KR20170026842A - Reduced graphene oxide/carbon nanotube/manganese dioxide composite for supercapacitor electrode materials, and preparation method thereof - Google Patents
Reduced graphene oxide/carbon nanotube/manganese dioxide composite for supercapacitor electrode materials, and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 50
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 47
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 47
- 239000002131 composite material Substances 0.000 title claims description 29
- 239000007772 electrode material Substances 0.000 title description 9
- 238000002360 preparation method Methods 0.000 title description 2
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 12
- 239000002105 nanoparticle Substances 0.000 claims description 12
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 9
- 239000011541 reaction mixture Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 3
- 125000003172 aldehyde group Chemical group 0.000 claims description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 2
- 125000000524 functional group Chemical group 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 239000002071 nanotube Substances 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 8
- 230000009467 reduction Effects 0.000 abstract description 2
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 230000003252 repetitive effect Effects 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 7
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 5
- 238000004769 chrono-potentiometry Methods 0.000 description 4
- 238000002484 cyclic voltammetry Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002525 ultrasonication Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- GOPYZMJAIPBUGX-UHFFFAOYSA-N [O-2].[O-2].[Mn+4] Chemical class [O-2].[O-2].[Mn+4] GOPYZMJAIPBUGX-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- -1 graphene graphene Chemical class 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 230000027756 respiratory electron transport chain Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
The present invention relates to a reduced oxide graphene / carbon nanotube / manganese dioxide complex for a high performance supercapacitor and a method of manufacturing the same, wherein the electrode made of the reduced oxidized graphene / carbon nanotube / manganese dioxide complex has a current of 0.2 A / g It is very useful as an electrode for electrochemical supercapacitors because it has a very high non-storage capacity, such as 915 F / g at the density, and excellent cyclic stability after 1500 repetitive charge-discharge cycles and a capacity reduction of only 1.9% And in particular, the complex can be prepared in a very simple and efficient manner.
Description
The present invention relates to reduced oxidized graphene / carbon nanotube / manganese dioxide composites for high performance supercapacitor electrode materials and methods of making the same.
The super capacitor is an energy storage device that stores and supplies electric energy by using the capacitor behavior caused by the electrochemical reaction between the electrode and the electrolyte. The super capacitor is superior in energy density and power density to the conventional electrolytic capacitor and the secondary battery, It is a new concept of energy storage power source that can store and supply energy quickly.
Generally, a supercapacitor is composed of an electrode material, an electrolyte, a separator, and a current collector, and the electrode material is the most important component and dominates the overall electrochemical performance of the supercapacitor.
Ideal supercapacitor electrode materials require a variety of properties such as high specific surface area, well controlled porosity, high electrical conductivity, desirable electroactive sites, high thermal and chemical stability and low cost of manufacture and manufacturing process.
Various attempts have been made to develop active electrode materials for supercapacitors, and transition metal oxides, which are known as capacitive materials, have been noted as attractive materials. However, such transition metal oxides have limitations that hinder rapid electron transfer requiring high charge / discharge rates due to low rate capacity and poor stability.
It is an object of the present invention to provide reduced oxidized graphene / carbon nanotube / manganese dioxide composites for high performance supercapacitor electrode materials.
Another object of the present invention is to provide an electrode for a high performance supercapacitor including a reduced oxidized graphene oxide / carbon nanotube / manganese dioxide complex.
Still another object of the present invention is to provide a method for manufacturing a reduced oxide graphene / carbon nanotube / manganese dioxide composite for a high performance supercapacitor.
In order to accomplish the above object, the present invention provides a reduced oxidized graphene sheet; Carbon nanotubes formed on the surface of the reduced oxidized graphene sheet; And a reduced oxide graphene / carbon nanotube / manganese dioxide composite comprising manganese dioxide (MnO 2 ) nanoparticles formed on the surface of the reduced oxidized graphene sheet.
The present invention also relates to a reduced oxidized graphene sheet; Carbon nanotubes formed on the surface of the reduced oxidized graphene sheet; And a reduced oxide graphene / carbon nanotube / manganese dioxide composite comprising manganese dioxide (MnO 2 ) nanoparticles formed on the surface of the reduced oxidized graphene sheet.
The present invention also relates to a method for manufacturing a carbon nanotube, which comprises dispersing and functionalizing carbon nanotubes and graphene oxide in water and suspending them by ultrasonication (first step); Adding a permanganate to the suspended solution and stirring (second step); Heating the stirred reaction mixture in an electronic oven and cooling to room temperature (Step 3); And a step of washing and cooling the cooled reaction mixture (step 4), thereby producing a reduced oxidized graphene / carbon nanotube / manganese dioxide composite.
The electrode made of the reduced oxide graphene / carbon nanotube / manganese dioxide complex according to the present invention has a very high non-storage capacity such as 915 F / g at a current density of 0.2 A / g, and has 1500 repeated charge- Since it exhibits excellent cycle stability and a capacity reduction of only 1.9%, it can be very usefully used as an electrode for an electrochemical supercapacitor. In particular, the complex can be produced in a very simple and efficient manner.
Fig. 1 shows SEM images (a, c, e) and TEM images (b, d, f) of CNT-COOH, GO / MnO 2 and RGO / CNT / MnO 2 composites.
FIG. 2 shows XRD analysis results of GO, CNT-COOH, RGO / MnO 2 and RGO / CNT / MnO 2 complexes.
3 shows XPS analysis results of the RGO / CNT / MnO 2 composite.
FIG. 4 shows the results of electrochemical performance analysis of RGO / CNT / MnO 2 electrodes, showing (a) CV results, (b) constant current charge-discharge results, (c) Nyquist plot results, And the change of the non-storage capacity.
The present inventors have studied and found a more useful material as an electrode material for a high-performance supercapacitor. As a result, they have found that reduced graphene graphene modified with carbon nanotubes and manganese dioxide (MnO 2 ) nanoparticles on the surface of a reduced oxidized graphene sheet, Carbon nanotube / manganese dioxide complex as an electrode for an electrochemical supercapacitor has excellent performance and is stable, thereby completing the present invention.
Hereinafter, the present invention will be described in more detail.
The present invention relates to a reduced oxidized graphene sheet; Carbon nanotubes formed on the surface of the reduced oxidized graphene sheet; And a reduced oxide graphene / carbon nanotube / manganese dioxide composite comprising manganese dioxide (MnO 2 ) nanoparticles formed on the surface of the reduced oxidized graphene sheet.
The composite may include 50 to 150 parts by weight of carbon nanotubes and 150 to 250 parts by weight of MnO 2 nanoparticles relative to 100 parts by weight of the reduced oxidized graphene sheet.
The carbon nanotubes have a role of promoting electrical conductivity. When the content is out of the above range, the electrical conductivity may be too low. If the content is too large, the carbon nanotube may be expensive and the surface area may decrease The MnO 2 nanoparticles have an average diameter of 2 to 7 nm and an average length of 30 to 70 nm. The MnO 2 nanoparticles have the role of enhancing the non-storage capacity, and when the content is out of the above range, Lt; / RTI >
The present invention also provides an electrode for a supercapacitor including the reduced oxide graphene / carbon nanotube / manganese dioxide composite.
The present invention also relates to a method for manufacturing a carbon nanotube, which comprises dispersing and functionalizing carbon nanotubes and graphene oxide in water and suspending them by ultrasonication (first step); Adding a permanganate to the suspended solution and stirring (second step); Heating the stirred reaction mixture in an electronic oven and cooling to room temperature (Step 3); And a step of washing and cooling the cooled reaction mixture (step 4), thereby producing a reduced oxidized graphene / carbon nanotube / manganese dioxide composite.
The first step may be performed by dispersing 0.15 to 0.45 parts by weight of functionalized carbon nanotubes and 0.15 to 0.45 parts by weight of oxidized graphene to 100 parts by weight of water and ultrasonication. At this time, the ultrasonic treatment can be performed at 40 kHz, 8 W for 30 minutes to 2 hours.
The functionalized carbon nanotube may be a carbon nanotube having a functional group selected from the group consisting of a carboxyl group (-COOH), a carbonyl group (> CO), an aldehyde group (-CHO), and a hydroxyl group (-OH).
In the second step, 0.75 to 1.25 parts by weight of potassium permanganate may be added to 100 parts by weight of the suspended solution, and stirring may be performed. If the content is out of the above range, the reserve specific amount may be lowered.
In the third step, the stirred reaction mixture may be heated in an electromagnetic oven at 100 to 150 W for 5 to 15 minutes and then cooled to room temperature. If the heating temperature is lower than the heating range, formation of MnO 2 particles is difficult The problem may be caused, and if it is high, the graphene sheet may be damaged.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the following examples. However, the scope of the present invention is not limited to the following examples.
≪ Example 1 > Reduced graphene oxide / carbon nanotube / MnO 2 (RGO / CNT / MnO 2 ) Preparation of complex
Oxidation graphene (GO) was synthesized from graphite powder (Alfa Aesar, 99.995%) using a modified Hummers method (ACS Nano 4 (2010) 4806-4814). Reduced GO / CNT / MnO 2 was prepared by dispersing 0.15 g of CNT (CNT-COOH) functionalized with carboxyl group and 0.15 g of GO in 50 mL of deionized water and sonicating for 1 hour. Then, 0.5 g of KMnO 4 was added to the suspension prepared above and stirred for 1 hour. The resulting reaction mixture was heated in a domestic electronic oven at 130 W for 10 minutes and then cooled to room temperature. The complex thus obtained was washed several times with deionized water and anhydrous alcohol, and then dried in a vacuum oven at 60 ° C for 24 hours.
≪ Example 2 > Reduced graphene oxide / carbon nanotube / MnO 2 (RGO / CNT / MnO 2 ) Composite Performance Analysis
SEM (Hitachi, S-4200) was used as a scanning electron microscope (SEM) to analyze the characteristics of the composite prepared in Example 1, and transmission electron microscopy (TEM X-ray diffraction (XRD) was performed using X-ray diffraction (XRD) (PANalytical, X'Pert-PRO MPD) using Cu Kα irradiation. And X-ray photoelectron spectroscopy (XPS) were analyzed using XPS (ULVAC-PHI, Quantera SXM) using Al X source.
FIG. 1 shows SEM images (a, c, e) and TEM images (b, d, f) of CNT-COOH, CNT / MnO 2 , RGO / MnO 2 and RGO / CNT / MnO 2 composites, The carbon tube and graphene sheet surface of the composite were clearly coated with MnO 2 nanoparticles. MnO 2 having a needle-shaped layer was 5 nm in diameter and 50 nm in length and uniformly grown on the surface of the RGO sheet. The MnO 2 nanoparticles were strongly bonded on the CNT surface with the RGO sheet to form MnO 2 and Thereby enabling rapid electron transfer between RGOs.
FIG. 2 shows the XRD patterns of CNT, CNT / MnO 2 , RGO / MnO 2 and RGO / CNT / MnO 2 composites. CNT shows a peak at 26.5 ° 2θ, GO shows a peak at 11.85 ° 2θ, RGO showed a broad peak at 26.0
FIG. 3 shows the results of XPS analysis of the RGO / CNT / MnO 2 composite. As shown in FIG. 3 A, XPS peaks of
≪ Example 3 > Reduced graphene oxide / carbon nanotube / MnO 2 (RGO / CNT / MnO 2 Performance Analysis of Composite Electrode
An electrochemical test was carried out using the composite prepared in Example 1 above as a working electrode. Cyclic voltammograms (CV) analysis, chronopotentiometry (CP) analysis and electrochemical impedance spectroscopy (EIS) were performed at room temperature on a three-electrode system Autolab PGSTAT302N (Metrohm, Netherlands). The working electrode was prepared by mixing the previously prepared composite powder (3 mg, 80 wt%) with 15 wt% acetyl black and 5 wt% polytetrafluoroethylene (PTFE) binder and using a nickel foam dust collector cm. Electrochemical analysis was performed on a 1M Na 2 SO 4 aqueous electrolyte at room temperature. The non-storage capacity (Cs) of the electrode was calculated from the CP curve using the following equation.
The non-storage capacity (Cs) of the electrode was calculated from the CP curve using the following equation.
C = It / m? V
C, I, t, m and ΔV mean the non-storage capacity (F / g), the discharge current (A), the discharge time (s), the mass (g) of the active material and the discharge potential range .
FIG. 4 shows the results of electrochemical analysis of RGO / CNT / MnO 2 composite, wherein FIG. 4A shows CV results at a scanning speed of 5 to 150 mV / s and shows a relatively rectangular shape at all scanning speeds without a definite redox peak This means that the electrode modified with RGO / CNT / MnO 2 composite exhibits low resistance and excellent capacity behavior. Figure 4b shows a constant current charge-discharge curve at various current densities showing a relatively symmetric linearity, which means quick IV reaction and excellent electrochemical reversible reaction. Figure 4c is the impedance result of the RGO / CNT / MnO 2 complex at a frequency range of 100 kHz to 0.1 Hz at an open potential with AC perturbation of 5 mV. The Nyquist plot shows mostly vertical lines at lower frequencies, And has electrochemical stability. FIG. 4d shows the non-storage capacity at a current density of 0.2 A / g, calculated from the charge-discharge curve, indicating that the supercapacitor based on the RGO / CNT / MnO 2 composite electrode exhibits excellent stability under repeated charge- . That is, when charging and discharging were performed at 1500 cycles at a rate of 0.2 A / g, 98.1% of the initial capacity was maintained.
While the invention has been described with reference to a limited number of embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. Accordingly, the true scope of the present invention should be determined by the technical idea of the appended claims.
Claims (9)
Carbon nanotubes formed on the surface of the reduced oxidized graphene sheet; And
A reduced oxidized graphene / carbon nanotube / manganese dioxide complex comprising manganese dioxide (MnO 2 ) nanoparticles formed on the surface of the reduced oxidized graphene sheet.
Adding a permanganate to the suspended solution and stirring (second step);
Heating the stirred reaction mixture in an electronic oven and cooling to room temperature (Step 3); And
Washing the cooled reaction mixture and drying (step 4)
/ RTI > The method of claim 1, wherein the reduced graphene graphene / carbon nanotube /
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| KR20190126570A (en) * | 2018-05-02 | 2019-11-12 | 인하대학교 산학협력단 | Reduced graphene oxide/carbon nanotube composite material having a sponge structure and method for manufacturing the same |
| CN116453874A (en) * | 2022-11-30 | 2023-07-18 | 湖南金阳烯碳新材料股份有限公司 | Graphene carbon nanocomposite and preparation method and application thereof |
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| KR102455421B1 (en) | 2020-10-16 | 2022-10-19 | 한국과학기술원 | nitrogen-doped MXene and supercapacitors containing the same |
| KR102629285B1 (en) | 2022-05-16 | 2024-01-25 | 한국과학기술원 | A supercapacitor having a mxene surface-treated using pyrrole and a method for manufacturing the same |
| KR20240048600A (en) | 2022-10-06 | 2024-04-16 | 연세대학교 산학협력단 | Re-stacked inorganic nanosheet and method for manufacturing same |
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| KR101486429B1 (en) | 2013-12-20 | 2015-01-26 | 한국세라믹기술원 | Composite for supercapacitor electrode with low initial resistance, manufacturing method of supercapacitor electrode using the composite and supercapacitor using the supercapacitor electrode manufactured by the method |
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| KR101486429B1 (en) | 2013-12-20 | 2015-01-26 | 한국세라믹기술원 | Composite for supercapacitor electrode with low initial resistance, manufacturing method of supercapacitor electrode using the composite and supercapacitor using the supercapacitor electrode manufactured by the method |
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| KR20190126570A (en) * | 2018-05-02 | 2019-11-12 | 인하대학교 산학협력단 | Reduced graphene oxide/carbon nanotube composite material having a sponge structure and method for manufacturing the same |
| CN116453874A (en) * | 2022-11-30 | 2023-07-18 | 湖南金阳烯碳新材料股份有限公司 | Graphene carbon nanocomposite and preparation method and application thereof |
| CN116453874B (en) * | 2022-11-30 | 2024-06-14 | 湖南金阳烯碳新材料股份有限公司 | Graphene carbon nanocomposite and preparation method and application thereof |
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| E902 | Notification of reason for refusal | ||
| GRNT | Written decision to grant |