CN109056117B - Preparation method of graphene fiber - Google Patents
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- CN109056117B CN109056117B CN201810803618.XA CN201810803618A CN109056117B CN 109056117 B CN109056117 B CN 109056117B CN 201810803618 A CN201810803618 A CN 201810803618A CN 109056117 B CN109056117 B CN 109056117B
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Abstract
The invention provides a preparation method of graphene fibers, which comprises the following steps: and (3) heating the SiC fibers in a vacuum environment and/or an inert gas environment, and keeping the temperature after heating to the decomposition escape temperature of the silicon element to obtain the graphene fibers. The method takes SiC fibers as raw materials, and adopts a simple process to realize continuous industrial preparation of the graphene fibers.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a preparation method of graphene fibers.
Background
Graphene is a two-dimensional material consisting of carbon atoms in sp2 hybrid orbitals and having a two-dimensional hexagonal honeycomb structure. Since graphene has a series of excellent physical properties such as high strength, high thermal conductivity and high electrical conductivity, and has a great application prospect in the field of materials, graphene has become a research hotspot internationally in recent years. However, graphene is insoluble in general solvents, has poor dispersibility, and is not easy to process and use. In order to realize large-scale application of graphene, preparation and application research of graphene macroscopic materials are concerned, and graphene fibers are included in the graphene macroscopic materials. The graphene fiber is a novel fiber with integrated structure and function, has wide application prospect in the fields of flexible super capacitors, fibrous batteries, intelligent sensors, functional fabrics, catalysis and the like, and has huge development potential. At present, the main preparation methods of graphene fibers include a wet spinning method, a hydrothermal method, a thin film twisting method, a chemical vapor deposition method, and the like.
The graphene fiber prepared by the existing wet spinning technology has the advantages of uneven structure, unstable mechanical property and larger discreteness. The graphene fiber prepared by the existing hydrothermal method is limited by the length of a capillary tube and is not suitable for continuous large-scale preparation of the graphene fiber. The graphene fiber prepared by the existing film twisting method has many structural defects. In the three methods, graphene oxide is used as a raw material, harsh conditions such as strong acid and strong alkali are required in the preparation process, the method is not environment-friendly, the formed graphene oxide fiber needs to be reduced, the operation steps are multiple and complicated, and oxygen-containing functional groups are difficult to completely remove. The existing chemical vapor deposition method is difficult to realize continuous preparation of graphene fibers, the transfer process is complex, the operation difficulty is high, and large-scale preparation is also difficult to form.
At present, the research on the graphene fiber is still in a starting stage, the continuous and large-scale preparation of the graphene fiber is difficult to realize, and the application and development of the graphene fiber are greatly limited, so that the development of a production method capable of realizing mass production of the high-quality continuous graphene fiber is urgently needed.
Disclosure of Invention
The invention aims to provide a preparation method of graphene fibers, and solves the technical problems that in the preparation process of graphene fibers in the prior art, the process steps are multiple, strong acid and strong alkali are needed, the environment friendliness is poor, impurities are introduced into the fibers, and the morphology of the graphene fibers is difficult to control.
The invention provides a preparation method of graphene fibers, which comprises the following steps: and (3) heating the SiC fibers in a vacuum environment and/or an inert gas environment, and keeping the temperature after heating to the decomposition escape temperature of the silicon element to obtain the graphene fibers.
The SiC fibers in the invention comprise all the first generation, second generation and third generation SiC fibers which are commercially available, and also comprise other SiC fibers prepared by a precursor conversion method and SiC fibers doped with heteroatoms such as iron, silver, aluminum, hafnium, tantalum, boron, zirconium, nickel, manganese, gold, copper, titanium and the like, and SiC fiber felts, SiC nanowires and the like prepared by other methods. The decomposition and escape temperature of silicon element in the present specification means a temperature at which SiC in the SiC fiber starts to decompose, resulting in escape of silicon element. The SiC fibers used herein may be of continuous or discontinuous structure.
According to the method provided by the invention, the SiC fiber is heated and insulated, so that the silicon element in the SiC fiber is decomposed and escaped, and the residual carbon in the fiber is reassembled to form a two-dimensional carbon structure, thereby obtaining the graphene fiber. The method is simple and easy to operate, environment-friendly, does not need strong acid and strong alkali conditions, fully utilizes the structure of the formed continuous silicon carbide fiber, enables the prepared graphene fiber to be uniform in structure, stable in mechanical property and small in discreteness, does not need reduction and other operations on the fiber, and simplifies the operation flow. The method is not limited by the structure or length of the preparation container, and continuous large-scale production of the graphene fiber can be realized. The continuous silicon carbide fiber is used as a raw material, the oxygen content is low, and the adverse effect of residual oxygen-containing functional groups on the performance of the graphene fiber is avoided. The method provided by the invention can realize the temperature for silicon in the silicon carbide fiber to escape. The graphene fiber obtained in the invention is a fiber structure comprising a graphene fiber layer, and can be a composite fiber structure in which the whole fiber is made of graphene material or a graphene layer is only coated outside a fiber core layer. Specifically, the graphene fiber includes a fiber composed of graphene; the graphene/silicon carbide composite fiber also comprises graphene/silicon carbide composite fibers which take silicon carbide as a core and form a graphene layer on the outer wall of the core.
By continuous silicon carbide fiber is meant herein a continuous unbroken, complete silicon carbide fiber having a length of more than 100 m.
Further, the temperature is increased to 1500-2500 ℃ according to the temperature increase rate of 100-900 ℃/hour.
The heating step is carried out under the condition, so that the defect of excessive structures in the obtained graphene can be avoided, the mechanical property of the obtained graphene fiber is improved, the preparation efficiency of the graphene fiber is improved, and the silicon element can escape and the graphene can be formed.
Further, the vacuum degree of the vacuum environment is less than 1.0 multiplied by 103Pa. The steps of temperature rise and heat preservation are carried out under the condition, so that the escape speed of silicon element in the continuous SiC fiber can be increased, and the preparation efficiency is improved. In the vacuum degree range, the silicon element of the SiC fiber can be better removed, thereby being beneficial to the formation of graphene. Vacuum degree less than 1.0 × 103The atmosphere of Pa means an atmosphere in which the degree of vacuum in the atmosphere is kept lower than the degree of vacuum by continuously or intermittently evacuating during the test.
Further, the inert gas is one or more of nitrogen, argon or helium. Specifically, the inert gas atmosphere is an atmosphere formed by filling the reaction space with the inert gas.
Further, the temperature rise rate in the temperature rise step is 300-600 ℃/h. The upper limit of this range may also be 550 ℃/hour; 400 ℃/hour; 500 deg.C/hour.
Further, in the temperature rising step, the temperature rises to 1700-2200 ℃. The upper limit of the range may be 1900 ℃ or 2000 ℃; the lower limit of the range may be 1800 ℃ or 2000 ℃.
Further, the heat preservation step is to preserve the heat of the continuous SiC fibers for 0.5 to 30 hours at the temperature after the temperature rise step.
Further, the heat preservation step is to preserve the heat of the continuous SiC fibers for 1-20 hours at the temperature after the temperature rise step. The upper limit of the range may be 8 hours or 10 hours.
The invention also provides a graphene fiber prepared by the method, wherein the continuous graphene fiber has the tensile strength of more than 200MPa, the modulus of more than 20GPa and the density of more than 1.2g/cm3。
The graphene fibers obtained may be continuous or discontinuous fibers. When a bundle of continuous graphene fibers is prepared, the continuous graphene fibers are continuous in length and free from breakage, and the total length can reach more than 100 m.
The graphene/silicon carbide composite fiber prepared by the method comprises silicon carbide fibers and a graphene layer coated on the outer surfaces of the silicon carbide fibers, wherein the thickness of the graphene layer is 0.001-0.5 times of the diameter of the graphene/silicon carbide composite fiber.
The decomposition and escape degree of the silicon element in the silicon carbide fiber can be controlled by controlling the heat preservation time and the temperature rise in the temperature rise step, so that the fiber material with the composite structure is prepared. The obtained graphene/silicon carbide composite fiber is continuous in length, and the length of one bundle of fiber can reach more than 100m without fracture.
Further, the tensile strength of the continuous graphene/silicon carbide composite fiber is more than 500MPa, the modulus is more than 150GPa, and the density is more than 1.5g/cm3And continuous large-scale preparation can be realized.
The method comprises the following steps:
and (3) placing the SiC fibers in a graphite furnace, heating to 1500-2500 ℃ in a vacuum environment and/or an inert gas environment according to a heating rate of 100-900 ℃/hour, and then preserving heat for 0.5-30 hours to obtain the graphene fibers.
Compared with the prior art, the invention has the technical effects that:
1. the preparation method of the graphene fiber provided by the invention can obtain the graphene fiber with the purity of more than 99%, has the advantages of simple process, convenient operation and high preparation efficiency, does not need solvent reagents such as strong acid and strong alkali, does not need complicated procedures such as reduction, washing and drying, and is environment-friendly.
2. According to the preparation method of the graphene fiber, continuous SiC fibers which are already industrially produced are used as raw materials, the raw materials are wide in source, the process is simple, and continuous and large-scale preparation of the graphene fibers can be realized.
3. The preparation method of the graphene fiber provided by the invention is wide in application range, and the graphene product with the corresponding form can be prepared by adopting SiC raw materials with different forms such as continuous SiC fibers, SiC nano fibers, two-dimensional SiC fiber felt/cloth, SiC nano wires and the like.
4. According to the graphene fiber provided by the invention, the obtained graphene fiber can keep the shape of the silicon carbide fiber as an initial raw material, so that the graphene fiber with a circular, trilobal, pentalobal, strip-shaped or hollow cross section and other different shapes can be prepared, and the surface of the fiber is smooth, uniform and complete, thereby ensuring that the graphene fiber has good flexibility, mechanical strength and conductivity.
5. According to the continuous graphene/silicon carbide composite fiber provided by the invention, the outer layer is uniformly distributed graphene, the core part is silicon carbide, and the relative thicknesses of the graphene and the silicon carbide in the fiber can be regulated and controlled by changing preparation conditions such as vacuum degree, temperature and heat preservation time.
The above and other aspects of the present invention will become apparent from the following description of various embodiments, which is set forth in particular with reference to a method of preparing graphene fibers according to the present invention.
Drawings
FIG. 1 is an X-ray diffraction pattern of a third generation continuous SiC fiber used in preferred embodiment 1 of the present invention;
FIG. 2 is a sectional scanning electron micrograph of a third generation continuous SiC fiber used in preferred embodiment 1 of the present invention;
fig. 3 is an X-ray diffraction spectrum of the graphene fiber prepared in preferred embodiment 1 of the present invention;
fig. 4 is a raman spectrum of the graphene fiber prepared in preferred embodiment 1 of the present invention;
fig. 5 is a cross-sectional scanning electron micrograph of the graphene fiber prepared in preferred embodiment 1 of the present invention;
fig. 6 is a surface scanning electron micrograph of the graphene fiber prepared in preferred embodiment 1 of the present invention.
Fig. 7 is a cross-sectional scanning electron micrograph of the continuous graphene/silicon carbide composite fiber prepared in preferred embodiment 2 of the present invention;
fig. 8 is a scanning electron micrograph of the surface of the continuous graphene/silicon carbide composite fiber prepared in preferred embodiment 2 of the present invention.
Detailed Description
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention.
Examples
Unless otherwise specified, the raw materials in the examples of the present invention were purchased commercially, in which the tensile strength and modulus of the fibers were measured using an M350-5CT universal tester manufactured by Testometric, UK, and the original length of the fiber tensile was 25mm, and the strength and modulus of 10 or more fibers were measured and averaged.
The density of the fibers is measured by liquid displacement or sink-and-float methods.
Example 1 continuous graphene fiber 1#Preparation method of (1)
Third-generation continuous SiC fibers (in this example, the third-generation continuous SiC fibers had a fiber diameter of 10.3 μm, a tensile strength of 1820MPa, a modulus of 331GPa, and a density of 2.95g/cm3) Placing the graphene fiber in a graphite furnace, continuously vacuumizing until the vacuum degree is less than 30Pa, heating to 1800 ℃ according to the heating rate of 600 ℃/h, and then preserving heat for 10 h to obtain the continuous graphene fiber 1#. The resulting continuous graphene fiber 1#Has a tensile strength of 375MPa, a modulus of 34GPa and a density of 1.60g/cm3。
FIG. 1 is an X-ray diffraction pattern of a third-generation continuous SiC fiber used in preferred embodiment 1 of the present invention, in which peaks at diffraction angles of 35.6,41.4,60.0,71.8 and 75.5 degrees correspond to (111), (200), (220), (311) and (222) crystal planes of 3C-SiC crystal grains, respectively. Fig. 2 is a cross-sectional scanning electron micrograph of a third generation continuous SiC fiber used in preferred embodiment 1 of the present invention. It can be seen that the fiber is composed of 3C-SiC, and has a high degree of crystallinity, a dense fiber cross section, and distinct SiC grains can be seen.
Fig. 3 is an X-ray diffraction pattern of the graphene fiber prepared in preferred embodiment 1 of the present invention, in which the diffraction peak of only one carbon indicates that the SiC crystal grains in the raw material are completely converted into carbon without other impurities. Fig. 4 is a raman spectrum of the graphene fiber prepared in preferred embodiment 1 of the present invention, and typical D, G and 2D peaks of graphene can be seen, which proves that carbon exists in the graphene fiber prepared by the method provided by the present invention in the form of graphene. From this, it was found that the SiC fiber was completely converted into the graphene fiber. Fig. 5 is a cross-sectional scanning electron microscope photograph of the continuous graphene fiber prepared in preferred embodiment 1 of the present invention, and fig. 6 is a surface scanning electron microscope photograph of the continuous graphene fiber prepared in preferred embodiment 1 of the present invention. As can be seen from fig. 5 to 6, the graphene fiber has a complete morphology, a smooth, uniform and complete surface, no protrusions or other special-shaped structures, and a circular cross section with the morphology of the raw material SiC fiber well maintained.
Example 2 continuous graphene/silicon carbide composite fiber 1#Preparation method of (1)
Third-generation continuous SiC fibers (in this example, the third-generation continuous SiC fibers had a fiber diameter of 10.3 μm, a tensile strength of 1820MPa, a modulus of 331GPa, and a density of 2.95g/cm3) Placing in a graphite furnace, vacuumizing to vacuum degreeHeating to 1800 ℃ at a heating rate of 300 ℃/h for 1 h under the pressure of less than 1Pa to obtain the continuous graphene/silicon carbide composite fiber 1#The fiber has a tensile strength of 622MPa, a modulus of 195GPa and a density of 2.49g/cm3。
Fig. 7 is a cross-sectional scanning electron microscope photograph of the continuous graphene/silicon carbide composite fiber prepared in preferred embodiment 2 of the present invention, and fig. 8 is a surface scanning electron microscope photograph of the continuous graphene/silicon carbide composite fiber prepared in preferred embodiment 2 of the present invention. The figure shows that the fiber has complete appearance, smooth, uniform and complete surface, no protrusion or other special-shaped structures, circular cross section, obvious boundary between the graphene layer and the silicon carbide at the cross section, wherein the outer layer is graphene, and the core part is sintered silicon carbide.
Example 3 continuous graphene fiber 2#Preparation method of (1)
Third-generation continuous SiC fibers (in this example, the third-generation continuous SiC fibers had a fiber diameter of 10.3 μm, a tensile strength of 1820MPa, a modulus of 331GPa, and a density of 2.95g/cm3) Placing the graphene fiber in a graphite furnace, vacuumizing until the vacuum degree is less than 1000Pa, heating to 1800 ℃ according to the heating rate of 400 ℃/h, and then preserving heat for 8 h to obtain the continuous graphene fiber 2#. The fiber has a tensile strength of 473MPa, a modulus of 45GPa and a density of 1.61g/cm3。
Example 4 continuous graphene fiber 3#Preparation method of (1)
Third-generation continuous SiC fibers (in this example, the third-generation continuous SiC fibers had a fiber diameter of 10.3 μm, a tensile strength of 1820MPa, a modulus of 331GPa, and a density of 2.95g/cm3) Placing the graphene fiber in a graphite furnace, vacuumizing until the vacuum degree is less than 10Pa, heating to 2200 ℃ according to the heating rate of 500 ℃/h, and then preserving heat for 0.5 h to obtain the continuous graphene fiber 3#The fiber has a tensile strength of 322MPa, a modulus of 30GPa and a density of 1.60g/cm3。
Example 5 continuous graphene/silicon carbide composite fiber 2#Preparation method of (1)
Second generation continuous SiC fibers (of the second generation continuous SiC fibers in the present embodiment)The fiber diameter is 11.2 μm, the tensile strength is 2880MPa, the modulus is 281GPa, and the density is 2.72g/cm3) Placing the composite fiber in a graphite furnace, vacuumizing the graphite furnace until the vacuum degree is less than 500Pa, heating the composite fiber to 1900 ℃ according to the heating rate of 600 ℃/h, and then preserving the heat for 1 h to obtain the continuous graphene/silicon carbide composite fiber 2#. The fiber has a tensile strength of 568MPa, a modulus of 163GPa and a density of 2.12g/cm3。
Example 6 continuous graphene/silicon carbide composite fiber 3#Preparation method of (1)
Second-generation continuous SiC fibers (in this example, the second-generation continuous SiC fibers had a fiber diameter of 11.2 μm, a tensile strength of 2880MPa, a modulus of 281GPa, and a density of 2.72g/cm3) Placing the composite fiber in a graphite furnace, vacuumizing the graphite furnace until the vacuum degree is less than 5Pa, heating the composite fiber to 1700 ℃ according to the heating rate of 550 ℃/h, and then preserving the heat for 20 h to obtain the continuous graphene/silicon carbide composite fiber 3#. The tensile strength of the fiber is 1360MPa, the modulus is 205GPa, and the density is 2.41g/cm3。
See Table 1 for experimental parameters in examples 1-6.
TABLE 1
The fiber performance results obtained in examples 1-6 are shown in Table 2:
TABLE 2
Example 7 continuous graphene fiber 4#Preparation method of (1)
The difference from example 1 is that: the temperature rise step is to raise the temperature to 2200 ℃ according to the temperature rise rate of 900 ℃/hour and keep the temperature for 30 hours. Heating step in vacuum and inert gas environmentThe inert gas is nitrogen, and the vacuum degree is less than 100 Pa. Obtaining the continuous graphene fiber 4#。
Example 8 continuous graphene/silicon carbide composite fiber 4#Preparation method of (1)
The difference from example 1 is that: the temperature rise step is to raise the temperature to 1500 ℃ according to the temperature rise rate of 100 ℃/hour. Obtaining the continuous graphene/silicon carbide composite fiber 4#。
Example 9 continuous graphene fiber 5#Preparation method of (1)
The difference from example 1 is that: in the temperature rising step, the temperature is raised to 2500 ℃. The temperature raising step is carried out in an inert gas environment, and the inert gas is argon. Obtaining the continuous graphene fiber 5#。
From examples 1 to 6, the graphene fiber can be simply and conveniently prepared by the method provided by the invention only by heating and insulating, the length of the graphite fiber tow can reach more than 100m without breaking, and all performances are better.
It will be clear to a person skilled in the art that the scope of the present invention is not limited to the examples discussed in the foregoing, but that several amendments and modifications thereof are possible without deviating from the scope of the present invention as defined in the attached claims. While the invention has been illustrated and described in detail in the drawings and the description, such illustration and description are to be considered illustrative or exemplary only, and not restrictive. The invention is not limited to the disclosed embodiments.
Variations to the disclosed embodiments can be understood and effected by those skilled in the art in practicing the claimed invention, from a study of the drawings, the disclosure, and the appended claims. In the claims, the term "comprising" does not exclude other steps or elements, and the indefinite article "a" or "an" does not exclude a plurality. The mere fact that certain measures are recited in mutually different dependent claims does not indicate that a combination of these measures cannot be used to advantage. Any reference signs in the claims shall not be construed as limiting the scope of the invention.
The above description is only for the purpose of illustrating the present invention and is not intended to limit the present invention in any way, and the present invention is not limited to the above description, but rather should be construed as being limited to the scope of the present invention.
Claims (5)
1. A preparation method of graphene fibers is characterized by comprising the following steps: heating the SiC fibers in a vacuum environment and/or an inert gas environment, and keeping the temperature after the temperature is raised to the temperature at which the silicon element is decomposed and escapes to obtain the graphene fibers;
the temperature rise step is to raise the temperature to 2000-2500 ℃ according to the temperature rise rate of 500-600 ℃/hour.
2. The method for preparing graphene fiber according to claim 1, wherein the vacuum degree of the vacuum environment is less than 1.0 x 103Pa。
3. The method for producing a graphene fiber according to claim 1, wherein the heat-retaining step is to retain the SiC fiber at the temperature after the temperature rise for 0.5 to 30 hours after the temperature rise step.
4. The method for producing a graphene fiber according to claim 1, wherein the heat-retaining step is to retain the SiC fiber at the temperature after the temperature rise for 1 to 20 hours after the temperature rise step.
5. The graphene fiber prepared by the method of any one of claims 1 to 4, wherein the graphene fiber has a tensile strength of more than 200MPa, a modulus of more than 20GPa, and a density of more than 1.2g/cm3。
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| CN104310372A (en) * | 2014-09-30 | 2015-01-28 | 张映波 | Method for directly growing carbon nano tube array on fiber substrate |
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| CN102256914A (en) * | 2008-12-16 | 2011-11-23 | 斯奈克玛动力部件公司 | Method for processing ceramic fibres |
| WO2014114874A1 (en) * | 2013-01-22 | 2014-07-31 | Herakles | Method of creating a carbon interface on silicon carbide fibres under hydrothermal conditions |
| CN103160955B (en) * | 2013-03-18 | 2014-09-17 | 中国人民解放军国防科学技术大学 | Preparation method of continuous SiC fiber having surface carbon-rich structure |
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