CN-122000211-A - Flexible supercapacitor electrode material and preparation method thereof based on cyclic electrochemical deposition

CN122000211ACN 122000211 ACN122000211 ACN 122000211ACN-122000211-A

Abstract

The invention relates to the technical field of electrode materials, in particular to a flexible supercapacitor electrode material and a preparation method thereof based on cyclic electrochemical deposition, comprising the following steps of preprocessing flexible carbon cloth to obtain modified carbon cloth; preparing aniline electroplating solution and graphene oxide electroplating solution, and alternately electrodepositing a PANI layer and a rGO layer on the modified carbon cloth to obtain the electrode material with the PANI/rGO R layer. According to the flexible supercapacitor electrode material and the preparation method based on cyclic electrochemical deposition, which are disclosed by the invention, through controlling the electrodeposition time, the potential and the cycle times, the thickness and the proportion of the PANI layer and the rGO layer can be accurately regulated, so that the PANI layer and the rGO layer are alternately deposited to form a compact and firmly-combined layered structure, and the problem of peeling of PANI caused by volume change in the charge and discharge process is effectively relieved.

Inventors

GU YAN
LAI CHAOJIN
SONG HAIPING
CHEN XIAO
LIU SHANSHAN
GUO CHENGRUI
CHEN YIMIN
WANG GANGQIANG
SHAN XINGGANG
CHEN SHUJUN
XU KUNHONG

Assignees

浙江理工大学科技与艺术学院

Dates

Publication Date: 20260508
Application Date: 20260310

Claims (10)

1. The preparation method of the flexible supercapacitor electrode material based on the cyclic electrochemical deposition is characterized by comprising the following steps of: s1, immersing the flexible carbon cloth into a mixed acid solution, standing, taking out, repeatedly washing with deionized water to be neutral, and drying to obtain modified carbon cloth; S2, adding aniline into a sulfuric acid solution, performing ultrasonic treatment to obtain an aniline electroplating solution for standby, adding graphene oxide into deionized water, and performing ultrasonic treatment to obtain a graphene oxide electroplating solution for standby; S3, taking the modified carbon cloth obtained in the step S1 as a working electrode, setting a counter electrode and a reference electrode, and assembling to obtain a three-electrode system; S4, placing the working electrode in the three-electrode system in the S3 into the aniline electroplating solution obtained in the S2, performing electrodeposition, drying to obtain a PANI layer, then placing the working electrode into the graphene oxide electroplating solution obtained in the S2, depositing a rGO layer on the surface of the PANI layer in situ, and drying to obtain the PANI/rGO layer; S5, repeating the step S4 to obtain the electrode material with the PANI/rGO R layer, wherein R is the cycle number of the step S4.
2. The method for preparing the electrode material of the flexible supercapacitor based on the cyclic electrochemical deposition according to claim 1, wherein in S1, the mixed acid solution is concentrated nitric acid and concentrated sulfuric acid with a volume ratio of 1:1, the standing temperature is 20-30 ℃, the standing time is 20-40min, and the drying temperature is 50-70 ℃.
3. The preparation method of the flexible supercapacitor electrode material based on the cyclic electrochemical deposition according to claim 1, wherein in S2, the ultrasonic time is 20-40min, and the ultrasonic temperature is 50-70 ℃.
4. The preparation method of the flexible supercapacitor electrode material based on the cyclic electrochemical deposition according to claim 1, wherein in S2, the concentration of the aniline electroplating solution is 0.1-1mol/L, and the concentration of the graphene oxide electroplating solution is 0.5-2mg/mL.
5. The method for preparing the electrode material of the flexible supercapacitor based on the cyclic electrochemical deposition of claim 1, wherein in S3, the counter electrode is a platinum wire, and the reference electrode is a saturated calomel electrode.
6. The method for preparing the electrode material of the flexible supercapacitor based on cyclic electrochemical deposition according to claim 1, wherein in the step S4, the electrodeposition time is 10-60S, and the electrodeposition potential is-1.5V to 1.5V.
7. The method for preparing the electrode material of the flexible supercapacitor based on cyclic electrochemical deposition according to claim 1, wherein in S4, the drying temperature is 80-100 ℃ and the drying time is 2-10min.
8. The method for preparing the electrode material of the flexible supercapacitor based on cyclic electrochemical deposition according to claim 1, wherein in S4, the electrodeposition time and the electrodeposition potential of the PANI layer and the rGO layer are the same.
9. The method for preparing the electrode material of the flexible supercapacitor based on cyclic electrochemical deposition according to claim 1, wherein in S5, R is 5-45.
10. The flexible supercapacitor electrode material is characterized in that the flexible supercapacitor electrode material based on cyclic electrochemical deposition is prepared by the preparation method of the flexible supercapacitor electrode material based on cyclic electrochemical deposition according to any one of claims 1-9, and the PANI/rGO R layers are alternately laminated to form a compact and uniform composite conductive structure.

Description

Flexible supercapacitor electrode material and preparation method thereof based on cyclic electrochemical deposition Technical Field The invention relates to the technical field of electrode materials, in particular to a flexible supercapacitor electrode material and a preparation method thereof based on cyclic electrochemical deposition. Background With the continuous decrease of fossil energy reserves and the continuous enhancement of environmental protection consciousness, the development of green and efficient energy storage technologies has become an important direction in the energy field. Super capacitors are considered as an important component of a new generation of sustainable energy systems because of the advantages of high power density, rapid charge and discharge speed, long cycle life, environmental friendliness and the like. The electrode material is a key factor determining the performance of the supercapacitor, and the structural stability and the conductivity of the electrode material directly influence the energy density and the cycle life of the device. Polyaniline (PANI) is a typical conductive polymer material, has higher theoretical specific capacitance and good reversible oxidation-reduction characteristics, but is easy to generate volume expansion and structural pulverization in the repeated charge and discharge process, so that a conductive network is damaged, and the cycle performance is degraded. Graphene Oxide (GO) and its reduced form (rGO) have excellent conductivity, large specific surface area and flexibility, and can be used as a carrier material to improve the conductivity and structural stability of PANI. However, the traditional PANI/rGO composite electrode is mostly prepared by adopting a chemical oxidation polymerization method, the film structure is uneven, the interface binding force is poor, the rGO preparation process is complex, the cost is high, and the popularization and the application of the electrode in flexible energy storage devices are limited. Therefore, how to construct a PANI/rGO composite electrode with high conductivity, excellent adhesion and long-term cycling stability on a flexible carbon cloth substrate becomes a technical problem to be solved in the current flexible supercapacitor field. Disclosure of Invention The invention aims to provide a flexible supercapacitor electrode material and a preparation method based on cyclic electrochemical deposition, wherein the thickness and the proportion of a PANI layer and a rGO layer can be accurately regulated by controlling the electrodeposition time, the potential and the cycle times, so that the PANI layer and the rGO layer are alternately deposited to form a compact and firmly combined layered structure, the problem of peeling of PANI caused by volume change in the charging and discharging process is effectively relieved, the overall performance of the electrode is obviously improved, and the preparation cost is reduced. In order to achieve the above purpose, the invention provides a preparation method of a flexible supercapacitor electrode material based on cyclic electrochemical deposition, which comprises the following steps: s1, immersing the flexible carbon cloth into a mixed acid solution, standing, taking out, repeatedly washing with deionized water to be neutral, and drying to obtain modified carbon cloth; S2, adding aniline into a sulfuric acid solution, performing ultrasonic treatment to obtain an aniline electroplating solution for standby, adding graphene oxide into deionized water, and performing ultrasonic treatment to obtain a graphene oxide electroplating solution for standby; S3, taking the modified carbon cloth obtained in the step S1 as a working electrode, setting a counter electrode and a reference electrode, and assembling to obtain a three-electrode system; S4, placing the working electrode in the three-electrode system in the S3 into the aniline electroplating solution obtained in the S2, performing electrodeposition, drying to obtain a PANI layer, then placing the working electrode into the graphene oxide electroplating solution obtained in the S2, depositing a rGO layer on the surface of the PANI layer in situ, and drying to obtain the PANI/rGO layer; S5, repeating the step S4 to obtain the electrode material with the PANI/rGO R layer, wherein R is the cycle number of the step S4. Preferably, in S1, the mixed acid solution is concentrated nitric acid and concentrated sulfuric acid with a volume ratio of 1:1, the standing temperature is 20-30 ℃, the standing time is 20-40min, and the drying temperature is 50-70 ℃. Preferably, in S2, the ultrasonic time is 20-40min and the ultrasonic temperature is 50-70 ℃. Preferably, in S2, the concentration of the aniline electroplating solution is 0.1-1mol/L, and the concentration of the graphene oxide electroplating solution is 0.5-2mg/mL. Preferably, in S3, the counter electrode is a platinum wire, and the reference electrode is a saturat