CN113936929B - Preparation method of dual-ion supercapacitor - Google Patents

Preparation method of dual-ion supercapacitor Download PDF

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CN113936929B
CN113936929B CN202111258934.1A CN202111258934A CN113936929B CN 113936929 B CN113936929 B CN 113936929B CN 202111258934 A CN202111258934 A CN 202111258934A CN 113936929 B CN113936929 B CN 113936929B
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CN113936929A (en
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刘博天
石成龙
庞有勇
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Guilin University of Technology
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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
    • H01G11/84—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
    • 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
    • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • 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
    • 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
    • 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
    • H01G11/46—Metal oxides
    • 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
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • 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
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    • Y02E60/13—Energy storage using capacitors

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Abstract

A preparation method of a battery type anode-pseudo-capacitive type cathode-based dual-ion super capacitor is disclosed. (1) Commercial nickel foil is pretreated by cleaning and the like, and then Ni (OH) is successfully prepared by the processes of electrodeposition, dealloying, in-situ oxidation and the like 2 And (3) a nanotube array anode. (2) The CNTs film is obtained by a commercial Carbon Nano Tube (CNT) through ultrasonic dispersion and vacuum filtration. (3) Electrodeposition of V on CNTs films 2 O 5 Obtaining a self-supporting V 2 O 5 a/CNTs negative electrode. (3) And (3) separating the positive electrode and the negative electrode through a diaphragm, and assembling the positive electrode and the negative electrode into the double-ion supercapacitor in the KOH electrolyte. The dual-ion supercapacitor is different from the traditional supercapacitor, and utilizes a novel energy storage mechanism: on charging, OH ‑ Coming to the positive electrode and Ni (OH) 2 Oxidation reaction occurs, ni 2+ Is oxidized into Ni 3+ ,K + Coming into negative electrode embedded V 2 O 5 (ii) a On discharge, OH ‑ Returning electrolyte from the positive electrode, and reducing the positive electrode material to Ni (OH) 2 ，K + V from the negative electrode 2 O 5 Then the electrolyte is released and returned to the electrolyte. The double-ion super capacitor has excellent electrochemical performance and good application prospect in the field of energy storage.

Description

Preparation method of dual-ion supercapacitor
Technical Field
The invention relates to the field of electrochemical energy storage devices, in particular to a preparation method of a battery type anode-pseudocapacitive type cathode-based dual-ion supercapacitor.
Background
With the growth of human population and the development of industrial technology, the consumption of fossil energy is dramatically increased, causing serious environmental pollution. Therefore, the development of efficient, clean and sustainable green energy is urgently needed. Renewable energy sources such as wind, water, solar, etc. are the most promising solutions. However, the intermittency of these clean energy sources makes them unable to be directly incorporated into the power supply network, and efficient electrochemical energy storage systems are key technologies to improve the intermittency of renewable energy sources and increase the utilization ratio of renewable energy sources. The super capacitor has the advantages of high power density, long cycle life, low manufacturing cost and the like.
It is well known that conventional supercapacitors utilize a single ion (K) + 、Na + 、OH - 、SO 4 2- Etc.) to perform redox reaction on the surface of the electrode material of the positive electrode and the negative electrode to realize energy storage, and a super capacitor for storing energy by utilizing multiple ions is lacked. In view of this, the present invention provides a novel super capacitor for storing energy based on a battery type positive electrode-pseudocapacitive type negative electrode dual-ion energy storage mechanism. Specifically, upon charging, OH - Coming to the positive electrode and Ni (OH) 2 Reaction takes place, K + Coming into negative electrode embedded V 2 O 5 (ii) a On discharge, OH - Returning electrolyte from the positive electrode, and reducing the positive electrode material to Ni (OH) 2 ，K + V from the negative electrode 2 O 5 Then the electrolyte is released and returned to the electrolyte. The invention uses a brand-new charge storage mechanism to promote the storage of the charge and realizes high specific capacity, thereby obviously improving the energy density of the super capacitor. The novel energy storage mechanism and the excellent electrochemical performance of the invention enable the invention to have good application prospect in the field of super capacitors.
Disclosure of Invention
The invention provides a design method of a double-ion super capacitor, which can effectively improve the energy density of a device by utilizing a brand new energy storage mechanism. Wherein an anion (OH) is stored - ) The key positive electrode material of (2) can include NiO, ni (OH) 2 、Co(OH) 2 、Co 3 O 4 A complex of one or more of (a).
The technical scheme adopted by the invention is as follows:
the method comprises the following steps: preparing a Ni (OH) 2 nanotube array anode:
(1) Ultrasonically cleaning a metal foil in deionized water and ethanol, and drying in an oven;
(2) Preparing NiSO with a certain concentration 4 、CuSO 4 、H 3 BO 3 In the mixed solution, a Pt sheet is used as a counter electrode, a nickel foil is used as a working electrode, ag/AgCl is used as a reference electrode through an electrodeposition technology, a Ni-Cu alloy film is prepared through constant voltage electrodeposition for a period of time under a certain potential, and then Cu is removed in the same electrolyte at a constant potential to obtain the Ni nanotube array film.
(3) The method comprises the steps of using a three-electrode system, taking a Pt sheet as a counter electrode, ag/AgCl as a reference electrode and a Ni nanotube array film as a working electrode, and oxidizing the Ni nanotube array into Ni (OH) in situ in KOH electrolyte with a certain concentration by a cyclic voltammetry method 2 。
Step two: the self-supporting V 2 O 5 The preparation steps of the/CNTs negative electrode are as follows:
(1) Commercial CNTs were dispersed with Sodium Dodecylbenzenesulfonate (SDBS) in deionized water by sonication, and then a certain amount of the suspension was vacuum filtered to prepare CNTs films.
(2) Preparing VOSO with a certain concentration by taking CNTs film as a working electrode 4 Preparation of self-supporting V with mixed solution of cetyltrimethylammonium bromide (CTAB) by potentiostatic electrodeposition 2 O 5 a/CNT electrode.
(3) Will be self-supporting V 2 O 5 the/CNT electrode is put in a tube furnace for high-temperature annealing.
Step three: assembling the double-ion super capacitor:
(1) The Ni (OH) obtained in the first step and the second step 2 Nanotube array anode and self-supporting V 2 O 5 the/CNTs negative electrode is assembled in KOH electrolyte by separating with a diaphragm.
The metal foil used in the step (1) in the first step is nickel foil, and the ultrasonic cleaning time is 10-60 min.
NiSO in the step (2) of the first step 4 The concentration of (A) is 0.5-2M 4 The concentration is 0.01-0.05M, H 3 BO 3 The concentration of the copper is 0.1-1M, the voltage of constant potential deposition is-0.6-1V, the deposition time is 5-30 min, the potential for removing Cu is 0.4-0.8V, and the time is 10-60 min.
KOH in step (3) of step oneThe concentration is 1-3M, the voltage window of cyclic voltammetry is 0-0.6V, and the sweep rate is 5-100 mV s -1 The number of the circulating circles is 10-100 circles.
In the step (1) of the second step, the concentration of CNT is 0.5-5 mg/ml, the concentration of SDBS is 0.1-1 mg/ml, the ultrasonic time is 1-5 h, and the volume of the suction filtration suspension is 100-300 ml.
VOSO in the second step (2) 4 The concentration of (A) is 0.2-2M, the concentration of CTAB is 0.1-0.3M, the deposition potential is 1-2V, and the deposition time is 5-10 min.
And (3) annealing at 300-500 deg.c for 2-6 hr in argon atmosphere.
And in the third step (1), the concentration of the KOH electrolyte is 1-6M.
Drawings
FIG. 1 shows a positive electrode material Ni (OH) 2 Scanning Electron Microscope (SEM) images of nanotube array electrodes;
FIG. 2 is a schematic view of a self-supporting V of the negative electrode material 2 O 5 SEM image of/CNT electrode;
FIG. 3 shows CNT film and self-supporting V 2 O 5 XRD spectrogram of/CNT electrode;
in FIG. 4, ni (OH) is on the upper side 2 The XRD pattern of the nanotube array electrode is the XRD pattern of the Ni-Cu alloy film;
FIG. 5 is a cyclic voltammogram of a bi-ionic supercapacitor at different scan rates;
FIG. 6 is a constant current charge and discharge curve of a dual-ion supercapacitor at different current densities;
FIG. 7 shows a dual ion supercapacitor at 100mV s -1 Capacity retention rates of different turns at the sweep rate of (1);
fig. 8 is a Ragone diagram of a dual ion supercapacitor.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be described explicitly and completely below. The examples, in which specific conditions are not specified, were carried out under conventional conditions or conditions recommended by the manufacturer. The reagents and apparatus used are conventional products which are commercially available, not indicated by the manufacturer. The embodiments of the invention will be further described with reference to the accompanying drawings and specific implementation thereof:
step one, ni (OH) 2 The specific preparation process of the nanotube array anode is as follows:
(1) Commercial nickel foil was ultrasonically cleaned using deionized water and ethanol for 10min, respectively, and dried at 80 ℃ for 5h.
(2) Preparation of 1M NiSO 4 、0.05M CuSO 4 、0.5M H 3 BO 3 The mixed solution is deposited for 10min under the constant potential of-0.8V, and the Ni nanotube array is prepared by applying the constant potential of 0.5V for 20min in the same electrolyte.
(3) In a 1M KOH electrolyte, at 10mV s -1 Under the sweep speed, the cyclic voltammetry is 100 circles, the voltage window is 0-0.6V, and the Ni nanotube array is oxidized into Ni (OH) 2 。
Step two, the self-supporting V 2 O 5 The specific preparation process of the/CNT electrode is as follows:
(1) Ultrasonically dispersing 200ml of suspension with the CNT concentration of 1mg/ml and the SDBS concentration of 0.2mg/ml for 3 hours, then performing vacuum filtration to obtain a self-supporting CNTs current collector, and washing the surfactant with deionized water during the filtration.
(2) Using the CNTs current collector prepared in (1) as a working electrode in VOSO 4 In a mixed solution with a concentration of 1M and a CTAB concentration of 0.2M, a self-supporting V is prepared by depositing for 10min at a potential of 1.5V by using a constant voltage electrodeposition technique 2 O 5 a/CNTs electrode.
(3) In a tube furnace under argon atmosphere, the self-supporting V 2 O 5 the/CNTs electrode was annealed at 400 ℃ for 3h.
Step three, assembling the double-ion super capacitor:
(1) Mixing Ni (OH) 2 Nanotube array anode and self-supporting V 2 O 5 the/CNT negative electrode is separated by a diaphragm and is immersed in 2M KOH electrolyte to be assembled into a dual-ion super capacitor
The electrochemical test method of the double-ion supercapacitor comprises the following steps: at 10-100 mV s -1 Performing cyclic voltammetry tests at different sweep speeds of 1.2-3 mA cm -2 The constant current charge and discharge test is carried out under different current densities, and the power density and the energy density are calculated and are 100mV s -1 The cyclic stability of the device is tested at the sweep speed of 10000 cycles of cyclic voltammetry.
Ni(OH) 2 Nanotube array anode and self-supporting V 2 O 5 The morphology and phase of the/CNTs negative electrode are characterized as follows: and (5) characterizing the surface topography of the sample by SEM. As shown in FIG. 1, ni (OH) was successfully prepared on a nickel foil 2 An array of nanotubes, the nanotubes having an aperture of about 100nm. It can be seen from FIG. 2 that a layer V is deposited on the surface of the carbon nanotube by the electrodeposition technique 2 O 5 。
Characterization of the phase of the sample by XRD spectrogram, CNT film and V in FIG. 3 2 O 5 Comparison of XRD spectrograms of self-supporting electrodes shows that V with good crystallinity is successfully deposited on CNTs thin film by using electrodeposition 2 O 5 . FIG. 4 shows a Ni-Cu alloy thin film and Ni (OH) 2 The comparison of the XRD spectrogram of the nanotube array shows that the Cu in the alloy film is successfully removed, and the Ni is successfully oxidized into Ni (OH) 2 。
The electrochemical test results are as follows:
as shown in FIG. 5, the sweep rate in the cyclic voltammetry test of the dual ion supercapacitor ranged from 10 to 100mV s -1 Obtaining cyclic voltammograms at different scan rates at 10mV s -1 The specific area capacity of the dual-ion supercapacitor obtained by calculation at the scanning speed is up to 127mF cm -2 . At 1.2-3 mA cm -2 Constant current charge and discharge tests are carried out under different current densities, and the fact that the potential changes linearly along with time can be seen from figure 6, which shows that the constant current charge and discharge test circuit has good rate performance.
FIG. 7 shows the device at 100mV s -1 The capacity retention rate of the dual-ion supercapacitor after 10000 cycles is 94.7%, which shows an ultra-long cycle life.
FIG. 8 is a graph of a calculationThe Ragon graph of the obtained double-ion super capacitor is 0.821mW cm -2 The area energy density is as high as 29.7 mu Wh cm -2 . Even at 5.34mW cm -2 Still 19.27. Mu. Wh cm at a high area power density -2 Area energy density of (1). The excellent electrochemical performance shows that the dual-ion super capacitor utilizing the novel energy storage mechanism has a good application prospect, and the dual-ion super capacitor is a good development direction in the field of energy storage.

Claims (8)

1. A preparation method of a battery type anode-pseudocapacitance type cathode-based dual-ion super capacitor is characterized by comprising the following steps:
the method comprises the following steps: ni (OH) 2 Preparing a nanotube array anode:
(1) Ultrasonically cleaning a metal foil in deionized water and ethanol, and drying in an oven;
(2) Preparing NiSO with a certain concentration 4 、CuSO 4 、H 3 BO 3 In the mixed solution, preparing a Ni-Cu alloy film by constant voltage electrodeposition for a period of time at a certain potential by taking a Pt sheet as a counter electrode, a nickel foil as a working electrode and Ag/AgCl as a reference electrode through an electrodeposition technology, and then removing Cu at a constant potential in the same electrolyte to obtain a Ni nanotube array film;
(3) The method comprises the steps of using a three-electrode system, taking a Pt sheet as a counter electrode, ag/AgCl as a reference electrode and a Ni nanotube array film as a working electrode, and oxidizing the Ni nanotube array into Ni (OH) in situ in KOH electrolyte with a certain concentration by a cyclic voltammetry method 2 ；
Step two: self-supporting V 2 O 5 The preparation steps of the/CNT negative electrode are as follows:
(1) Dispersing commercial CNT and Sodium Dodecyl Benzene Sulfonate (SDBS) in deionized water by ultrasonic, and then preparing a CNTs film by vacuum filtration of a certain amount of suspension;
(2) Preparing VOSO with a certain concentration by using CNTs film as a working electrode 4 Mixing with Cetyl Trimethyl Ammonium Bromide (CTAB), and performing constant potential electrodepositionSurgical preparation of self-supporting V 2 O 5 a/CNTs electrode;
(3) Will be self-supporting V 2 O 5 Placing the/CNTs electrode in a tube furnace for high-temperature annealing;
step three: assembling the double-ion super capacitor:
(1) Mixing the Ni (OH) obtained in the first step and the second step 2 Nanotube array anode and self-supporting V 2 O 5 the/CNTs negative electrode is assembled in KOH electrolyte by separating with a diaphragm.
2. The method for preparing the battery type positive electrode-pseudocapacitance type negative electrode-based double-ion supercapacitor according to claim 1, wherein in the step (1) of the first step, the metal foil is nickel foil, and the ultrasonic time is 10-60 min.
3. The method for preparing the battery-type anode-pseudocapacitive-type cathode-based dual-ion supercapacitor according to claim 1, wherein the NiSO in step (2) of step one 4 The concentration of (A) is 0.5-2M 4 The concentration is 0.01-0.05M 3 BO 3 The concentration of the copper is 0.1-1M, the voltage of constant potential deposition is-0.6-1V, the deposition time is 5-30 min, the potential for removing Cu is 0.4-0.8V, and the time is 10-60 min.
4. The method for preparing the battery type positive electrode-pseudocapacitance type negative electrode-based double-ion supercapacitor according to claim 1, wherein the concentration of KOH in the step (3) of the first step is 1-3M, the voltage window of cyclic voltammetry is 0-0.6V, and the sweep rate is 5-100 mV s -1 The number of the circulation circles is 10-100 circles.
5. The preparation method of the battery type positive electrode-pseudocapacitance type negative electrode-based double-ion supercapacitor as claimed in claim 1, wherein the concentration of CNT in the second step (1) is 0.5-5 mg/ml, the concentration of SDBS is 0.1-1 mg/ml, the ultrasonic time is 1-5 h, and the volume of the suction filtration suspension is 100-300 ml.
6. The method for preparing the battery-type anode-pseudocapacitive-type cathode-based dual-ion supercapacitor according to claim 1, wherein in the second step (2), VOSO is added 4 The concentration of the CTAB is 0.2-2M, the concentration of the CTAB is 0.1-0.3M, the deposition potential is 1-2V, and the deposition time is 5-10 min.
7. The method for preparing the battery-type anode-pseudocapacitive-type cathode-based double-ion supercapacitor according to claim 1, wherein in the second step (3), annealing is performed under the atmosphere of argon under the annealing condition of 300-500 ℃ for 2-6 hours.
8. The method for preparing the battery type positive electrode-pseudocapacitance type negative electrode-based double-ion supercapacitor according to claim 1, wherein the concentration of KOH electrolyte in the third step (1) is 1-6M.
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Publication number Priority date Publication date Assignee Title
CN110853938A (en) * 2019-11-22 2020-02-28 吉林建筑大学 Symmetrical super capacitor
CN112382513A (en) * 2020-10-01 2021-02-19 桂林理工大学 Preparation method of double-ion water system energy storage device

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110853938A (en) * 2019-11-22 2020-02-28 吉林建筑大学 Symmetrical super capacitor
CN112382513A (en) * 2020-10-01 2021-02-19 桂林理工大学 Preparation method of double-ion water system energy storage device

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