CN107540245B - In-situ direct preparation method of graphene optical fiber - Google Patents
In-situ direct preparation method of graphene optical fiber Download PDFInfo
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Abstract
The invention discloses an in-situ direct preparation method of a graphene optical fiber. The method comprises the following steps: 1) installing chemical vapor deposition equipment on an optical fiber drawing machine, placing a bare optical fiber drawn by the drawing machine in the equipment cavity, and heating to 500-1700 ℃ under the protection of inert atmosphere; 2) keeping the temperature in the step 1) constant, introducing a carbon source and hydrogen into the equipment cavity in the step 1) to perform chemical vapor deposition reaction, closing the carbon source after the reaction is finished, and quickly cooling to room temperature to obtain the graphene optical fiber. The graphene optical fiber prepared by the invention has the characteristics of high graphene crystallinity, uniform distribution, controllable layer number, high coverage rate and the like, has the advantages of high conductivity, saturable absorption, low energy loss and the like compared with the traditional optical fiber, is simple in preparation process, is compatible with the traditional optical fiber production process, is suitable for industrial continuous production, and has wide application prospects in the fields of high-speed optical communication, optical modulators, biosensors, intelligent wearable equipment and the like.
Description
Technical Field
The invention belongs to the field of optical fiber materials, and particularly relates to a method for directly preparing a graphene optical fiber in situ.
Background
Optical fibers are an important nonlinear optical medium, and the structures of the optical fibers are various. The laser has strong optical confinement capability, and can flexibly regulate and control a laser mode through different structural designs. Due to the advantages of wide frequency band, low loss, long working distance and the like, the optical fiber becomes a core basic device in modern optical communication, photoelectric interconnection, optical sensing and optical computing systems. With the development of the optical fiber laser technology, the nonlinear optical crystal with high nonlinear coefficient, high optical damage threshold and low loss combined with the optical fiber gradually becomes an important material applied to modern optical fiber communication, and has received extensive attention of researchers.
Graphene is a two-dimensional atomic crystal material with carbon atoms arranged in a hexagonal symmetric and periodic manner, and shows very excellent optical, electrical and thermal properties, such as nonlinear polarizability of 10-7esu, approximately 5 orders of magnitude higher than the silicon material; the mobility is as high as 2 x 105cm2v-1s-1100 times as much as silicon; resistivity as low as 10-8Ω · m, lower than copper; the transmittance is as high as 97.7%; the thermal conductivity reaches 5000Wm-1K-1. As an excellent saturable absorber, graphene has the advantages of wide waveband, ultra-fast response, controllable modulation depth, low saturable absorption intensity and the likeThe point can be used for mode-locked or Q-switched pulse lasers; as a good nonlinear optical medium, graphene has a very high third-order nonlinear coefficient, and can be used for a four-wave mixing wavelength conversion technology in optical fiber communication. These unusual characteristics of graphene open up a wide space for developing new nonlinear optical composite materials and optoelectronic functional devices, and will certainly bring great interest in science and technology and the industry.
The construction method of the graphene and optical fiber composite structure at present comprises the following two methods: (1) the graphene dispersion liquid is prepared by a chemical stripping method, and then the graphene dispersion liquid is directly coated on the surface of an optical fiber (ACS Nano 2010,4,803; Opt.express 2013,21,16763). The graphene used in the method has poor quality, uneven coating and low coverage, and has oxygen-containing functional groups or chemical residues, so that the optical fiber has high absorption and scattering loss. (2) Firstly, a graphene film is grown on a metal substrate of copper, nickel and the like by a chemical vapor deposition method, and then the graphene film is transferred to the surface of an optical fiber (adv. funct. mater.2009,19,3077; phys. rev. lett.2010,105, 097401; Nature photo.2011, 5,411). The method relates to the technologies of metal substrate corrosion, transfer medium removal and the like, and is complex in process, unsatisfactory in graphene coating effect and difficult to prepare on a large scale. In addition, most of the traditional chemical vapor deposition methods uniformly grow graphene on a two-dimensional plane open structure, and direct uniform growth and complete coverage of graphene on special structural materials such as three-dimensional porous and semi-closed optical fibers are difficult to realize. Therefore, how to prepare high-performance graphene optical fibers is a common difficulty in the field.
Disclosure of Invention
The invention aims to provide an in-situ direct preparation method of a graphene optical fiber. Compared with the conventional graphene coated optical fiber, the graphene optical fiber prepared by the invention adopts a one-step method to directly grow graphene in situ, has the characteristics of high graphene crystallinity, complete coverage, uniform distribution, controllable growth layer number and the like, is simple in preparation process, is compatible with the conventional optical fiber production process, and is suitable for industrial continuous production. Furthermore, the growth method provided by the invention overcomes the limitation that the traditional chemical vapor deposition process is difficult to completely and uniformly cover the graphene film on the non-planar structure, and can uniformly grow graphene on the curved surface and the inner hole wall of the optical fiber by adopting the strategies of low-pressure and low-carbon source flow control and long-time growth, so that the graphene optical fiber material completely and uniformly covered is prepared in situ.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
an in-situ direct preparation method of a graphene optical fiber comprises the following steps:
1) installing chemical vapor deposition equipment on an optical fiber drawing machine, placing a bare optical fiber drawn by the drawing machine in a cavity of the chemical vapor deposition equipment, and heating to 500-1700 ℃ under the protection of inert atmosphere;
2) keeping the temperature in the step 1) constant, introducing a carbon source and hydrogen into the equipment cavity in the step 1) to perform chemical vapor deposition reaction, closing the carbon source after the reaction is finished, and quickly cooling to room temperature to obtain the graphene optical fiber.
In the step 1) of the method, the bare fiber obtained by the wire drawing method is selected from at least one of a porous fiber, a micro-nano fiber, a D-type fiber and a conventional fiber; wherein the optical fiber is made of any one of quartz and mixed fluoride;
the chemical vapor deposition equipment is any one of hot wall chemical vapor deposition equipment, cold wall chemical vapor deposition equipment and plasma enhanced chemical vapor deposition equipment;
the inert atmosphere is argon or a hydrogen-argon mixed gas containing 5% of hydrogen by volume fraction;
in the temperature raising step, the temperature is 500-1700 ℃.
In step 2) of the above method, the carbon source is methane, ethylene, propylene, acetylene or ethanol;
in the chemical vapor deposition reaction step, the volume ratio of the carbon source gas to the hydrogen gas is 1-5: 5; specifically, it may be 1.5: 5 or 2: 5 or 3: 5 or 5: 5.
the reaction time is 30 minutes to 120 minutes, and specifically can be 30 minutes, 60 minutes or 120 minutes;
the reaction temperature may be specifically 500 ℃ or 700 ℃ or 1000 ℃ or 1100 ℃ or 1700 ℃;
the chemical vapor deposition reaction pressure is 200-1.01 multiplied by 105The pressure may be 200 Pa, 1000 Pa or normal pressure.
In the step 2), the obtained graphene optical fiber is of a composite structure of graphene grown in situ on a bare optical fiber;
the inner surface and the outer surface of the bare optical fiber are both covered with continuous graphene films, and the coverage degree is 100%;
the graphene in the graphene optical fiber is uniform in thickness, and 1-10 layers of graphene are adjustable;
the surface of the graphene does not contain oxygen-rich functional groups and metal impurity residues.
The preparation method of the graphene optical fiber provided by the invention has the advantages of controllable process and high efficiency, and is one of ideal ways for preparing the graphene optical fiber in situ by one-step method. Compared with the traditional optical fiber, the prepared graphene optical fiber has the characteristics of high conductivity, saturable absorption and the like, is low in energy loss and adjustable in nonlinear optical characteristics, and can be used in the fields of high-speed optical communication, optical modulators, biosensors, intelligent wearable equipment and the like.
Drawings
Fig. 1 is a schematic structural diagram of in-situ direct preparation of a graphene photonic crystal fiber according to embodiment 1 of the present invention;
FIG. 2 is a photograph of an optical transmission microscope for in-situ direct preparation of graphene photonic crystal fibers according to example 1 of the present invention;
FIG. 3 is a scanning electron microscope photograph of in-situ directly prepared graphene photonic crystal fiber according to example 1 of the present invention;
FIG. 4 is a scanning electron microscope photograph of a cross section of a graphene photonic crystal fiber prepared directly in situ in example 1 of the present invention;
fig. 5 is a raman spectrum of graphene with different thicknesses prepared directly in situ for a graphene photonic crystal fiber according to example 1 of the present invention;
fig. 6 is a schematic structural diagram of in-situ direct preparation of a graphene micro-nano solid fiber in embodiment 2 of the present invention;
FIG. 7 is a scanning electron microscope photograph of in-situ directly prepared graphene micro-nano solid-core optical fibers in embodiment 2 of the present invention;
fig. 8 is a raman spectrogram of a graphene micro-nano solid-core optical fiber directly prepared in situ in embodiment 2 of the present invention.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are conventional unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Example 1 in-situ direct preparation of graphene photonic crystal fibers
1) Installing high-temperature tube furnace equipment on an optical fiber drawing machine, placing a bare photonic crystal quartz optical fiber obtained by a drawing method in a high-temperature tube furnace, and heating to 1100 ℃ under the protection of argon;
2) keeping the temperature constant, introducing methane and hydrogen into the tubular furnace to perform chemical vapor deposition reaction, wherein the volume ratio of the methane to the hydrogen is 1.5: 5,2: 5 and 3: 5, the reaction time is 120 minutes, the reaction pressure is 1.01X 105And (6) handkerchief.
3) And after the reaction is finished, closing methane gas and rapidly cooling to room temperature to obtain the graphene photonic crystal fiber, wherein the structural schematic diagram is shown in figure 1, and the physical appearance of the optical transmission microscope is shown in figure 2. As can be seen from fig. 2, the surface contrast of the optical fiber is uniform, the thickness is uniform, and the vertical transmittance of the optical fiber after growth becomes low.
The graphene optical fiber obtained in the embodiment is an in-situ composite structure of the photonic crystal optical fiber and graphene, and the inner surface and the outer surface of the bare optical fiber are both covered with continuous graphene films, wherein the coverage degree is 100%. The coated graphene is adjustable from single-layer to multi-layer and has uniform thickness, the electron microscopic appearances of the outer surface and the section of the coated graphene are respectively shown in fig. 3(a is a photonic crystal fiber, and b is a graphene photonic crystal fiber) and fig. 4(a is the section appearance of the graphene photonic crystal fiber, and b is the graphene appearance at the section of the graphene photonic crystal fiber), and the raman spectrums of the coated graphene with different thicknesses are shown in fig. 5. The graphene optical fiber in this embodiment has a sheet resistance in the range of about 500-3000 ohms/square, as tested. From the result, the graphene layer has the advantages of good crystallinity, controllable layer number, uniform distribution, no surface group and no metal impurity residue, high conductivity and better comprehensive quality than the reduced graphene oxide coated optical fiber.
Example 2 in-situ direct preparation of graphene micro-nano solid-core optical fiber
1) Installing high-temperature tube furnace equipment on an optical fiber drawing machine, placing the micro-nano solid-core quartz optical fiber obtained by a drawing method in a high-temperature tube furnace, and heating to 700 ℃ under the protection of hydrogen and argon mixed gas;
2) keeping the temperature constant, and introducing propylene and hydrogen into the tubular furnace to perform chemical vapor deposition reaction, wherein the volume ratio of the propylene to the hydrogen is 4: 5, the reaction time is 60 minutes, and the reaction pressure is 1.01X 105And (6) handkerchief.
3) And after the reaction is finished, closing the propylene gas and quickly cooling to room temperature to obtain the graphene micro-nano optical fiber, wherein the structural schematic diagram is shown in fig. 6.
The graphene optical fiber obtained in the embodiment is of an in-situ composite structure of the micro-nano optical fiber and graphene, the outer surface of the bare optical fiber is covered with a continuous graphene film, and the coverage degree is 100%. The coated graphene is adjustable from single-layer to multi-layer and has uniform thickness, the scanning electron microscopic morphology of the outer surface of the coated graphene is shown in fig. 7, and the raman spectra of the coated graphene with different thicknesses are shown in fig. 8. From the results, the comprehensive quality of the graphene optical fiber is superior to that of the reduced graphene oxide coated optical fiber.
Example 3 in-situ direct preparation of graphene D-type optical fiber
1) Installing high-temperature tube furnace equipment on an optical fiber drawing machine, placing a D-type quartz optical fiber obtained by a drawing method in a high-temperature tube furnace, and heating to 1700 ℃ under the protection of argon;
2) keeping the temperature constant, introducing methane and hydrogen into the tubular furnace to perform chemical vapor deposition reaction, wherein the volume ratio of the methane to the hydrogen is 1: 5, the reaction time is 60 minutes, and the reaction pressure is 1.01X 105And (6) handkerchief.
3) And after the reaction is finished, closing methane gas and quickly cooling to room temperature to obtain the graphene D-type optical fiber.
The graphene optical fiber obtained in the embodiment is of an in-situ composite structure of a D-type quartz optical fiber and graphene, and the outer surface of the bare optical fiber is covered with a continuous graphene film, wherein the coverage degree is 100%.
Example 4 in-situ direct preparation of graphene fluoride Photonic Crystal fibers
1) Installing high-temperature tube furnace equipment on an optical fiber drawing machine, placing a bare photonic crystal fluoride optical fiber obtained by a drawing method in a high-temperature tube furnace, and heating to 1000 ℃ under the protection of argon;
2) keeping the temperature constant, introducing ethylene and hydrogen into the tubular furnace to perform chemical vapor deposition reaction, wherein the volume ratio of the ethylene to the hydrogen is 5: 5, the reaction time is 30 minutes, and the reaction pressure is 1000 Pa.
3) And after the reaction is finished, closing the ethylene gas and quickly cooling to room temperature to obtain the graphene fluoride photonic crystal fiber.
Example 5 in-situ direct preparation of graphene Photonic Crystal fibers
1) Installing a plasma enhanced chemical vapor deposition system on an optical fiber drawing machine, placing a bare photonic crystal quartz optical fiber obtained by a drawing method in the plasma enhanced chemical vapor deposition system, and heating to 500 ℃ under the protection of argon;
2) keeping the temperature constant, introducing methane and hydrogen into a reaction cavity of the deposition system to perform plasma enhanced chemical vapor deposition reaction, wherein the volume ratio of the methane to the hydrogen is 1.5: 5, the reaction time is 60 minutes, and the reaction pressure is 200 Pa.
3) And after the reaction is finished, closing the methane and the hydrogen and quickly cooling to room temperature to obtain the graphene photonic crystal fiber.
The graphene optical fiber obtained in the embodiment is an in-situ composite structure of the photonic crystal quartz optical fiber and graphene, and the outer surface of the bare optical fiber is covered with a continuous graphene film, wherein the coverage degree is 100%.
Example 6 in-situ direct preparation of graphene photonic crystal fibers
1) Installing a cold-wall chemical vapor deposition system on an optical fiber drawing machine, placing a bare photonic crystal quartz optical fiber obtained by a drawing method in the cold-wall chemical vapor deposition system, and heating to 1000 ℃ under a hydrogen-argon mixed atmosphere containing 5% of hydrogen;
2) keeping the temperature constant, introducing anhydrous ethanol gas and hydrogen into a reaction cavity of the deposition system to perform cold wall chemical vapor deposition reaction, wherein the volume ratio of the ethanol to the hydrogen is respectively 5: 5, the reaction time is 30 minutes, and the reaction pressure is 1000 Pa.
3) And after the reaction is finished, closing the ethanol gas and the hydrogen gas and quickly cooling to room temperature to obtain the graphene photonic crystal fiber.
The graphene optical fiber obtained in the embodiment is an in-situ composite structure of bare photonic crystal quartz optical fiber and graphene, and the outer surface of the bare optical fiber is covered with a continuous graphene film, wherein the coverage degree is 100%.
Example 7 in-situ direct preparation of graphene micro-nano optical fiber
1) Installing a cold-wall chemical vapor deposition system on an optical fiber drawing machine, placing a bare micro-nano fluoride (ZBLAN) optical fiber obtained by a drawing method in the cold-wall chemical vapor deposition system, and heating to 700 ℃ under a hydrogen-argon mixed atmosphere containing 5% of hydrogen;
2) keeping the temperature constant, introducing acetylene and hydrogen into a reaction cavity of the deposition system to perform hot wall chemical vapor deposition reaction, wherein the volume ratio of the acetylene to the hydrogen is 1-5: 5, the reaction time is 30 minutes, and the reaction pressure is 200 Pa.
3) And after the reaction is finished, closing acetylene and hydrogen and quickly cooling to room temperature to obtain the graphene micro-nano optical fiber.
The graphene optical fiber obtained in the embodiment is of an in-situ composite structure of the micro-nano optical fiber and graphene, the outer surface of the bare optical fiber is covered with a continuous graphene film, and the coverage degree is 100%.
Example 8 in-situ direct preparation of graphene conventional silica optical fiber
1) Installing a plasma enhanced chemical vapor deposition system on an optical fiber drawing machine, placing a bare conventional quartz optical fiber obtained by a drawing method in the plasma enhanced chemical vapor deposition system, and heating to 600 ℃ under argon atmosphere;
2) keeping the temperature constant, introducing ethylene gas and hydrogen into a reaction cavity of the deposition system to perform plasma enhanced chemical vapor deposition reaction, wherein the volume ratio of ethylene to hydrogen is 1-5: 5, the reaction time is 60 minutes, and the reaction pressure is 200 Pa.
3) And after the reaction is finished, closing the ethylene and the hydrogen and quickly cooling to room temperature to obtain the graphene conventional quartz optical fiber.
The graphene optical fiber obtained in the embodiment is of an in-situ composite structure of a conventional quartz optical fiber and graphene, and the outer surface of the bare optical fiber is covered with a continuous graphene film, wherein the coverage degree is 100%.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. An in-situ direct preparation method of a graphene optical fiber comprises the following steps:
1) installing chemical vapor deposition equipment on an optical fiber drawing machine, placing a porous optical fiber drawn by the drawing machine in a cavity of the chemical vapor deposition equipment, and heating to 1100-1700 ℃ under the protection of inert atmosphere;
2) keeping the temperature in the step 1) constant, introducing a carbon source and hydrogen into the equipment cavity in the step 1) to perform chemical vapor deposition reaction, closing the carbon source after the reaction is finished, and quickly cooling to room temperature to obtain the graphene optical fiber.
2. The method of claim 1, wherein: in the step 1), the porous optical fiber obtained by the wire drawing method is made of any one of quartz and mixed fluoride.
3. The method of claim 1, wherein: the chemical vapor deposition equipment is any one of hot wall chemical vapor deposition equipment and cold wall chemical vapor deposition equipment.
4. The method of claim 1, wherein: the inert atmosphere is argon or a hydrogen-argon mixture containing 5% of hydrogen by volume fraction.
5. The method of claim 1, wherein:
the carbon source is any one of methane, ethylene, propylene, acetylene and ethanol;
in the chemical vapor deposition reaction step, the volume ratio of the carbon source gas to the hydrogen gas is 1-5: 5.
6. the method of claim 1, wherein: the pressure of the chemical vapor deposition reaction is 200 Pa-1.01 multiplied by 105Handkerchief; the reaction time is 30 minutes to 120 minutes.
7. The method according to any one of claims 1 to 6, wherein: the obtained graphene optical fiber is of a composite structure of graphene grown in situ on the porous optical fiber;
the inner surface and the outer surface of the porous optical fiber are both covered with continuous graphene films, and the coverage is 100%.
8. The method of claim 1, wherein: the graphene in the graphene optical fiber is uniform in thickness, and 1-10 layers of the graphene optical fiber are adjustable.
9. The method of claim 1, wherein: the graphene surface in the graphene optical fiber does not contain oxygen-rich functional groups and metal impurity residues.
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| CN108459449B (en) * | 2018-03-05 | 2020-06-02 | 北京大学 | All-optical modulator based on graphene optical fiber and modulation method thereof |
| CN108545966A (en) * | 2018-07-16 | 2018-09-18 | 北京石墨烯研究院 | A kind of Graphene glass fiber and preparation method thereof |
| CN110554455B (en) * | 2019-08-21 | 2020-06-09 | 北京大学 | Method for rapidly preparing transition metal chalcogenide composite optical fiber material |
| CN110922068A (en) * | 2019-10-25 | 2020-03-27 | 武汉大学 | Graphene optical fiber and preparation method thereof |
| CN110684652A (en) * | 2019-10-30 | 2020-01-14 | 德州学院 | Graphene nucleic acid biosensor, and preparation method and application thereof |
| CN113725704A (en) * | 2020-05-25 | 2021-11-30 | 北京石墨烯研究院 | Saturable absorber and all-fiber mode-locked laser |
| CN112068241B (en) * | 2020-09-24 | 2022-11-01 | 西安科技大学 | Terahertz photonic crystal fiber composite waveguide based on graphene coating |
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| CN102161482B (en) * | 2011-01-25 | 2013-08-14 | 中国科学院化学研究所 | Method for preparing graphene |
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