 4 cm. And then, traction output of the solidified fibers is connected to a twisting and collecting device with controllable speed through a traction roller, the twisting and collecting device is controlled to rotate firstly below the spinning channel, twisting with different twists is carried out on the fibers output by traction, meanwhile, the twisting and collecting device is controlled to rotate secondly, the twisted fibers are collected, and the graphene oxide fibers with certain twist structures are prepared. And the twisting rotating speed of the first rotation is 100r/min, and the linear speed of the second rotation is consistent with the filament outlet speed of the spinning hole.
S3, carrying out chemical reduction on the graphene oxide fibers to obtain graphene fibers. The method specifically comprises the following steps:
and (2) reducing the graphene oxide fibers with different twists in a reducing agent by using hydroiodic acid as the reducing agent at 80 ℃ for 8h, sequentially washing with deionized water and absolute ethyl alcohol for three times respectively, and drying at 60 ℃ to obtain the graphene fibers with a certain twist structure.
Example 4
The invention relates to a preparation method of a twist-controllable graphene fiber, which comprises the following steps:
s1, conveying the graphene oxide spinning solution into the spinning channel from the upper part of the spinning channel at a certain speed, wherein the method specifically comprises the following steps:
a graphene oxide aqueous solution with the concentration of 17mg/ml is prepared by a modified Hummers method, and is stirred at the speed of 500r/min for 36h at the temperature of 60 ℃ to obtain a spinning solution with the concentration of 50 mg/ml. Adding the spinning solution into a spinning container, and spinning the graphene oxide spinning solution into a spinning channel from the upper end of the spinning channel through a spinning hole with the inner diameter of 1mm by using a metering pump at the speed of 2 ml/h.
S2, in the spinning channel from top to bottom in proper order the spinning solution carries out hot air precuring, traction and twisting, obtains graphene oxide fiber, wherein, the below of spinning channel is provided with twisting collection device, through control twisting collection device' S rotation carries out the twisting of different twists to the fibre after pulling, leads to simultaneously to collect the fibre of twisting, obtains graphene oxide fiber, specifically includes:
after the spinning solution enters a spinning channel through a spinning hole of a spinning pipe, hot air is blown into an inner cavity of the spinning channel from the upper end of the spinning channel obliquely towards the spinning solution by using a hot air conveying device, so that the spinning solution is solidified into fibers, and solidified fibers are obtained. The axial included angle between the nozzle of the hot air conveying device and the spinning hole is 45 degrees, the temperature of the hot air is 350 ℃, and the flow of the hot air in the inner cavity of the spinning shaft is 20L/min. The distance between the traction roller and the spinning opening is 15cm, the length of the spinning channel is 40cm, and the diameter is 4 cm. And then, traction output of the solidified fibers is connected to a twisting and collecting device with controllable speed through a traction roller, the twisting and collecting device is controlled to rotate firstly below the spinning channel, twisting with different twists is carried out on the fibers output by traction, meanwhile, the twisting and collecting device is controlled to rotate secondly, the twisted fibers are collected, and the graphene oxide fibers with certain twist structures are prepared. And the twisting rotating speed of the first rotation is 300r/min, and the linear speed of the second rotation is consistent with the filament outlet speed of the spinning hole.
S3, carrying out chemical reduction on the graphene oxide fibers to obtain graphene fibers. The method specifically comprises the following steps:
and (2) reducing the graphene oxide fibers with different twists in a reducing agent by using hydroiodic acid as the reducing agent at 80 ℃ for 8h, sequentially washing with deionized water and absolute ethyl alcohol for three times respectively, and drying at 60 ℃ to obtain the graphene fibers with a certain twist structure.
Example 5
The invention relates to a preparation method of a twist-controllable graphene fiber, which comprises the following steps:
s1, conveying the graphene oxide spinning solution into the spinning channel from the upper part of the spinning channel at a certain speed, wherein the method specifically comprises the following steps:
a graphene oxide aqueous solution with the concentration of 17mg/ml is prepared by a modified Hummers method, and is stirred at the speed of 500r/min for 36h at the temperature of 60 ℃ to obtain a spinning solution with the concentration of 50 mg/ml. Adding the spinning solution into a spinning container, and enabling the graphene oxide spinning solution to pass through a spinning hole with the inner diameter of 5mm at the upper end of a spinning channel at the speed of 10ml/h by using a metering pump to be spun into the spinning channel.
S2, in the spinning channel from top to bottom in proper order the spinning solution carries out hot air precuring, traction and twisting, obtains graphene oxide fiber, wherein, the below of spinning channel is provided with twisting collection device, through control twisting collection device' S rotation carries out the twisting of different twists to the fibre after pulling, leads to simultaneously to collect the fibre of twisting, obtains graphene oxide fiber, specifically includes:
after the spinning solution enters a spinning channel through a spinning hole, hot air is sprayed out from the upper end of the spinning channel into an inner cavity of the spinning channel obliquely towards the spinning solution by using a hot air conveying device, so that the spinning solution is solidified into fibers, and solidified fibers are obtained. The axial included angle between the nozzle of the hot air conveying device and the spinning hole is 45 degrees, the temperature of the hot air is 500 ℃, and the flow of the hot air in the inner cavity of the spinning channel is 3L/min. The distance between the traction roller and the spinning hole is 15cm, the length of the spinning channel is 40cm, and the diameter is 4 cm. And then, traction output of the solidified fibers is connected to a twisting and collecting device with controllable speed through a traction roller, the twisting and collecting device is controlled to rotate firstly below the spinning channel, twisting with different twists is carried out on the fibers output by traction, meanwhile, the twisting and collecting device is controlled to rotate secondly, the twisted fibers are collected, and the graphene oxide fibers with certain twist structures are prepared. And the twisting rotating speed of the first rotation is 500r/min, and the linear speed of the second rotation is consistent with the filament outlet speed of the spinning hole.
S3, carrying out chemical reduction on the graphene oxide fibers to obtain graphene fibers. The method specifically comprises the following steps:
and (2) reducing the graphene oxide fibers with different twists in a reducing agent by using hydroiodic acid as the reducing agent at 80 ℃ for 8h, sequentially washing with deionized water and absolute ethyl alcohol for three times respectively, and drying at 60 ℃ to obtain the graphene fibers with a certain twist structure.
Example 6
The invention relates to a preparation method of a twist-controllable graphene fiber, which comprises the following steps:
s1, conveying the graphene oxide spinning solution into the spinning channel from the upper part of the spinning channel at a certain speed, wherein the method specifically comprises the following steps:
a graphene oxide aqueous solution with the concentration of 17mg/ml is prepared by a modified Hummers method, and is stirred at the speed of 500r/min for 36h at the temperature of 60 ℃ to obtain a spinning solution with the concentration of 50 mg/ml. Adding the spinning solution into a spinning container, and enabling the graphene oxide spinning solution to pass through a spinning hole with the inner diameter of 2.5mm at the upper end of a spinning channel at the speed of 5ml/h by using a metering pump to be spun into the spinning channel.
S2, in the spinning channel from top to bottom in proper order the spinning solution carries out hot air precuring, traction and twisting, obtains graphene oxide fiber, wherein, the below of spinning channel is provided with twisting collection device, through control twisting collection device' S rotation carries out the twisting of different twists to the fibre after pulling, leads to simultaneously to collect the fibre of twisting, obtains graphene oxide fiber, specifically includes:
after the spinning solution enters a spinning channel through a spinning hole, hot air is sprayed out from the upper end of the spinning channel into an inner cavity of the spinning channel obliquely towards the spinning solution by using a hot air conveying device, so that the spinning solution is solidified into fibers, and solidified fibers are obtained. The axial included angle between the nozzle of the hot air conveying device and the spinning hole is 45 degrees, the temperature of the hot air is 100 ℃, and the flow of the hot air in the inner cavity of the spinning channel is 50L/min. The distance between the traction roller and the spinning hole is 15cm, the length of the spinning channel is 40cm, and the diameter is 4 cm. And then, the solidified and molded fiber is drawn and output by a drawing roller and is connected to a twisting and collecting device with controllable speed, the twisting and collecting device is controlled to rotate for the first time under the spinning channel, the drawn and output fiber is twisted with different twists, meanwhile, the twisting and collecting device is controlled to rotate for the second time, the twisted fiber is collected, and the graphene oxide fiber with a certain twist structure is prepared. And the twisting rotating speed of the first rotation is 50r/min, and the linear speed of the second rotation is consistent with the filament outlet speed of the spinning hole.
S3, carrying out chemical reduction on the graphene oxide fibers to obtain graphene fibers. The method specifically comprises the following steps:
and (2) reducing the graphene oxide fibers with different twists in a reducing agent by using hydroiodic acid as the reducing agent at 80 ℃ for 8h, sequentially washing with deionized water and absolute ethyl alcohol for three times respectively, and drying at 60 ℃ to obtain the graphene fibers with a certain twist structure.
The properties of the graphene fibers with different twists prepared by the above embodiments are studied and analyzed with reference to fig. 4 to 6. FIGS. 1 and 2 are scanning electron micrographs of the graphene fibers prepared in examples 1 and 2, respectively, and the twists thereof are 130r/10cm and 1000r/10cm, respectively. Due to the totally different twist structure, the fibers have different mechanical properties. Fig. 3 is a stress-strain diagram of the graphene fiber and the untwisted graphene fiber, wherein the elongation at break of the graphene fiber with the twist of 130r/10cm is 15.2%, and the elongation at break of the graphene fiber with the twist of 1000r/10cm is 19.3%, which is greatly increased relative to the untwisted graphene fiber and can be effectively controlled through the twist structure.
The preparation of the macroscopic one-dimensional graphene fiber by using the graphene oxide solution is mainly based on the fact that graphene sheets are stacked in a staggered manner to form a continuous fiber. Therefore, the mechanical properties, electrochemical properties, etc. of the fiber are greatly affected by the size of graphene sheets in the fiber and the degree of compactness of stacking. The size of the graphene sheet has a great relationship with raw materials, an oxidation process and the like, but the densification degree of the sheet layer in fiber forming can be effectively adjusted through a spinning process. In common wet spinning or dry spinning, graphene on the outer surface layer is firstly solidified and formed to form a skin layer, so that the rapid forming of the graphene sheets in the fiber is prevented, the stacking of the graphene sheets in the fiber is influenced, and the overall performance of the fiber is influenced. According to the preparation method, the graphene sheets in the fiber can be rapidly stacked, cured and formed while the outer skin layer is formed by external twisting and extrusion in the fiber spinning forming process. Therefore, the graphene structure finished by the fibers is more compact, and the fiber performance is improved.
In the spinning process, the prepared graphene oxide aqueous solution is concentrated to achieve a spinnable condition, the high-concentration graphene oxide aqueous solution is extruded out from a spinneret orifice by using a metering pump, and graphene oxide sheets are orderly arranged along the flowing direction under the action of fluid flowing in the process that the graphene oxide is extruded from a spinning container to the spinneret orifice, so that the graphene sheets in the formed fiber are orderly arranged along the axial direction of the fiber, and the good mechanical property of the fiber is provided. When the graphene oxide is extruded from the spinning hole, the moisture is quickly volatilized under the action of hot air flow, and the outer surface of the fiber begins to be solidified, so that the fiber is formed. Thus, a certain distance is left between the spinning orifice and the drawing drum, during which distance mainly the outer surface of the fibre is gradually solidified, providing the basic mechanical properties and the outer structure of the fibre, while the fibre still contains a lot of moisture inside. The nascent fiber extruded from the spinning hole is not solidified and has no mechanical performance, so that the drawing speed of the drawing roller and the filament outlet speed of the spinning hole are kept consistent to prevent fiber breakage. After passing through the traction roller, the fibers are subjected to twisting torsional action force, so that moisture in the fibers is forced to diffuse outwards, the drying and forming speed of the whole fibers is accelerated, and meanwhile, due to the extrusion effect, the graphene oxide sheets in the fibers can be tightly stacked, so that the graphene oxide fibers with a certain twist structure are formed. Finally, the fiber is wound and collected by a winding roller on the twisting and collecting device.
According to the invention, in the dry spinning process of the graphene oxide solution, the fiber presents a certain single-fiber twist structure by an auxiliary twisting technical means, and the twist structure regulation of the fiber can be realized, so that the forming speed in the fiber is improved, and the densification degree of the graphene sheet layer is enhanced.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example" or "some examples" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples described in this specification can be combined and combined by one skilled in the art.
While embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that changes, modifications and variations may be made therein by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A preparation method of a twist-controllable graphene fiber is characterized by comprising the following steps:
conveying the graphene oxide spinning solution into a spinning channel from the upper part of the spinning channel at a certain speed;
carrying out hot air solidification, traction and twisting on the spinning solution in turn from top to bottom in a spinning channel to obtain graphene oxide fibers, wherein a twisting collecting device is arranged below the spinning channel, and twisting with different twists is carried out on the drawn fibers by controlling the rotation of the twisting collecting device;
and chemically reducing the graphene oxide fiber to obtain the graphene fiber.
2. The method as claimed in claim 1, wherein the graphene oxide spinning solution is conveyed into the spinning shaft from above the spinning shaft at a certain speed, and the method comprises the following steps:
s11, preparing a graphene oxide aqueous solution by an improved Hummers method, wherein the concentration of the graphene oxide aqueous solution is 5-30 mg/ml;
s12, stirring the graphene oxide aqueous solution at 40-100 ℃ for 12-48 hours to obtain a graphene spinning solution, wherein the stirring speed is 200-1000 r/min, and the concentration of the obtained graphene spinning solution is 40-60 mg/ml;
s13, adding the graphene oxide spinning solution into a spinning container, and spinning the graphene oxide spinning solution into an inner cavity of a spinning channel through a spinning pipe at the upper end of the spinning channel at a certain spinning speed by using a metering pump, wherein a spinning hole is formed at the outlet end of the spinning solution of the spinning pipe, and the inner diameter of the spinning hole is 0.1-5 mm; the spinning speed is 0.1-10 ml/h.
3. The method according to claim 2, wherein the spinning solution is subjected to hot air solidification, drawing and twisting in a spinning shaft from top to bottom in sequence to obtain the graphene oxide fiber, specifically comprising,
s21, blowing hot air from the upper end of the spinning channel into the inner cavity of the spinning channel obliquely towards the spinning solution through a hot air conveying device to solidify the spinning solution, and obtaining solidified fibers, wherein the included angle between the hot air spraying direction of the hot air conveying device and the central axis of a spinning hole is 0-60 degrees, the temperature of the hot air is 100-500 ℃, and the flow rate of the hot air in the inner cavity of the spinning channel is 3-50L/min;
s22, drawing and outputting the solidified fibers through a drawing roller, wherein the central shaft of the drawing roller is vertical to the central shaft of the spinning hole, and the drawing speed of the drawing roller is consistent with the filament outlet speed of the spinning hole;
and S23, carrying out first rotation below the spinning channel by controlling the twisting collecting device, twisting the fibers output by traction in the step S22 with different twists, and simultaneously controlling the twisting collecting device to carry out second rotation to collect the twisted graphene oxide fibers.
4. The method as claimed in claim 3, characterized in that in step S21, the length of the spinning shaft is 30-50 cm and the diameter is 2-5 cm;
in the step S22, the distance between the traction roller and the spinning hole is 10-20 cm;
in step S23, the first rotating twisting speed of the twisting collecting device is 50 to 500r/min, and the second rotating linear speed is consistent with the yarn outlet speed of the spinning hole.
5. The method according to claim 1, wherein the graphene oxide fibers are chemically reduced to obtain graphene fibers, and specifically comprises:
and reducing the graphene oxide fibers with different twists in a reducing agent for 4-10 hours at the temperature of 60-200 ℃, and washing and drying to obtain the graphene fibers with different twists, wherein the reducing agent is one or more of hydriodic acid, hydrazine hydrate, sodium borohydride and ascorbic acid.
6. The method according to any one of claims 1 to 5, characterized in that the preparation device of the method comprises a spinning shaft (5), a spinning tube (10), a metering pump (1), a hot air supply device (3), a traction roller (6) and a twist collection device (8),
the spinning channel is vertically arranged in a cylindrical shape and is provided with an inner cavity (52);
one end of the spinning pipe (10) is communicated with the metering pump, the other end of the spinning pipe forms a spinning hole, the spinning pipe is communicated with the spinning channel (5) from the upper end of the spinning channel through the spinning hole, and the metering pump is configured to spray spinning liquid into an inner cavity of the spinning channel through the spinning hole of the spinning pipe;
the hot air conveying device (3) is arranged on one side of the spinning channel, and is configured to eject hot air from the upper end of the spinning channel obliquely towards the inner cavity of the spinning channel to solidify spinning liquid to form solidified fibers;
the drawing roller (6) is positioned in the spinning shaft inner cavity (52), and is configured to hold and draw downwards to convey solidified fibers;
the twisting collecting device (8) is located below the spinning channel, the free end of the output fiber is supported and drawn by the twisting collecting device and twists around vertical axial rotation to the fiber, and meanwhile, the twisted fiber is wound and collected around horizontal axial rotation by the twisting collecting device.
7. The apparatus according to claim 6, characterized in that it further comprises a spinning container (2) which communicates with a spinning tube, the metering pump being configured to extrude the spinning fluid from the spinning container out of the spinning tube and through a spinning orifice into the spinning shaft interior from above the spinning shaft,
the lower end of the spinning channel is provided with an opening for the twisted fibers to pass through, and the central axis of the spinning channel (5) is superposed with the central axis of the spinning pipe (10);
the hot air conveying device is an air-blast electric heating gun, the air-blast electric heating gun comprises a spray head (31) and a control device (4) electrically connected with the spray head, the spray head obliquely extends into an inner cavity (52) of the spinning duct from the upper part of the spinning duct, the spray head is configured to generate hot air to solidify spinning liquid to obtain solidified fibers under the control of the control device, and the spray head is further configured to control the flow and the temperature of the sprayed hot air under the control of the control device;
the traction roller (6) comprises a first roller (61) and a second roller (62), the first roller and the second roller are arranged in parallel and adjacent to each other, a gap for solidified fibers to pass through is arranged between the first roller and the second roller, and central axes of the first roller and the second roller are respectively vertical to a central axis of the spinning channel;
twisting collection device include revolving stage (81), set up in coiling cylinder (7) on the revolving stage, drive respectively revolving stage and coiling cylinder pivoted drive arrangement and with controller (9) that the drive arrangement electricity is connected, the revolving stage is configured by the drive arrangement drive is twisted around vertical axial rotation to the fibre after pulling, the coiling cylinder is configured by the drive arrangement drive is wound around horizontal axial rotation and is collected twisting's fibre.
8. The apparatus according to claim 7, characterized in that the air-blast electric heating gun further comprises a bracket (11), the nozzle (31) comprises a nozzle (311), a heating device, an air blowing device and a handle (312), the heating device and the air blowing device are both positioned in the handle, the handle is erected on the bracket, one end of the handle is connected with the nozzle, the other end of the handle is electrically connected with a control device, the nozzle obliquely extends into the inner cavity of the spinning shaft from the upper part of the spinning shaft, the heating device is configured to control the temperature of hot air generated by the control device, and the air blowing device is configured to control the flow of the hot air sprayed out by the control device;
the first roller and the second roller are respectively fixed at one end of a fixed shaft (12), the other end of the fixed shaft is connected with a motor, the motor is electrically connected with a controller, the controller controls the motor to rotate, and the motor drives the fixed shaft to drive the first roller and the second roller to rotate;
the twisting collecting device further comprises a translation table arranged on the rotating table, the winding roller is fixed on the translation table, and the translation table is configured and driven by the driving device to perform reciprocating translation so that twisted fibers are distributed on the winding roller.
9. The device according to claim 8, characterized in that the central axis of the nozzle (311) forms an angle of 0 to 60 ° with the central axis of the spinning orifice (51), which coincides with the central axis of the spinning shaft and has an internal diameter of 0.1 to 5 mm;
the length of the spinning channel (5) is 30-50 cm, the diameter of the spinning channel is 2-5 cm, and the distance between the traction roller (6) and the spinning hole (51) is 10-20 cm.
10. The apparatus according to claim 7, characterized in that the spinning vessel (2) is a glass injector, which communicates with the spinning tube, which is a stainless steel metal tube, and the spinning shaft (5) is a quartz tube.
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| CN115094545A (en) * | 2022-07-21 | 2022-09-23 | 苏州大学 | Graphene fiber and preparation method and equipment thereof |
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