WO2015126464A2 - Multicouches empilées d'oxyde de graphène réduit et de nanotubes de carbone en alternance pour supercondensateurs planaires ultra-minces - Google Patents

Multicouches empilées d'oxyde de graphène réduit et de nanotubes de carbone en alternance pour supercondensateurs planaires ultra-minces Download PDF

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WO2015126464A2
WO2015126464A2 PCT/US2014/060232 US2014060232W WO2015126464A2 WO 2015126464 A2 WO2015126464 A2 WO 2015126464A2 US 2014060232 W US2014060232 W US 2014060232W WO 2015126464 A2 WO2015126464 A2 WO 2015126464A2
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graphene oxide
rgo
cnt
gel electrolyte
layers
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PCT/US2014/060232
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WO2015126464A3 (fr
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Yadong Yin
Geon Dae MOON
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The Regents Of The University Of California
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • 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

Definitions

  • the present disclosure relates to supercapacitors, for example, stacked multilayers of alternating reduced graphene oxide and carbon nanotubes for ultrathin planar supercapacitors.
  • Supercapacitors for example, electrochemical capacitors, ECs
  • ECs electrochemical capacitors
  • graphene is a suitable electrode material due to its large surface area (theoretically 2630 m 2 g "1 for a single graphene sheet) and high in-plane electrical conductivity.
  • specific capacitance can improve, considering the theoretical value of 550 F/g for single-layer graphene while currently achievable values can be below 300 F/g.
  • the relatively low specific capacitance can be first attributed to restacking of the graphene sheets during processing due to sheet-to-sheet van der Waals interactions, leading to reduction of the specific surface area.
  • LBL Layer-by-layer processes have also been attempted to assemble graphene nanosheets or alternating layers of graphene and other carbon materials such as carbon nanotubes (CNTs) and polyaniline (PANi) through electrostatic attraction.
  • CNTs carbon nanotubes
  • PANi polyaniline
  • a hybrid film supercapacitor composed of poly(ethyleneimine)-modified graphene nanosheets and acid- treated multiwalled CNT via sequential self-assembly in an aqueous electrolyte have been studied. The results obtained in this study
  • the following criteria can be desirable: minimum restacking and agglomeration of graphene sheets, porous matrix structure for easy path of electrolyte ions, and good mechanical adhesion of active materials to the current collector.
  • a method of stacking multilayers of alternating graphene and carbon nanotubes (CNT) for a supercapacitor structure comprising: synthesizing graphene oxide (GO) from high purity graphite flake powder using a modified Hummer's method with an improved purification and then chemical reduction to form exfoliated graphene oxide; dispersing the reduced graphene oxide (rGO) nanosheets and CNTs in ethanol and 1-butanol, respectively;
  • an ultrathin supercapacitor structure comprising: a plurality of alternating layers of graphene and carbon nanotubes (CNT), wherein the layers of graphene are reduced graphene oxide nanosheets.
  • Figure 1 shows (a) a schematic illustration showing the formation of alternately stacked rGO/CNT films through repeated transfer of assembled monolayers of rGO and CNTs from water surfaces; (b,c) TEM images of rGO-CNT layer (b) and rGO-CNT-rGO layer (c), respectively, and wherein the inset in (b) shows an SEM image of the rGO-CNT layer, with a scale bar of 200 nm. (d,e) Cross-section SEM image (d) and AFM image (e) of alternately stacked rGO/CNT consisting of 16 rGO and 15 CNT layers. The thickness of the representative stacked film is about 200 nm.
  • Figure 2 shows (a) CV curves of alternately stacked rGO/CNT consisting of 16 rGO and 15 CNT layers at various scan rates in the range of 0 to 1V, (b) Galvanostatic charge-discharge curves of four samples at a current density of 2 ⁇ /cm 2 , (c) Nyquist plots for different samples over the frequency range from 1 MHz to 10 mHz. Inset: Enlarged plots in the high frequency region, (d) Cycling performance of representative samples at a current density of 5 juA/cm 2 for 3000 cycles, (e) The volumetric capacitance of the representative samples calculated from Galvanostatic
  • Figure 3 shows (a) galvanostatic charge/discharge curves of layer- by-layer stacked rGO/CNT (L-rGO/CNT) supercapacitor with different number of layers at a current density of 2 ⁇ /cm 2 , (b) Areal capacitances calculated for L-rGO/CNT with different number of layers and unit areal capacitances by dividing them by the number of layers (N), and (c, d) Increase in the output voltage and current via tandem serial and parallel electrochemical capacitors. Galvanostatic charge/discharge curves for a single cell and two/four cells connected in series (c) and in parallel (d) under the same constant current conditions.
  • L-rGO/CNT layer- by-layer stacked rGO/CNT
  • Figure 4 shows (a) a digital image of the large-sized planar stacked rGO/CNT supercapacitor and the stacked geometry, (b) CV curves of alternately stacked rGO/CNT consisting of 16 rGO and 15 CNT layers at various scan rates, (c) Galvanostatic charge-discharge curves of the sample at a current of 70 ⁇ , and (d) Nyquist plots over the frequency range from 1 MHz to 10 mHz. Inset: Enlarged plots in the high frequency region.
  • An ultrathin planar supercapacitor electrode by alternatively stacking multilayers of reduced graphene oxide (rGO) and multi-walled CNTs without the need of any binding materials is disclosed.
  • two-dimensional monolayer assemblies of rGO and multi-walled CNTs were separately formed at the air/water interface and these films were readily transferred onto a solid substrate, repeatedly, to fabricate an alternating multi-stacked electrode.
  • This in-plane architecture embedded with CNTs between rGO layers can enhance the interaction of electrolyte ions with all graphene layers leading to the full utilization of the high surface area of the graphene sheets, which can be important for thin film-based supercapacitors.
  • the stacked multilayers of rGO and CNTs can be capable of offering higher output voltage and current production via serial and parallel connections.
  • a large-scale (5x7 cm 2 ) stacked supercapacitor has been demonstrated without sacrificing the electrochemical performance.
  • Figure 1A shows the overall process of fabricating the stacked multilayers of rGO/CNT (L-rGO/CNT) for supercapacitor electrodes.
  • the rGO was firstly prepared by a modified Hummer's method, followed by reduction in an aqueous solution with N 2 H 4 .
  • Multi-walled CNTs were treated with a mixture of H 2 SO and HNO 3 to render them dispersible in polar solvents.
  • To form a 2D assembly rGO and CNTs were firstly dispersed in alcohol (for example, ethanol, IPA, 1 -butanol) and then dropped on water surface with a pipette.
  • alcohol for example, ethanol, IPA, 1 -butanol
  • rGO sheets or CNTs spread on the water surface, then become trapped at the air/water interface, and finally produce closely- packed assembly.
  • the 2D monolayer of rGO was first collected on a current collector and then a CNT layer was gathered on the same substrate.
  • the reduced graphene oxide nanosheets can be atomically-thin, leading to overlapped or crumpled areas due to the limited available air/water interface.
  • CNTs also overlap to appear as a fabric. This process was repeated, sequentially, to make an alternating multi-stacked rGO/CNT electrode.
  • This layer-by-layer (LBL) electrochemical device structure can alleviate agglomeration of the 1 D and 2D carbon nanomaterials and can maximize the utilization of the surface of the graphene nanosheets to guarantee the permeation of electrolyte ions and reliable mechanical adhesion of the active materials to the current collector.
  • Figures 1 b and 1 c show TEM images of stacked rGO/CNT films exposing CNT and rGO layers on the top, respectively.
  • the inset in Figure 1 b shows the rGO/CNT film in which the CNT fabric is well adhered to the bottom of the rGO layer.
  • This layer-by-layer deposition of rGO and CNT in a sequential manner ensures full coverage of each nanomaterial, which can be important in planar supercapacitor devices in terms of uniform orientation with respect to the current collector.
  • a mixture solution of rGO and CNT in ethanol 0.5 mg/mL for both
  • the resultant film after transferring to a substrate shows partial coverage or phase separation due to a lack of strong interactions between the two components.
  • graphene oxide nanosheets possess amphiphilic properties corresponding to their hydrophilic edges from ionizable carbonyl/carboxyl groups and the more hydrophobic basal plane.
  • the ⁇ - ⁇ attraction between the hydrophobic plane of GO and CNTs can be considerably weak and non-uniform as the amphiphilicity of GO varies by the degree of reduction and the ⁇ -conjugated domains in CNTs have been significantly disrupted after acid treatment.
  • each CNT layer can be sandwiched between two rGO layers, producing uniform films with thicknesses
  • the CNT layers can serve as well-defined porous spacers that not only prevent restacking of rGO sheets but also provide sufficient separation between the wrinkled rGO nanosheets to ensure efficient permeation of electrolyte ions.
  • polymer gel electrolyte can serve as an ionic electrolyte as well as a separator, enabling a new supercapacitor design.
  • Figure 2d presents the cyclic performance of each device, indicating a better stability of the CNT-incorporated rGO devices (L- rGO/CNT and R-rGO/CNT) than the rGO device.
  • the capacitance value calculated from the discharge curves after 3000 cycles improved from 34% (rGO) to 10% (L-rGO/CNT).
  • the L-rGO/CNT electrode can effectively absorb the gel electrolyte and act as an efficient electrolyte reservoir because the porous CNT layer can facilitate ion transport and minimize the diffusion length to the interior surface of the rGO nanosheets.
  • This synergistic effect originates from the large active surface area of the rGO nanosheets, which can be maintained due to the prevention of agglomeration through the intercalation of CNT layers, which in turn improves the conductivity of the device.
  • this layer-by-layer process requires no organic binder, and thus enables a reduction in interfacial resistance and enhances the chemical reaction rate.
  • Figure 2f shows the Ragone plots of the four types of devices indicating the overall performance based on the specific volume of the whole device.
  • the same area (1 x1 cm 2 ) of electrodes was used for calculation.
  • the thickness of each device was in the range of 60.1 pm (rGO), 60.3 pm (CNT), 60.4 pm (R-rGO/CNT), and 60.4 pm (L-rGO/CNT) because the active layers are too thin compared to the electrolyte (about 10 pm) and current collector (2x25 pm).
  • the L-rGO/CNT electrode shows better energy density compared to the other devices.
  • one advantage of the L-rGO/CNT supercapacitor can lie in the feasibility of controlling its electrochemical performance by changing the thickness of the active layer.
  • Figure 3a shows galvanostatic charge/discharge curves of four L- rGO/CNT electrodes comprising different numbers of layers. For example, the runtime of the charging/discharging increases with the number of layers, indicating efficient control over the capacitance value. The areal
  • the unit capacitances as calculated by dividing each areal capacitance by the number of layers (blue dots), was found to be in the range of 0.181 ⁇ 0.042 mF/cm 2 .
  • the unit capacitances as calculated by dividing each areal capacitance by the number of layers (blue dots), was found to be in the range of 0.181 ⁇ 0.042 mF/cm 2 .
  • porous CNT buffer layers between rGO layers can enable a simple layer-by-layer alternating stacking scheme for constructing efficient electrochemical energy storage devices whose performance can be conveniently controlled by the number of layers.
  • Aqueous electrolyte can operate only in the voltage range of 0 to 1V, which can be limited to a small number of applications.
  • portable devices often require cell packaging either in series, in parallel, or in a combination of the two methods to meet energy and power requirements.
  • it can be important to develop an electrochemical energy storage device with control over the operating voltage and current by constructing tandem serial and parallel assemblies while minimizing energy loss.
  • Figure 3d shows galvanostatic charge/discharge curves of parallel tandem structures under the same constant current conditions.
  • the charging and discharging time of the L-rGO/CNT supercapacitor increases by a factor of two and four when connecting two and four devices, respectively.
  • the tandem devices in series and in parallel
  • a large substrate (5x7 cm 2 ) was introduced as a current collector to stack rGO nanosheets and CNT layers in a layer-by-layer manner.
  • Figure 4a shows a digital image of the large-sized L-rGO/CNT electrodes after covering polymer gel electrolyte.
  • the device architecture is the same as that of the small L-rGO/CNT electrodes (1 x1 cm 2 ) as depicted in the scheme.
  • the electrochemical properties were measured under the same conditions.
  • Cyclic voltammography (CV) curves of the large-sized L- rGO/CNT device show a nearly rectangular shape at every scan rate (2 to 100 mV/s), indicating an efficient establishment of an electric double layer (Figure 4b).
  • Galvanostatic charge/discharge curves in also exhibit the same trend as the regular-sized L-rGO/CNT device except for a large increase of capacitance according to the increased size of the active layers.
  • the CD curves are close to a triangular shape, signifying the formation of an efficient EDL and good charge transport across the planar electrodes.
  • the large-sized L-rGO/CNT electrode exhibits stable cycling performance at five different current densities.
  • the Nyquist plots from electrochemical impedance spectra display a good capacitive behavior with small internal resistance as seen in the inset in Figure 4d.
  • a layer-by-layer approach for the construction of 2D planar ultrathin supercapacitors of multi- stacked rGO and CNTs has been disclosed.
  • This 2D in-plane architecture allows for the formation of an efficient electrical double layer and the utilization of the maximum active surface area of rGO nanosheets by using a CNT layer as a porous physical spacer to enhance the permeation of gel electrolyte inside the structure and reduce the agglomeration of rGO nanosheets along the out-of-plane axis.
  • the electrochemical performance can be increased simply by controlling the number of layers and constructing serial/parallel tandem architectures.
  • the proposed LBL process can be extended to the fabrication of a large-sized ultrathin supercapacitor without diminishing its electrochemical properties, which is critically important in a practical energy storage device.
  • Graphene oxide (GO) was synthesized from high purity graphite flake powder using a modified Hummer's method with an improved purification method and then reduced by chemical reduction.
  • the exfoliated graphene oxide was redispersed in 20 mL of water (0.5 mg/mL) after sonication for h (one hour), then mixed with water (20 mL), N2H4 (60 pL), and NH 4 OH (420 pL). After heating the reaction at 70 °C for 1 h, the sample was washed with H 2 O three times.
  • Fabrication of the solid-state stacked supercapacitor Fabrication of the solid-state stacked supercapacitor.
  • Reduced graphene oxide nanosheets and CNTs were redispersed in ethanol and 1-butanol, respectively. These suspensions were dropped on a water surface in separate Petri dishes until a robust film was formed. The film was scooped up by a substrate, repeatedly, to make a multi-layer film. All solid-state devices were assembled by pouring polymer gel electrolyte (100 pL/cm 2 ) onto the stacked rGO/CNT electrodes. The device was left overnight in a desiccator for complete drying of the gel electrolyte.
  • the area of the electrodes was confined to 1 x1 cm 2 (5 x 7 cm 2 for the large-sized electrodes).
  • Electrochemical impedance spectra (EIS) experiments were carried out at an open circuit potential with a sinusoidal signal with an amplitude of 10 mV in a frequency range of 1 MHz to 10 mHz. [0038] When the word "about” is used in this specification in connection with a numerical value, it is intended that the associated numerical value include a tolerance of ⁇ 10% around the stated numerical value.

Abstract

La présente invention concerne une approche couche-par-couche de la construction de supercondensateurs planaires ultrafins 2D (bidimensionnels) composés de plusieurs rGO (oxydes de graphène réduits) et nanotubes de carbone empilés. L'architecture dans le plan 2D peut permettre la formation d'une double couche électrique efficace et l'utilisation de la surface active maximale de nanofeuilles de rGO en utilisant une couche de CNT comme espaceur physique poreux afin d'améliorer la pénétration de gel électrolyte à l'intérieur de la structure et de réduire l'agglomération de nanofeuilles de rGO le long de l'axe hors du plan. La performance électrochimique peut être augmentée par le contrôle du nombre de couches et la construction d'architectures en tandem en série/parallèle. En outre, le procédé couche-par-couche peut être étendu à la fabrication d'un supercondensateur ultramince de grande taille sans diminuer ses propriétés électrochimiques, ce qui peut être important dans un dispositif de stockage d'énergie pratique.
PCT/US2014/060232 2013-10-11 2014-10-13 Multicouches empilées d'oxyde de graphène réduit et de nanotubes de carbone en alternance pour supercondensateurs planaires ultra-minces WO2015126464A2 (fr)

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Cited By (8)

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CN105679548A (zh) * 2016-01-08 2016-06-15 国网智能电网研究院 一种用于石墨烯基超级电容器的电极极片及其制备方法
CN108147392A (zh) * 2018-01-16 2018-06-12 西南大学 用于3d打印的碳纳米管/金属混合溶液的制备方法
CN109243670A (zh) * 2018-09-14 2019-01-18 昆明理工大学 一种增强三维石墨烯骨架结构制备三维石墨烯/高分子聚合物复合材料的方法
CN109273287A (zh) * 2018-08-17 2019-01-25 同济大学 一种自愈合水凝胶聚电解质及其制备与应用
CN109904002A (zh) * 2019-01-14 2019-06-18 清华大学 一种低阻抗电极的制备方法及低阻抗电极
CN110054174A (zh) * 2019-04-09 2019-07-26 中国人民解放军军事科学院军事医学研究院 氮掺杂碳基复合材料及其制备方法与应用
EP3435392A4 (fr) * 2016-03-22 2019-11-20 National Institute for Materials Science Procédé permettant de produire un stratifié de graphènes et de nanotubes de carbone, matériau d'électrode constitué d'un stratifié de graphènes et de nanotubes de carbone et condensateur électrique à double couche utilisant ce dernier
WO2019079723A3 (fr) * 2017-10-19 2020-04-02 Cornell University Cathodes au lithium-oxygène en couches

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US8182917B2 (en) * 2008-03-20 2012-05-22 The United States Of America, As Represented By The Secretary Of The Navy Reduced graphene oxide film
US8520365B2 (en) * 2010-04-18 2013-08-27 Amperics Inc. Charge storage device architecture for increasing energy and power density
CN103153843B (zh) * 2010-12-30 2014-04-02 海洋王照明科技股份有限公司 石墨烯衍生物-碳纳米管复合材料及其制备方法

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105679548A (zh) * 2016-01-08 2016-06-15 国网智能电网研究院 一种用于石墨烯基超级电容器的电极极片及其制备方法
CN105679548B (zh) * 2016-01-08 2019-11-01 国网智能电网研究院 一种用于石墨烯基超级电容器的电极极片及其制备方法
EP3435392A4 (fr) * 2016-03-22 2019-11-20 National Institute for Materials Science Procédé permettant de produire un stratifié de graphènes et de nanotubes de carbone, matériau d'électrode constitué d'un stratifié de graphènes et de nanotubes de carbone et condensateur électrique à double couche utilisant ce dernier
WO2019079723A3 (fr) * 2017-10-19 2020-04-02 Cornell University Cathodes au lithium-oxygène en couches
CN108147392A (zh) * 2018-01-16 2018-06-12 西南大学 用于3d打印的碳纳米管/金属混合溶液的制备方法
CN108147392B (zh) * 2018-01-16 2020-10-30 西南大学 用于3d打印的碳纳米管/金属混合溶液的制备方法
CN109273287A (zh) * 2018-08-17 2019-01-25 同济大学 一种自愈合水凝胶聚电解质及其制备与应用
CN109243670A (zh) * 2018-09-14 2019-01-18 昆明理工大学 一种增强三维石墨烯骨架结构制备三维石墨烯/高分子聚合物复合材料的方法
CN109904002A (zh) * 2019-01-14 2019-06-18 清华大学 一种低阻抗电极的制备方法及低阻抗电极
CN110054174A (zh) * 2019-04-09 2019-07-26 中国人民解放军军事科学院军事医学研究院 氮掺杂碳基复合材料及其制备方法与应用

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