KR101573877B1 - Method for manufacturing grphene based nanocarbon fiber using self assembly of layers - Google Patents
Method for manufacturing grphene based nanocarbon fiber using self assembly of layers Download PDFInfo
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- KR101573877B1 KR101573877B1 KR1020140049082A KR20140049082A KR101573877B1 KR 101573877 B1 KR101573877 B1 KR 101573877B1 KR 1020140049082 A KR1020140049082 A KR 1020140049082A KR 20140049082 A KR20140049082 A KR 20140049082A KR 101573877 B1 KR101573877 B1 KR 101573877B1
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
Abstract
A method for manufacturing graphene-based nano carbon fibers using interlayer self-assembly is provided. The method of manufacturing graphene-based nanocarbon fibers using interlayer self-assembly according to an embodiment of the present invention includes the steps of providing nanocarbon oxide and spinning the nanocarbon oxide dispersion liquid into a coagulating bath containing polyamine, Thereby producing a crosslinked oxidized nano-carbon gel fiber.
Description
The present invention relates to a method of manufacturing graphene-based nanocarbon fibers using interlayer self-assembly, and more particularly, to a method of manufacturing graphene-based nanocarbon fibers using graphene and graphene based graphene nanoribbons, carbon nanotubes, The present invention relates to a method for manufacturing nanofiber carbon fibers using miraculous attraction.
Nano carbon including graphene and carbon nanotubes is emerging as a next-generation high-tech material that can be utilized as electronic materials, heat dissipation materials, and ultrahigh strength structural materials because of its excellent properties including electrical, thermal and mechanical characteristics. The physical properties of these excellent nanocarbons are currently being realized in molecular carbon nanotubes and graphenes using chemical vapor deposition methods. However, due to the difficulty in realizing large-area and large-volume synthesis and uniform nanocarbon crystal structure in the bulk unit, Excellent characteristics can not be effectively expressed.
In order to solve the above problem, a research to expand the graphene oxide and carbon oxide nanotubes to a bulk unit by enlarging and densifying the graphene oxide and carbon oxide nanotubes through a van der Waals force between a connecting medium or a graphene layer It is progressing. Among these technologies, nanofiber carbon fiber spinning technology is maximizing the orientation and interaction of the graphene layer, and it is attracting attention as a technique to maximize the electrical and thermal properties as well as the mechanical properties of the nanocarbon. Here, the fiberization of nanocarbon can be realized by spinning nanocarbon in a coagulating bath, which can reduce the repulsive force between the nanocarbon dispersion graphene layers, and coagulating the nanocarbon linearly.
Particularly, graphene fibers in nano carbon fibers can be produced by mass-produced graphene oxide dispersions using positively charged molecules (CTAB) which can maximize mutual attraction between graphene layers (Sci. Rep.2012, 2, 613.] Polymer (chitosan) [Adv. Func. Mater.2013, 23, 5345.), high salt (CaCl2) (Adv. Mater.2013, 25, 188.), weak reducing material (NaOH) [Nat. Comm.2011, 2, 571.] or by adjusting the temperature and pH of the coagulating bath [Chem. Comm.2011, 47, 8650.].
However, these methods simply induce the assembly of graphene layers by weakening the electrostatic repulsion between the graphene layers or by strengthening the van der Waals force, which can not induce graphene orientation and reciprocal attraction sufficiently, it's difficult. Therefore, it is necessary to coagulate the radiated graphene oxide fibers in the coagulating bath for a long period of time, to further elongate the fibers using a rotating plate, and to use coagulant such as ethanol. .
Thus, in order to solve the problem involved in spinning nano carbon fibers including graphene and carbon nanotubes, it is necessary to develop a simple and safe spinning process by maximizing the attraction force between graphene layers.
Accordingly, a problem to be solved by the present invention is to provide a nano carbon fiber excellent in mechanical and electrical properties through self-assembly and reduction through polyamine crosslinking rule, and a method for manufacturing it quickly and simply.
Another problem to be solved by the present invention is to provide a method for easily controlling the physical properties of the nano-carbon fiber, which can reduce the manufacturing process and costs.
According to an aspect of the present invention, there is provided a method of manufacturing a graphene-based nano carbon fiber using interlayer self-assembly according to an embodiment of the present invention, comprising the steps of: providing nanocarbon oxide; And then spinning in a coagulating bath to produce an oxidized nanocarbon gel fiber crosslinked with the polyamine.
And washing and drying the nano-carbon oxide gel fibers to produce nano-carbon oxide nanofibers.
And reducing the nano-carbon oxide nanofiber.
The nano-carbon oxide may include one of carbon oxide nanotubes, graphen oxide, and oxidized graphene nanoribbons.
The dispersion of nanocarbon oxide is prepared by mixing distilled water, N, N dimethylforamide, methanol, ethanol, ethyleneglycol, n-butanol, tert- containing one of isopropyl alcohol, isopropyl alcohol, n-propanol, ethyl acetate, dimethyl sulfoxide, and tetrahydrofuran, Can be used.
The concentration of the nano-carbon oxide solution may be 1 mg / mL to 50 mg / mL.
The polyamines can use polyamines, including molecules containing two or more amine functional groups.
The concentration of the polyamine in the coagulation bath may be 0.001M to 1M.
Examples of the solvent in the coagulation bath of the polyamine include distilled water, N, N dimethylformamide, methanol, ethanol, ethyleneglycol, n-butanol, tert- Examples of the solvent include butyl alcohol, tert-butyl alcohol, isopropyl alcohol, n-propanol, ethyl acetate, dimethyl sulfoxide, and tetrahydrofuran. can do.
The step of reducing the nano-carbon oxide nanofiber may further include a step of performing thermal reduction or a step of performing chemical reduction.
The step of performing the thermal reduction may be performed by raising the temperature at a temperature of 200 ° C to 1000 ° C at a room temperature of 0.1 ° C / min to 10 ° C / min.
The step of performing the chemical reduction may be carried out using a reducing agent such as hydrazine, hydroiodic acid, hydrobromic acid, sodium borohydride, lithium aluminum hydride or sulfuric acid, And a reducing reagent containing a reducing agent.
The details of other embodiments are included in the following description and drawings.
According to the embodiments of the present invention, the polyamine molecule binds the graphene layer in the nano-carbon oxide effectively by ionic bonding and covalent bonding to the orientation of the graphene layer by the shear stress along with radiation, Nano carbon fiber excellent in carbon and electrical properties can be produced.
The nano-sized carbon nanofibers thus produced can be obtained by simple drying in air, and subsequent processes such as drawing and high-temperature vacuum drying are unnecessary, thereby simplifying the entire process.
It is also possible to manufacture customized nanocarbon fibers by varying the interlayer spacing and hierarchical structure of the graphene in the nanocarbon according to the chain length and structure characteristics of the introduced polyamines.
The effects of the present invention are not limited to the effects mentioned above, and the effects of the other inventions can be clearly understood from the description of the claims.
FIG. 1 is a flow chart of a method for fabricating graphene-based nano carbon fibers using interlayer self-assembly according to an embodiment of the present invention.
Fig. 2 is an SEM image of the surface (a) and the cross section (b) of the graphene oxide fiber among the oxidized nano carbon fibers produced according to the manufacturing method of Fig. 1;
3 is a C1s XPS result of the graphene oxide fiber produced by the manufacturing method of FIG.
4 is a graph showing the results of XRD pattern analysis of graphene oxide fibers crosslinked by (a) graphene oxide film and (b) different amine-based materials prepared according to the manufacturing method of FIG.
5 is a graph showing a curve of a tensile test result of the graphene oxide fiber produced by the manufacturing method of FIG.
BRIEF DESCRIPTION OF THE DRAWINGS The advantages and features of the present invention, and the manner of achieving them, will be apparent from and elucidated with reference to the embodiments described hereinafter in conjunction with the accompanying drawings. The present invention may, however, be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. Is provided to fully convey the scope of the invention to those skilled in the art, and the invention is only defined by the scope of the claims. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Reference will now be made in detail to the preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings. &Quot; and / or "include each and every combination of one or more of the mentioned items. ≪ RTI ID = 0.0 >
The terminology used herein is for the purpose of illustrating embodiments and is not intended to be limiting of the present invention. In the present specification, the singular form includes plural forms unless otherwise specified in the specification. The terms " comprises "and / or" comprising "used in the specification do not exclude the presence or addition of one or more other elements in addition to the stated element.
Unless defined otherwise, all terms (including technical and scientific terms) used herein may be used in a sense commonly understood by one of ordinary skill in the art to which this invention belongs. Also, commonly used predefined terms are not ideally or excessively interpreted unless explicitly defined otherwise.
Hereinafter, a method for fabricating graphene-based nano carbon fibers using interlayer self-assembly according to embodiments of the present invention will be described with reference to FIGS.
FIG. 1 is a flow chart of a method for fabricating graphene-based nano carbon fibers using interlayer self-assembly according to an embodiment of the present invention.
Referring to FIG. 1, a method of fabricating graphene-based nano carbon fibers using interlayer self-assembly according to an embodiment of the present invention includes the steps of (S10) preparing a nano-carbon oxide dispersion, (S20) spinning the nanofibers, washing and drying the nanofiber nano-carbon fibers (S30), and reducing the nanofiber nano-carbon fibers to nano carbon fibers (S40).
The nanocarbon oxide for fiber production may be carbon nanotubes, graphene oxide, or graphene oxide nanoparticles, but is not limited thereto, and materials having a nano-sized structure may be included without limitation.
The dispersion of nano-carbon oxide for spinning may have a concentration of 1 mg / mL to 50 mg / mL. As the solvent, distilled water, N, N dimethylforamide, methanol, ethanol, ethyleneglycol, n-butanol, tert-butylalcohol, isopropyl alchol, n-propanol, ethyl acetate, dimethyl Dimethyl sulfoxide, tetrahydrofuran, or the like.
The polyamines contained in the coagulation bath for the agglomeration of the radiated oxidized nanocarbon can use any molecule containing two or more primary or secondary amine groups.
A polyamine molecule is a weak base molecule containing two or more primary or secondary amines (-NH 2 , or? H-) groups, and accepts hydrogen ions of acidic functional groups such as carboxyl group (-COOH) of graphene oxide and carbon oxide nanotube It produces aminic acid salts. This amine salt forms an ion pair with a strong electrical attraction with the carboxyl salt, the conjugated base of the carboxyl group. Therefore, when the nano-carbon dispersion having a large amount of acidic functional groups in the coagulation bath containing polyamine is spun out, the graphene layer is agglomerated in a short time due to the strengthening of the polyamine and nano carbon, And is maintained without a separate subsequent process. Also, in the drying process, the residual polyamine forms a covalent bond through the ring-opening polymerization with the epoxy (-O-) functional group of the nanocarbon oxide, and the binding between the graphene layers is strengthened. Such ion pair formation and covalent bond formation enable production of nano-carbon nanofiber with excellent mechanical properties, and reduction nano carbon fibers can be produced by thermal or chemical reduction.
For example, the polyamines according to this embodiment include ethylenediamine, 1,3 diaminopropane, 1,2 diaminopropane, and 1,2-diaminopropane, where the amine functionality is linked to an alkyl chain, 1,4 diaminobutane, 1,5 diaminopentane, hexamethylenediamine, 1,7 diaminoheptane, 1,8 diamine, Aliphatic polyamines including 1,8 diaminooctane, and p-phenylenediamine, m-phenylenediamine, o-phenylenediamine, amine functional groups connected to the benzene ring, (o-phenylenediamine), benzidine (benzidine) can be used.
The concentration of the polyamine solution for spinning can be set at 0.001M to 1M. When the concentration of the polyamine is less than 0.001M, crosslinked fibers between the nanocarbon are not formed because the amount of the polyamine to be crosslinked is small. Conversely, when the concentration of the polyamine exceeds 1M, only one of the terminal functional groups of the polyamine is bonded to the functional group So that no crosslinked fibers are formed.
Depending on the type of polyamine, the physical properties may vary. For example, in the case of aliphatic amines, the shorter the length of the polyamine, the narrower the distance between the nanocarbon layers, and the shorter the range in which the molecules can move, the greater the modulus and tensile strength. In the case of amine, the mechanical strength can be improved because the rigidity of the molecule is higher than that of aliphatic amine.
The solvent of the coagulating bath for the emulsification may be distilled water, N, N dimethylforamide, methanol, ethanol, ethyleneglycol, n-butanol, tert-butyl alcohol a method of dissolving a polyamine molecule including a tert-butylalcohol, isopropylalcohol, n-propanol, ethyl acetate, dimethyl sulfoxide, and tetrahydrofuran, All possible solvents are available.
Radiation of the nanocarbon oxide is carried out through a spinneret having an inner diameter of 0.00725 mm to 0.15 mm and can be carried out at a flow rate of 0.1 mL / min to 100 mL / min with the nozzle immersed in a coagulating bath or positioned at 0 cm to 1 cm from the top .
The radiated nano-carbon can be recovered by the roller and the remaining polyamine can be washed with the solvent of the coagulation bath described above. More preferably, it can be washed with an alcohol-based solvent which evaporates at room temperature.
The nano-sized carbon nanofibers cleaned through the above process can be dried at room temperature and normal pressure, but there is no particular limitation as long as the temperature and the pressure range do not cause reduction of the nano-carbon oxide.
In some other embodiments, the oxidized nanocarbon fiber in step S20) of spinning the nanocarbon oxide dispersion into a polyamine-containing coagulation bath may be an oxidized nanocarbon gel fiber, The step of washing and drying the fibers to prepare the nano-sized carbon nanofibers can be further performed.
The nanocomposite nanocarbon fibers crosslinked with the polyamine produced through the above process can be reduced to nanocarbon fibers by a thermal reduction method and / or a chemical reduction method.
The thermal reduction method may be performed by raising the temperature at a temperature of 200 ° C to 1000 ° C at a room temperature of 0.1 ° C / minute to 10 ° C / minute.
The chemical reduction method can be carried out using any one of hydrazine, hydroiodic acid, hydrobromic acid, sodium borohydride, lithium aluminum hydride and sulfuric acid. Or by using a reducing reagent including the reducing agent.
Advantages and features of the present invention will be clearly described with reference to the following experimental examples. However, the present embodiments are presented so that those skilled in the art can fully understand the scope of the present invention. It is only defined by category.
Example One
This example relates to the production of reduced graphene oxide fibers in the nanocarbon fibers described in the present invention.
In step S10, the modified Hummer? method [Chem. Mater. 1999, 11, 771.], 10 mg / mL of graphene oxide aqueous solution was prepared. To this end, 2.4 g of graphite flake (Sigma-aldrich) was mixed with 10 ml of sulfuric acid in which 2.0 g of potassium persulfate (Sigma-aldrich) and 2.0 g of phosphorus pentoxide (Sigma-aldrich) And reacted at 80 ° C for 72 hours.
Thereafter, the reacted graphite was diluted with water and then obtained by vacuum filtration, followed by drying at room temperature in vacuum for 24 hours to obtain expanded graphite.
12.0 g of potassium permanganate (manufactured by Sigma-aldrich) was dissolved and reacted at 35 ° C for 2 hours and 30 minutes. Then, 1.0 L of distilled water was added to the dispersion solution at a temperature of 45 ° C , And then the reaction was terminated by adding 20 mL of 30% aqueous hydrogen peroxide (produced by Daejeon Chemical).
Thereafter, the reaction mixture was centrifuged at a speed of 10,000 rpm for 10 minutes, and then centrifugation was repeated three times or more by adding 1.0 M hydrochloric acid aqueous solution, followed by centrifugation at a speed of 13,000 rpm for 40 minutes Was repeated five or more times to obtain an aqueous graphene oxide solution.
Following step S20, graphene oxide gel fibers crosslinked with a polyamine were prepared. The graphene oxide aqueous solution obtained in the step S10 was diluted with an aqueous solution to an amount of 10 mg / mL and put into a 5 mL syringe. Then, 0.1 M aqueous solution of hexamethylenediamine (manufactured by Sigma-aldrich) at a rate of 10 mL / min through a nozzle having an inner diameter of 0.413 mm To thereby obtain gel-type graphene oxide fibers.
According to step S30, the graphene oxide gel fibers were washed in methanol to prepare graphene oxide fibers crosslinked with polyamines, and then dried at room temperature and atmospheric pressure for 24 hours.
Example 2
In order to produce reduced graphene oxide fibers of the nano carbon fibers provided in the present invention, the graphene oxide fibers prepared according to Example 1 of the present invention were heated to 200 ° C at a rate of 0.1 ° C / (S40).
Example 3
In order to produce reduced graphene oxide fibers according to another embodiment of the present invention, the graphene oxide fibers prepared in Example 1 of the present invention were reacted with iodonic acid (Sigma-aldrich) for 12 hours, And then dried.
Experimental Example 1 - Scanning Electron Microscope ( SEM ) analysis
2 is a cross-sectional photograph (a) of the polyamine-crosslinked graphene oxide fiber prepared according to Example 1 of the present experiment and a cross-sectional photograph (b). 2, it is confirmed that the graphene layer is oriented and densified according to the embodiment of the present invention.
Experimental Example 2 - XPS (X- ray photoelectron spectroscopy ) analysis
3 shows the results of analysis of C1s XPS of graphene oxide film (a) and graphene oxide fiber (b) prepared according to Example 1 of the present invention. As a result of ring opening reaction of amine group and epoxy group, graphene oxide film The CO bond of the epoxy functional group was converted to the CN bond as a result of the ring opening reaction of the epoxy functional group.
Experimental Example 3 - X-ray diffraction (X- ray diffraction ) analysis
FIG. 4 is a graph showing the results obtained when a graphene oxide film, a polyamine crosslinked graphene oxide fiber prepared in accordance with Example 1 of the present invention, and a polyamine crosslinked graphene oxide fiber according to an embodiment of the present invention were produced, instead of hexamethylene diamine Graphs showing the XRD pattern of graphene oxide fibers using ethylenediamine (Sigma-aldrich) or 1,8-diaminooctane (Sigma-aldrich).
The interlayer spacing (d 002 ) of the (002) plane representing the distance between the graphene layers when compared to the graphene film increases as the length of the alkyl chain of the polyamine increases, thereby increasing the structure of the graphene oxide fiber to the type of polyamine (Table 1).
Graphen oxide fiber
Graphen oxide fiber
Experimental Example 4 - Tensile test
5 is a strain-stress curve representative of the tensile test results of the graphene oxide fibers crosslinked with the three kinds of polyamines mentioned in Experimental Example 3. Fig. It can be seen from FIG. 5 that the mechanical properties of the polyamine crosslinked graphene oxide fibers vary depending on the type of the crosslinked polyamine, and by introducing various polyamines, it is possible to prepare graphene oxide or reduced graphene oxide fibers of desired physical properties Is possible. Table 2 shows the average Young's modulus and tensile strength of each graphene oxide fiber.
Graphen oxide fiber
Graphen oxide fiber
Experimental Example 5 - Electrical conductivity measurement
Table 3 shows the electrical conductivities of the reduced graphene oxide fibers prepared according to Examples 2 and 3 according to the reduction method.
(Example 1)
(Example 2)
(Example 3)
While the present invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, It will be understood that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive.
Claims (12)
And spinning the nano-carbon oxide dispersion liquid into a coagulation bath containing polyamine to prepare an oxidized nano-carbon fiber crosslinked with the polyamine.
The step of preparing the nano-
Spinning the nano-carbon oxide dispersion liquid into a coagulation bath containing a polyamine to prepare an oxidized nano-carbon fiber fiber crosslinked with the polyamine; And
And washing and drying the nano-carbon oxide gel fibers to prepare nano-sized carbon nanofibers.
After the step of producing the nano-carbon oxide nanofiber,
Further comprising the step of reducing the nano-carbon nano-carbon fibers.
Wherein the nano-carbon nanotubes comprise one of carbon nanotubes, graphene oxide, and graphene oxide nanoribbons.
The dispersion of nanocarbon oxide is prepared by mixing distilled water, N, N dimethylforamide, methanol, ethanol, ethyleneglycol, n-butanol, tert- containing one of isopropyl alcohol, isopropyl alcohol, n-propanol, ethyl acetate, dimethyl sulfoxide, and tetrahydrofuran, (Manufacturing method of graphene - based nano carbon fiber using self - assembly).
Wherein the concentration of the nano-carbon oxide dispersion is 1 mg / mL to 50 mg / mL.
Wherein the polyamine is an organic compound containing two or more amine functional groups, wherein the graphene-based nano carbon fibers are prepared by interlayer self-assembly.
Wherein the concentration of the polyamine in the coagulation bath is in the range of 0.001M to 1M.
Examples of the solvent in the coagulation bath of the polyamine include distilled water, N, N dimethylformamide, methanol, ethanol, ethyleneglycol, n-butanol, tert- One of tertiary butyl alcohol, isopropyl alcohol, n-propanol, ethyl acetate, dimethyl sulfoxide and tetrahydrofuran. Based nanocarbon fiber fabrication method using interlayer self-assembly.
Wherein the step of reducing the nano-carbon oxide nanofibers comprises one of the steps of performing thermal reduction or performing chemical reduction.
Wherein the step of performing the thermal reduction is performed by raising the temperature at a temperature of 200 ° C to 1000 ° C at a rate of 0.1 ° C / min to 10 ° C / min at room temperature to produce graphene-based nano- Way.
The step of performing the chemical reduction may be carried out using a reducing agent such as hydrazine, hydroiodic acid, hydrobromic acid, sodium borohydride, lithium aluminum hydride or sulfuric acid, Wherein the method is carried out using any one of the reducing reagents.
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| PCT/KR2015/003158 WO2015163595A1 (en) | 2014-04-24 | 2015-03-31 | Method for producing graphene-based nano carbon fiber using inter-layer self-assembly |
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| KR20170121504A (en) * | 2016-04-25 | 2017-11-02 | 재단법인차세대융합기술연구원 | Method for preparing graphene oxide fibers, graphene fibers or their composite fibers by using wet spinning induced by electric field |
| KR101812536B1 (en) * | 2016-05-04 | 2017-12-29 | 재단법인 차세대융합기술연구원 | Wet spinningMethod for preparing GO-CNT composite fibers, GO-Graphene composite fibers, GO-Grephene-CNT composite fibers |
| KR101812534B1 (en) * | 2016-06-27 | 2017-12-29 | 재단법인 차세대융합기술연구원 | Method for preparing GO-CNT composite fibers, GO-Graphene composite fibers, GO-Graphene-CNT composite fibers |
| US11542411B2 (en) * | 2017-05-27 | 2023-01-03 | Hangzhou Gaoxi Technology Co., Ltd. | Method for preparing composites on basis of graphene bonding |
| KR101992456B1 (en) * | 2018-01-25 | 2019-06-24 | 한국과학기술연구원 | Graphene oxide fiber with improved mechanical property and method of making the same |
| KR102602632B1 (en) | 2018-02-13 | 2023-11-15 | 아톰 드레드즈 코퍼레이션 | Graphene oxide fiber and method for manufacturing the same |
| KR102529541B1 (en) | 2018-03-20 | 2023-05-04 | 아톰 드레드즈 코퍼레이션 | High Strength Graphene Fiber and Manufacturing Method Thereof |
| KR20190110470A (en) | 2018-03-20 | 2019-09-30 | 한양대학교 산학협력단 | Nitrogen and Sulfur Doped Graphene Fibers and Manufacturing Method Thereof |
| CN109112822B (en) * | 2018-07-23 | 2021-01-22 | 河南工业大学 | Method for preparing carbon fiber in-situ growth graphene composite carrier |
| KR102102594B1 (en) * | 2018-10-25 | 2020-04-21 | 한국세라믹기술원 | Manufacturing method of carbon fiber-BN composite |
| KR102301706B1 (en) * | 2020-02-10 | 2021-09-14 | 한국과학기술원 | Method of mxene fiber and mxene fiber manufactured therefrom |
| KR102480878B1 (en) * | 2020-11-16 | 2022-12-23 | 광주과학기술원 | Nanofiber composite material, manufacturing method thereof, and ion exchange membrane including the same |
| CN112791697B (en) * | 2020-12-16 | 2022-08-05 | 中山市华锌工材料科技有限公司 | Elastic super-hydrophobic graphene gel ball and preparation method and application thereof |
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