CN113223865A - Vanadium oxide electrode material with nanorod structure and preparation method and application thereof - Google Patents
Vanadium oxide electrode material with nanorod structure and preparation method and application thereof Download PDFInfo
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- 229910001935 vanadium oxide Inorganic materials 0.000 title claims abstract description 49
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000007772 electrode material Substances 0.000 title claims abstract description 14
- 239000002073 nanorod Substances 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000004744 fabric Substances 0.000 claims abstract description 61
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 58
- 238000002484 cyclic voltammetry Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000004070 electrodeposition Methods 0.000 claims abstract description 10
- 230000004913 activation Effects 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims description 27
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000003792 electrolyte Substances 0.000 claims description 23
- 238000001291 vacuum drying Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 150000001721 carbon Chemical class 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 7
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Inorganic materials [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 229910000352 vanadyl sulfate Inorganic materials 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 5
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical group [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 claims description 5
- 239000011149 active material Substances 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 238000010408 sweeping Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- -1 vanadium oxide compound Chemical class 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 230000003213 activating effect Effects 0.000 abstract description 2
- 239000013049 sediment Substances 0.000 abstract description 2
- 238000009827 uniform distribution Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 11
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- 238000004146 energy storage Methods 0.000 description 7
- 238000005520 cutting process Methods 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- 239000003990 capacitor Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000013543 active substance Substances 0.000 description 1
- 238000007600 charging Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010277 constant-current charging Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
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- H—ELECTRICITY
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- 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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
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- 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
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- H01G11/46—Metal oxides
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- 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
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Abstract
The invention belongs to the technical field of new energy, and particularly relates to a vanadium oxide electrode material with a nanorod structure, and a preparation method and application thereof. Firstly, arranging carbon under a three-electrode system, activating by adopting a cyclic voltammetry method, then performing electrodeposition of vanadium oxide, and drying to obtain the vanadium oxide with the nano rod-like structure. According to the invention, the specific capacity of the carbon cloth is firstly improved by a surface activation method, the number of oxygen-containing functional groups on the surface of the carbon cloth is increased, and then a layer of vanadium oxide is plated on the surface of the carbon cloth by an electrodeposition method, so that the pseudo capacitance of the electrode material is improved. The method has the advantages of simple operation and short preparation time, and vanadium oxide sediments with a nanorod structure and uniform distribution are obtained on the treated carbon cloth, so that the area specific capacitance is higher.
Description
Technical Field
The invention belongs to the technical field of new energy, and particularly relates to a vanadium oxide electrode material with a nanorod structure, and a preparation method and application thereof.
Background
In the face of increasingly severe energy crisis and environmental issues, it is becoming increasingly important to develop efficient and reliable electrochemical energy storage systems. As a novel energy storage device, the super capacitor is widely concerned due to the advantages of high power density, high charging and discharging speed, long cycle life and the like, and has very wide application prospect. The current commercialized super capacitor generally adopts activated carbon as an electrode material, and has a major disadvantage of low energy density, while the metal oxide material stores energy by pseudo capacitance and has much higher energy density than activated carbon, thus becoming one of the current popular research subjects. Vanadium oxide has rich redox valence states, and the multi-valence state is accompanied with the Faraday reaction process of multiple electrons, so vanadium oxide has higher pseudocapacitance. Meanwhile, the vanadium oxide electrode material has a flexible and easily-controlled energy storage potential interval, can store energy in a large potential window, and effectively improves the energy density of the super capacitor.
Disclosure of Invention
The invention provides an electrode material with high specific capacitance, high rate performance and long cycle life by activating the carbon cloth, increasing the number of oxygen-containing functional groups on the surface of the carbon cloth and plating a layer of vanadium oxide on the modified carbon cloth.
The technical scheme adopted by the invention is as follows: a vanadium oxide electrode material with a nano rod-like structure is prepared by the following steps:
1) and (3) placing the carbon cloth under a three-electrode system for activation treatment: at KNO3Activating carbon cloth in electrolyte by adopting a potentiostatic method, cleaning the activated carbon cloth by using deionized water, then placing the carbon cloth in a three-electrode system, and recovering the electrode conductivity in a KCl solution within a certain potential range by adopting a cyclic voltammetry method;
2) active material deposition: preparing a solution containing vanadium, and performing electrodeposition of vanadium oxide on the carbon cloth obtained in the step 1) by adopting a cyclic voltammetry methodThe product is in the potential range of-1.5 to 1.5V and is calculated by 50mV s-1Performing cyclic voltammetry scanning at the scanning speed of 100-;
3) and soaking the carbon cloth deposited with the vanadium oxide compound in deionized water for 2-5 min to remove redundant electrolyte, and then drying in a vacuum drying oven at 60 ℃ for 8h to obtain the vanadium oxide nano rod-like structure.
In the preparation method, in the step 1), before the modification of the carbon cloth, the carbon cloth is washed by ethanol and deionized water, then is placed into the deionized water for ultrasonic cleaning, and then is dried in a vacuum drying oven at 60 ℃.
In the above preparation method, step 1), the potentiostatic conditions are as follows: the potential is 1.8V, and the reaction time is 2.5-3 h.
In the preparation method, in step 1), the conditions for recovering the conductivity of the electrode by using cyclic voltammetry are as follows: the potential is-1.2 to 1V, and the sweeping speed is 50 to 100mV s-1The number of scanning turns: 50-100 circles.
In the preparation method, in the step 1), the modified carbon cloth needs to be washed by deionized water.
In the preparation method, in the step 1), carbon cloth is used as a working electrode, carbon paper is used as a counter electrode, and a saturated calomel electrode is used as a reference electrode under a three-electrode system.
The preparation method comprises the step 2), wherein the solution containing vanadium is VOSO according to the molar ratio4：(NH4)2Ac is 1: 2.
In the preparation method, in the step 2), the number of cyclic voltammetry scanning cycles is as follows: 100. 300 and 500 circles.
The vanadium oxide electrode material with the nanorod structure is applied to a super capacitor.
The invention has the beneficial effects that:
1. the invention relates to a nano-rod-shaped vanadium oxide electrode material and a preparation method and application thereof, belonging to the technical field of energy storage. The invention adopts a strategy of combining activated carbon cloth and electrochemical deposition technology to construct nano rod-shaped vanadium oxide on a carbon cloth substrate. I.e. with VOSO4And (NH)4)2Ac is electrolyte, and is treatedThe surface of the carbon cloth is electrodeposited with a layer of vanadium oxide, the structure increases the specific surface area of the material, is beneficial to the contact of an electrode and electrolyte, and maximizes the utilization rate of the material.
2. The vanadium oxide prepared by the method is uniformly distributed and grows on the carbon cloth fiber in a nano rod shape, the structure among the active substances is favorable for the rapid diffusion of electrolyte, the specific surface area of the material is increased, the strain in the energy storage process is buffered, and the vanadium oxide has larger specific surface area and more exposed active sites, thereby showing better electrochemical performance.
3. Vanadium oxides, due to their variable oxidation states, are capable of undergoing redox reactions, and can utilize redox reactions between these oxidation states for energy storage, exhibiting high specific capacitance. According to the invention, the specific capacity of the carbon cloth is firstly improved by a surface activation method, the number of oxygen-containing functional groups on the surface of the carbon cloth is increased, and then a layer of vanadium oxide is plated on the surface of the carbon cloth by an electrodeposition method, so that the pseudo capacitance of the electrode material is improved. The method has the advantages of simple operation and short preparation time, and vanadium oxide sediments with a nanorod structure and uniform distribution are obtained on the treated carbon cloth, so that the area specific capacitance is higher.
Drawings
FIG. 1 is a scanning electron microscope image of the modified carbon cloth obtained in step (2) of example 1, wherein a is a low-magnification scanning electron microscope image, and b is a high-magnification scanning electron microscope image.
Fig. 2 is a picture related to the direct deposition of vanadium oxide on an empty carbon cloth in step (2) of example 2, wherein a is a low-magnification scanning electron microscope picture, b is a high-magnification scanning electron microscope picture, c is a cyclic voltammetry curve of the deposited vanadium oxide, and d is a constant current charge-discharge curve.
Fig. 3 is a picture related to the deposition of vanadium oxide on the modified carbon cloth in step (3) of example 3, wherein a is a low-magnification scanning electron microscope picture, b is a high-magnification scanning electron microscope picture, c is a cyclic voltammogram of the deposited vanadium oxide, and d is a constant current charge-discharge curve.
FIG. 4 is a picture of deposition of vanadium oxide on a modified carbon cloth in step (3) of example 4, wherein a is a low-magnification scanning electron microscope picture, b is a high-magnification scanning electron microscope picture, c is a cyclic voltammogram of the deposited vanadium oxide, and d is a constant current charge-discharge curve of the deposited vanadium oxide
Fig. 5 is an XRD spectrum of vanadium oxide deposited on the modified carbon cloth in step (3) of example 4.
Fig. 6a is a picture of vanadium oxide deposited on the modified carbon cloth in step (3) of example 4, wherein a is a scanning electron microscope picture of low magnification of vanadium oxide deposited on the carbon cloth, b is a scanning electron microscope picture of high magnification of vanadium oxide deposited on the carbon cloth, c is a cyclic voltammetry curve of vanadium oxide deposited, and d is a constant current charging and discharging curve of vanadium oxide deposited.
Detailed Description
Example 1
(1) Cutting the carbon cloth into a size of 1cm multiplied by 2.5cm, washing with absolute ethyl alcohol, then carrying out ultrasonic treatment for 5min by using deionized water, and drying the cleaned carbon cloth in a vacuum drying oven at 60 ℃.
(2) In a three-electrode system, carbon cloth is used as a working electrode, carbon paper is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, and the working electrode is heated to 1M KNO3The electrode is activated in the solution by a potentiostatic method, the potential is 1.8V, and the reaction time is 3 h. And (3) after activation, washing with deionized water to remove redundant electrolyte, then placing the electrolyte in a three-electrode system, and recovering the electrode conductivity in a 3M KCl solution under a potential window of-1.2-1V by adopting a cyclic voltammetry method, wherein the number of scanning turns is 100. And soaking the treated sample in deionized water to remove excessive electrolyte, and drying in a vacuum drying oven at 60 ℃ for 8 h.
FIG. 1 is a scanning electron microscope image of the product obtained in step (2) of example 1, in lower magnification FIG. 1(a) and in higher magnification FIG. 1 (b). As can be seen from FIG. 1, the surface of the functionalized carbon cloth has a spider-web structure, which has better performance than that of the unfunctionalized carbon cloth, but still has poorer energy storage capability.
Example 2
1) Cutting the carbon cloth into a size of 1cm multiplied by 2.5cm, washing with absolute ethyl alcohol, then carrying out ultrasonic treatment for 5min by using deionized water, and drying the cleaned carbon cloth in a vacuum drying oven at 60 ℃.
2) In a three-electrode system, carbon cloth is used as a working electrode, carbon paper is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, and in VOSO4：(NH4)2And performing electrodeposition in a mixed solution with Ac of 1:2 by adopting cyclic voltammetry. The potential window is-1.5V, and the scanning is performed for 100 circles. The obtained sample is soaked in deionized water to remove the redundant electrolyte, and then dried in a vacuum drying oven for 8 hours at 60 ℃.
FIG. 2 is a low magnification graph 2(a) and a high magnification graph 2(b) of the product obtained in step (2) of example 2, respectively showing a cyclic voltammetry curve (c) and a constant current charge-discharge curve (d) of the deposited vanadium oxide by scanning electron microscopy. From FIG. 2(d), the current at 5mA cm was calculated-2Has an area specific capacitance of 1404mF cm-2。
Example 3
1) Cutting the carbon cloth into a size of 1cm multiplied by 2.5cm, washing with absolute ethyl alcohol, then carrying out ultrasonic treatment for 5min by using deionized water, and drying the cleaned carbon cloth in a vacuum drying oven at 60 ℃.
(2) In a three-electrode system, carbon cloth is used as a working electrode, carbon paper is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, and the working electrode is heated to 1M KNO3The electrode is activated in the solution by a potentiostatic method, the potential is 1.8V, and the reaction time is 3 h. And (3) after activation, washing with deionized water to remove redundant electrolyte, then placing the electrolyte in a three-electrode system, and recovering the electrode conductivity in a 3M KCl solution under a potential window of-1.2-1V by adopting a cyclic voltammetry method, wherein the number of scanning turns is 100. And soaking the treated sample in deionized water to remove excessive electrolyte, and drying in a vacuum drying oven at 60 ℃ for 8 h.
3) In VOSO4：(NH4)2And performing electrodeposition in a mixed solution with Ac of 1:2 by adopting cyclic voltammetry. The potential window is-1.5V, and the scanning is performed for 100 circles. The obtained sample is soaked in deionized water to remove the redundant electrolyte, and then dried in a vacuum drying oven for 8 hours at 60 ℃.
FIG. 3 is a graph showing the low magnification (a) and high magnification (b) of the product obtained in step (3) of example 3, respectively, in a scanning electron microscope, and the cycle of depositing vanadium oxideA ring volt-ampere curve (c) and a constant current charge-discharge curve (d). The scanning electron micrograph of FIG. 3 shows that the deposition is relatively uniform, and the current at 5mA cm can be calculated from FIG. 3(d)-2Has an area specific capacitance of 3302mF cm-2。
Example 4
1) Cutting the carbon cloth into a size of 1cm multiplied by 2.5cm, washing with absolute ethyl alcohol, then carrying out ultrasonic treatment for 5min by using deionized water, and drying the cleaned carbon cloth in a vacuum drying oven at 60 ℃.
2) In a three-electrode system, carbon cloth is used as a working electrode, carbon paper is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, and the working electrode is heated to 1M KNO3The electrode is activated in the solution by a potentiostatic method, the potential is 1.8V, and the reaction time is 3 h. And (3) after activation, washing with deionized water to remove redundant electrolyte, then placing the electrolyte in a three-electrode system, and recovering the electrode conductivity in a 3M KCl solution under a potential window of-1.2-1V by adopting a cyclic voltammetry method, wherein the number of scanning turns is 100. And soaking the treated sample in deionized water to remove excessive electrolyte, and drying in a vacuum drying oven at 60 ℃ for 8 h.
3) In VOSO4：(NH4)2And performing electrodeposition in a mixed solution with Ac of 1:2 by adopting cyclic voltammetry. The potential window is-1.5V, and the scanning is performed for 300 circles. The obtained sample is soaked in deionized water to remove the redundant electrolyte, and then dried in a vacuum drying oven for 8 hours at 60 ℃.
FIG. 4 is a graph of the low magnification graph 4(a), the high magnification graph (b) of the scanning electron microscope, the cyclic voltammetry curve (c) of the deposited vanadium oxide, and the constant current charge-discharge curve (d) of the product obtained in step (3) of example 4. It can be seen from the scanning electron microscope picture that the vanadium oxide deposited on the surface of the carbon cloth is very uniform and shows a nanorod structure, and the current can be calculated from fig. 4(d) at 5mA cm-2Has an area specific capacitance of 3375mF cm-2. FIG. 5 is the XRD spectrum of the vanadium oxide nano-rod, the characteristic peak and JCPDS card 45-1401V5O12And 31-1438VO2And the consistency indicates that the vanadium oxide nano rod is in mixed valence state distribution.
Example 5
1) Cutting the carbon cloth into a size of 1cm multiplied by 2.5cm, washing with absolute ethyl alcohol, then carrying out ultrasonic treatment for 5min by using deionized water, and drying the cleaned carbon cloth in a vacuum drying oven at 60 ℃.
2) In a three-electrode system, carbon cloth is used as a working electrode, carbon paper is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, and the working electrode is heated to 1M KNO3The electrode is activated in the solution by a potentiostatic method, the potential is 1.8V, and the reaction time is 3 h. And (3) after activation, washing with deionized water to remove redundant electrolyte, then placing the electrolyte in a three-electrode system, and recovering the electrode conductivity in a 3M KCl solution under a potential window of-1.2-1V by adopting a cyclic voltammetry method, wherein the number of scanning turns is 500. And soaking the treated sample in deionized water to remove excessive electrolyte, and drying in a vacuum drying oven at 60 ℃ for 8 h.
3) In VOSO4：(NH4)2And performing electrodeposition in a mixed solution with Ac of 1:2 by adopting cyclic voltammetry. The potential window is-1.5V, and the scanning is performed for 500 circles. The obtained sample is soaked in deionized water to remove the redundant electrolyte, and then dried in a vacuum drying oven for 8 hours at 60 ℃.
FIG. 6 is a graph of the low magnification FIG. 6(a), the high magnification (b) of the scanning electron microscope, the cyclic voltammogram (c) and the constant current charge-discharge curve (d) of the product obtained in step (3) of example 5. The scanning electron microscope picture shows that some vanadium oxide deposited for 500 circles is agglomerated, but the good energy storage effect of the people still exists, and the current of 5mA cm can be calculated from the graph in FIG. 6(d)-2Has an area specific capacitance of 3958mF cm-2。
Claims (9)
1. A vanadium oxide electrode material with a nanorod structure is characterized in that the preparation method comprises the following steps:
1) and (3) placing the carbon cloth under a three-electrode system for activation treatment: at KNO3Activating carbon cloth in electrolyte by adopting a potentiostatic method, cleaning the activated carbon cloth by using deionized water, then placing the carbon cloth in a three-electrode system, and recovering the electrode conductivity in a KCl solution within a certain potential range by adopting a cyclic voltammetry method;
2) active material deposition: preparing vanadium-containing solutionPerforming electrodeposition of vanadium oxide on the carbon cloth obtained in the step 1) by adopting cyclic voltammetry within a potential range of-1.5V in 50mV s-1Performing cyclic voltammetry scanning at the scanning speed of 100-;
3) and soaking the carbon cloth deposited with the vanadium oxide compound in deionized water for 2-5 min to remove redundant electrolyte, and then drying in a vacuum drying oven at 60 ℃ for 8h to obtain the vanadium oxide nano rod-like structure.
2. The preparation method of claim 1, wherein in the step 1), before the modification of the carbon cloth, the carbon cloth is washed by ethanol and deionized water, then is placed into the deionized water for ultrasonic cleaning, and then is dried in a vacuum drying oven at 60 ℃.
3. The method according to claim 1, wherein in step 1), the potentiostatic conditions are: the potential is 1.8V, and the reaction time is 2.5-3 h.
4. The preparation method according to claim 1, wherein in step 1), the conditions for recovering the electrode conductivity by cyclic voltammetry are as follows: the potential is-1.2 to 1V, and the sweeping speed is 50 to 100mV s-1The number of scanning turns: 50-100 circles.
5. The preparation method according to claim 1, wherein in step 1), the modified carbon cloth needs to be washed with deionized water.
6. The preparation method according to claim 1, wherein in step 1), carbon cloth is used as a working electrode, carbon paper is used as a counter electrode, and a saturated calomel electrode is used as a reference electrode under a three-electrode system.
7. The method according to claim 1, wherein in step 2), the solution containing vanadium is VOSO4：(NH4)2Ac is 1: 2.
8. The method according to claim 1, wherein in step 2), the number of cyclic voltammetry scans is: 100. 300 and 500 circles.
9. Use of the vanadium oxide electrode material having a nanorod structure of any one of claims 1 to 8 in a supercapacitor.
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