CN112635201A - Flexible all-solid-state asymmetric supercapacitor electrode and preparation method thereof by dividing flexible all-solid-state asymmetric supercapacitor electrode into two parts - Google Patents
Flexible all-solid-state asymmetric supercapacitor electrode and preparation method thereof by dividing flexible all-solid-state asymmetric supercapacitor electrode into two parts Download PDFInfo
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Abstract
The invention belongs to the technical field of flexible energy storage devices, and particularly relates to a flexible all-solid-state asymmetric supercapacitor electrode and a preparation method thereof. The preparation method starts from a nickel hydroxide @ polydopamine composite material, and the nickel oxide array electrode is obtained by calcining in the air and is used as the positive electrode of the super capacitor; calcining in argon gas, and performing acid treatment to obtain the graphene nano-sieve array electrode which is used as a super capacitor cathode. The flexible all-solid-state asymmetric supercapacitor obtained after assembly has good electrochemical performance. The preparation method has wide application prospect in the development of asymmetric supercapacitor electrodes.
Description
Technical Field
The invention belongs to the technical field of flexible energy storage devices, and particularly relates to a flexible all-solid-state asymmetric supercapacitor electrode and a preparation method thereof.
Background
In recent years, the rise of flexible wearable electronics has pushed the rapid development of flexible energy storage technologies. Therefore, designing high performance, low cost flexible energy storage devices is a current research focus. Among various energy storage devices, the flexible all-solid-state supercapacitor brings hopes to people by the advantages of quick charge and discharge, long service life, environmental protection and the like, and draws wide attention. However, the low energy density of supercapacitors limits their large-scale application.
According to the formula (E = CV)2/2), the energy density needs to be increased by increasing the capacitance and operating voltage of the whole device. Asymmetric/hybrid supercapacitors designed using high capacitance double layer capacitor (EDLC) materials (e.g., porous carbon, carbon nanotubes, graphene, etc.) and pseudocapacitor/battery type materials (e.g., cobalt oxide, nickel oxide, iron oxide, etc.) are expected to improve energy storage performance. So far, many reports have been made on the research on different electrode materials in asymmetric supercapacitors. Research work in recent years shows that the nano morphology and structure control of the electrode active material are a very effective strategy for realizing the maximization of electrochemical performance, and the development of three-dimensional porous structures, nano sheet/nano rod array structures and multilayer hierarchical structures can generate the surface area and active sites of the electrode which are decisively promoted. However, the overall performance of an asymmetric supercapacitor is not limited to a single electrode, requiring co-contribution and synergy between the two electrodes. Therefore, the development of high-performance anode and cathode materials by a simple synthesis method is a challenging problem for preparing the high-performance asymmetric supercapacitor. The development of two or more materials from a single precursor through different conditions is an important advance in the field of material synthesis. This strategy makes it easy to adjust the composition of the final product while inheriting some morphological and structural features of the precursor. The concept of 'dividing into two' provides a simple and feasible new approach for material synthesis and preparation. Thus, two different methods of making flexible supercapacitors using this methodSelf-supporting electrodes have many interesting advantages, such as flexibility and nanostructure similarity, simple manufacturing process and low cost. Therefore, the electrode materials with different capacitance characteristics are prepared from a single precursor and assembled into an integrated device, and the method has a great application prospect.
Disclosure of Invention
In view of the above defects or improvement needs of the prior art, the present invention aims to provide a flexible all-solid-state asymmetric flexible supercapacitor electrode and a method for preparing the same in a two-in-one manner.
The invention realizes that the anode electrode material and the cathode electrode material required by assembling the flexible super capacitor are simultaneously prepared from one precursor composite material by improving the whole process flow and the reaction conditions and parameters (such as the types and the proportions of reaction raw materials, the concentration of reactants, the reaction atmosphere, the reaction temperature and the like) of each key process step. The preparation method has the advantages of simple process, convenient operation and cheap and easily obtained reaction materials.
The invention provides a 'one-into-two' preparation method of a flexible all-solid-state asymmetric supercapacitor electrode, which comprises the following specific steps of:
(1) growing a nickel hydroxide nanosheet array on the surface of a carbon cloth serving as a substrate, and then coating polydopamine to form a carbon cloth @ nickel hydroxide @ polydopamine composite material;
(2) calcining the carbon cloth @ nickel hydroxide @ polydopamine composite material in air to form a carbon cloth @ nickel oxide nanosheet array which is used as a super capacitor anode;
(3) calcining the carbon cloth @ nickel hydroxide @ polydopamine composite material in argon, and then performing acid treatment to form a carbon cloth @ graphene nano-sieve array which is used as a cathode of a super capacitor;
(4) and assembling the flexible solid-state supercapacitor based on the two electrodes.
Preferably, the solution for growing the nickel hydroxide nanosheet array in step (1) is a mixed solution of 0.1 to 0.15mol/L of nickel chloride hexahydrate and 0.2 to 0.3mol/L of hexamethylenetetramine.
Preferably, the growth temperature of the nickel hydroxide in the step (1) is 90-100 ℃, and the time is 10-12 h.
Preferably, the coating of the polydopamine in the step (1) is carried out in a dopamine hydrochloride-Tris mixed solution, the concentration of Tris is 1.21-1.81 g/L, and the reaction time is 24-48 h.
Preferably, in the calcination process in step (2), air in the tube furnace is exhausted, the flow of argon is controlled to be 100-: firstly, heating to 400 ℃ at the temperature rising speed of 2-5 ℃/min, and preserving heat for 2-4h at the temperature; then, the sample is taken out and placed in a muffle furnace, and is heated to 350-400 ℃ under the air condition and is kept for 1-3 h.
Preferably, in the calcination process in step (3), air in the tube furnace is exhausted, the flow of argon is controlled to be 50-200 sccm, and the calcination conditions are as follows: firstly, keeping the temperature at 400 ℃ for 2-4h at 300-; then raising the temperature to 700-800 ℃ at the temperature raising rate of 2-5 ℃/min, and keeping the temperature for 1-3 h; 1-3mol/L hydrochloric acid or 1-3mol/L sulfuric acid is adopted in the subsequent acid treatment process; and finally, washing with deionized water.
The flexible asymmetric all-solid-state supercapacitor electrode prepared by the method has excellent performance, and is represented by a flexible asymmetric all-solid-state supercapacitor assembled by the electrode, and the flexible asymmetric all-solid-state supercapacitor electrode has good energy storage property, wider working voltage, excellent flexibility and mechanical stability.
The invention also relates to a flexible asymmetric all-solid-state supercapacitor assembled by the electrodes, in particular to a flexible all-solid-state asymmetric supercapacitor assembled by taking the carbon cloth @ nickel oxide nanosheet array electrode as a positive electrode and the carbon cloth @ graphene nano-sieve array electrode as a negative electrode, firstly immersing the electrodes into PVA/KOH solid electrolyte and then sandwiching a diaphragm in the middle.
The invention realizes that the flexible asymmetric super capacitor electrode is directly prepared from the same precursor by the strategy of dividing into two parts, and the invention has the following advantages:
(1) the strategy of 'dividing into two' is simple and easy to implement, and can be suitable for large-scale and expanded production. Meanwhile, the two electrodes can inherit some excellent characteristics of the precursor material, so that the anode and cathode materials have similar structures, such as a nanosheet array structure, and the flexibility and good mechanical property of the whole electrode;
(2) the preparation method comprises the following steps of preparing a nickel oxide electrode with pseudo-capacitance effect and a graphene nano-sieve electrode with double electric layer capacitance property from a nickel hydroxide @ polydopamine precursor by a 'splitting' strategy, and applying the two electrodes to the positive electrode and the negative electrode of a super capacitor respectively to form an asymmetric super capacitor;
(3) the nickel oxide nanosheet array electrode and the graphene nanosieve array electrode prepared by the method have a three-dimensional porous vertically-oriented nanosheet array structure, the structure can provide a large specific surface area and ensure more active sites, and meanwhile, the multi-stage porous structure can provide more ion/substance transmission channels, so that the uniform contact and permeation of electrolyte and the rapid transmission of substances in the electrochemical reaction process are ensured, and the performance of a high-performance energy storage device is ensured.
In conclusion, the preparation method is simple and easy to operate, the preparation strategy of dividing the positive electrode and the negative electrode of the flexible asymmetric supercapacitor into two parts from the same precursor is innovatively provided, the two electrodes are ensured to inherit the excellent appearance and structural characteristics of the precursor, and the performance and application of the flexible asymmetric all-solid-state supercapacitor assembled by the two electrodes are further explored. The invention provides a new technical scheme for designing and preparing the electrode of the high-performance flexible energy storage device.
Drawings
FIG. 1 is a flow chart of a "two-in-one" manufacturing method for providing a flexible asymmetric all-solid-state supercapacitor electrode in the present invention.
FIG. 2 is a scanning electron micrograph of the CC @ NiO electrode prepared in example 1.
FIG. 3 is a scanning electron micrograph of the CC @ NVGMs electrode prepared in example 1.
FIG. 4 is an XRD pattern of the carbon cloth substrate, CC @ NiO electrode and CC @ NVGMs electrode prepared in example 1.
Fig. 5 is a schematic structural diagram of the flexible asymmetric all-solid-state supercapacitor in example 1.
Fig. 6 is a sweep cyclic voltammogram of the flexible asymmetric all-solid-state supercapacitor in example 1.
Fig. 7 is the constant current charge and discharge curve of the flexible asymmetric all-solid-state supercapacitor in example 1.
Fig. 8 is the relationship between the bending angle and the energy storage performance of the flexible asymmetric all-solid-state supercapacitor in example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
(1) Placing carbon in a nickel hydroxide growth solution (a mixed solution of 0.1mol/L nickel chloride hexahydrate and 0.2mol/L hexamethylenetetramine); the growth temperature is 100 ℃ and the time is 10 h. Then coating polydopamine on the surface of the polydopamine, and carrying out the polydopamine coating in a dopamine hydrochloride-Tris mixed solution, wherein the concentration of Tris is 1.21g/L, the concentration of dopamine hydrochloride is 1.5/L, and the reaction time is 24 h; forming a carbon cloth @ nickel hydroxide @ polydopamine composite material;
(2) in the calcining process, the carbon cloth @ nickel hydroxide @ polydopamine composite material is placed in a tubular furnace, air in the tubular furnace is firstly exhausted, the flow of argon is kept at 100sccm, the temperature is firstly increased at 300 ℃ at the speed of 2 ℃/min, and the temperature is kept for 2 hours; the sample was then removed and placed in a muffle furnace and heated to 350 ℃ under air for 1 h. Forming a carbon cloth @ nickel oxide nanosheet array; FIG. 2 is a scanning electron microscope image of the prepared CC @ NiO electrode;
(3) placing the carbon cloth @ nickel hydroxide @ polydopamine composite material in a tubular furnace, ensuring that air in the tubular furnace is exhausted, keeping the argon flow at 50sccm, and keeping the calcination condition at 300 ℃ for 2 hours; then keeping the temperature rise rate of 2 ℃/min to 700 ℃, and keeping the temperature for 1 h; 1mol/L hydrochloric acid is adopted in the subsequent acid treatment process; finally, washing with deionized water to obtain a carbon cloth @ graphene nano-sieve array; FIG. 3 is a scanning electron micrograph of the prepared CC @ NVGMs electrode. FIG. 4 is an XRD pattern of a carbon cloth substrate, a CC @ NiO electrode and a CC @ NVGMs electrode prepared;
(4) the flexible all-solid-state asymmetric supercapacitor is assembled by taking the carbon cloth @ nickel oxide nanosheet array electrode as a positive electrode and the carbon cloth @ graphene nano-sieve array electrode as a negative electrode and firstly soaking the electrodes in PVA/KOH solid electrolyte and then sandwiching a diaphragm, and the structural schematic diagram of the flexible all-solid-state asymmetric supercapacitor is shown in FIG. 5. The scanning cyclic voltammetry curve of the flexible asymmetric all-solid-state supercapacitor is shown in fig. 6, the working voltage of the device can reach 1.6V, and the device shows good capacitance behavior at different scanning speeds; according to the constant current charging and discharging curve in FIG. 7, the specific capacity of the device at a current density of 1A/g is 175F/g, and the device exhibits good energy storage performance; the graph of the relationship between the capacitance retention rate of the device at different bending angles is shown in fig. 8, the capacitance of the device still keeps 98.5% of the initial value when the whole device is bent by 180 degrees, and the device has good mechanical stability and can work normally under a bending state.
Example 2
(1) Placing carbon in a nickel hydroxide growth solution (a mixed solution of 0.15mol/L nickel chloride hexahydrate and 0.3mol/L hexamethylenetetramine); the growth temperature is 100 ℃ and the time is 12 h. Then coating polydopamine on the surface of the polydopamine, and carrying out the polydopamine coating in a dopamine hydrochloride-Tris mixed solution, wherein the concentration of Tris is 1.21g/L, the concentration of dopamine hydrochloride is 3g/L, and the reaction time is 48 h; forming a carbon cloth @ nickel hydroxide @ polydopamine composite material;
(2) in the calcining process, the carbon cloth @ nickel hydroxide @ polydopamine composite material is placed in a tubular furnace, air in the tubular furnace is firstly exhausted, the argon flow is kept at 200sccm, the temperature is firstly increased at 400 ℃ at the speed of 5 ℃/min, and the temperature is kept for 4 hours; the sample was then removed and placed in a muffle furnace and heated to 400 ℃ under air for 3 h. Forming a carbon cloth @ nickel oxide nanosheet array;
(3) placing the carbon cloth @ nickel hydroxide @ polydopamine composite material in a tubular furnace, ensuring that air in the tubular furnace is exhausted, keeping the argon flow at 200sccm, and keeping the calcination condition at 400 ℃ for 4 hours; then keeping the temperature rise rate of 5 ℃/min to 800 ℃, and keeping the temperature for 3 h; 3mol/L hydrochloric acid is adopted in the subsequent acid treatment process; finally, washing with deionized water to obtain a carbon cloth @ graphene nano-sieve array;
(4) the carbon cloth @ nickel oxide nanosheet array electrode is used as a positive electrode, the carbon cloth @ graphene nano-sieve array electrode is used as a negative electrode, the carbon cloth @ nickel oxide nanosheet array electrode is firstly immersed in PVA/KOH solid electrolyte, and then the flexible all-solid-state asymmetric supercapacitor is assembled by the aid of the interlayer diaphragm. Through electrochemical performance tests, the working voltage of the flexible asymmetric all-solid-state supercapacitor can reach 1.6V, the specific capacity is 172F/g when the current density is 1A/g, the capacity of the whole device still keeps 99.5% of the initial value when the whole device is bent by 180 degrees, and good energy storage performance and mechanical stability are shown.
Example 3
(1) Placing carbon in a nickel hydroxide growth solution (a mixed solution of 0.1mol/L nickel chloride hexahydrate and 0.2mol/L hexamethylenetetramine); the growth temperature is 100 ℃ and the growth time is 11 h. Then coating polydopamine on the surface of the polydopamine, and carrying out the polydopamine coating in a dopamine hydrochloride-Tris mixed solution, wherein the concentration of Tris is 1.21g/L, the concentration of dopamine hydrochloride is 2g/L, and the reaction time is 36 h; forming a carbon cloth @ nickel hydroxide @ polydopamine composite material;
(2) in the calcining process, the carbon cloth @ nickel hydroxide @ polydopamine composite material is placed in a tubular furnace, air in the tubular furnace is firstly ensured to be exhausted, the argon flow is kept at 150sccm, the temperature is firstly increased at 350 ℃ at the speed of 5 ℃/min, and the temperature is kept for 3 hours; the sample was then removed and placed in a muffle furnace and heated to 400 ℃ under air for 2 h. Forming a carbon cloth @ nickel oxide nanosheet array;
(3) placing the carbon cloth @ nickel hydroxide @ polydopamine composite material in a tubular furnace, ensuring that air in the tubular furnace is exhausted, keeping the argon flow at 100sccm, and keeping the calcination condition at 400 ℃ for 3 hours; then keeping the temperature rise rate of 5 ℃/min to 800 ℃, and keeping the temperature for 2 h; 1mol/L sulfuric acid is adopted in the subsequent acid treatment process; finally, washing with deionized water to obtain a carbon cloth @ graphene nano-sieve array;
(4) the carbon cloth @ nickel oxide nanosheet array electrode is used as a positive electrode, the carbon cloth @ graphene nano-sieve array electrode is used as a negative electrode, the carbon cloth @ nickel oxide nanosheet array electrode is firstly immersed in PVA/KOH solid electrolyte, and then the flexible all-solid-state asymmetric supercapacitor is assembled by the aid of the interlayer diaphragm. Through electrochemical performance tests, the working voltage of the flexible asymmetric all-solid-state supercapacitor can reach 1.6V, the specific capacity is 178F/g when the current density is 1A/g, the capacity of the whole device still keeps 97.7% of the initial value when the whole device is bent by 180 degrees, and good energy storage performance and mechanical stability are shown.
Example 4
(1) Placing carbon in a nickel hydroxide growth solution (a mixed solution of 0.15mol/L nickel chloride hexahydrate and 0.3mol/L hexamethylenetetramine); the growth temperature is 90 ℃ and the time is 12 h. Then coating polydopamine on the surface of the polydopamine, and carrying out the polydopamine coating in a dopamine hydrochloride-Tris mixed solution, wherein the concentration of Tris is 1.81g/L, the concentration of dopamine hydrochloride is 2g/L, and the reaction time is 24 hours; forming a carbon cloth @ nickel hydroxide @ polydopamine composite material;
(2) in the calcining process, the carbon cloth @ nickel hydroxide @ polydopamine composite material is placed in a tubular furnace, air in the tubular furnace is firstly exhausted, the argon flow is kept at 200sccm, the temperature is firstly increased at 400 ℃ at the temperature rise speed of 5 ℃/min, and the temperature is kept for 2 hours; the sample was then removed and placed in a muffle furnace and heated to 350 ℃ under air for 1 h. Forming a carbon cloth @ nickel oxide nanosheet array;
(3) placing the carbon cloth @ nickel hydroxide @ polydopamine composite material in a tubular furnace, ensuring that air in the tubular furnace is exhausted, keeping the argon flow at 200sccm, and keeping the calcination condition at 400 ℃ for 2 hours; then keeping the temperature rise rate of 5 ℃/min to 750 ℃ and keeping the temperature for 2 h; 3mol/L sulfuric acid is adopted in the subsequent acid treatment process; finally, washing with deionized water to obtain a carbon cloth @ graphene nano-sieve array;
(4) the carbon cloth @ nickel oxide nanosheet array electrode is used as a positive electrode, the carbon cloth @ graphene nano-sieve array electrode is used as a negative electrode, the carbon cloth @ nickel oxide nanosheet array electrode is firstly immersed in PVA/KOH solid electrolyte, and then the flexible all-solid-state asymmetric supercapacitor is assembled by the aid of the interlayer diaphragm. Through electrochemical performance tests, the working voltage of the flexible asymmetric all-solid-state supercapacitor can reach 1.6V, the specific capacity is 170F/g when the current density is 1A/g, the capacity of the whole device still keeps 96.8% of the initial value when the whole device is bent by 180 degrees, and good energy storage performance and mechanical stability are shown.
Claims (7)
1. A method for preparing a flexible all-solid-state asymmetric supercapacitor electrode in two parts is characterized by comprising the following specific steps:
(1) growing a nickel hydroxide nanosheet array on the surface of a carbon cloth serving as a substrate, and then coating polydopamine to form a carbon cloth @ nickel hydroxide @ polydopamine composite material;
(2) calcining the carbon cloth @ nickel hydroxide @ polydopamine composite material in argon to form a carbon cloth @ nickel oxide nanosheet array which is used as a super capacitor anode;
(3) the carbon cloth @ nickel hydroxide @ polydopamine composite material is calcined in argon, and then the carbon cloth @ graphene nano-sieve array is formed through acid treatment and used as a super capacitor negative electrode.
2. The production method according to claim 1, wherein the solution for growing the nickel hydroxide nanosheet array in step (1) is a mixed solution of 0.1 to 0.15mol/L of nickel chloride hexahydrate and 0.2 to 0.3mol/L of hexamethylenetetramine; the growth temperature of the nickel hydroxide is 90-100 ℃, and the growth time is 10-12 h.
3. The preparation method according to claim 2, wherein the coating of the polydopamine in the step (1) is performed in a dopamine hydrochloride-Tris mixed solution, the concentration of Tris is 1.21-1.81 g/L, the concentration of dopamine hydrochloride is 1.5-3g/L, and the reaction time is 24-48 h.
4. The method according to claim 3, wherein in the step (2), during the calcination process, air in the tube furnace is exhausted, the flow rate of argon gas is controlled to be 100-: firstly, heating to 400 ℃ at the temperature rising speed of 2-5 ℃/min, and preserving heat for 2-4h at the temperature; then, the sample is taken out and placed in a muffle furnace, and is heated to 350-400 ℃ under the air condition and is kept for 1-3 h.
5. The production method according to claim 4, wherein in the calcination in the step (3), air in the tube furnace is exhausted, an argon flow is controlled to be 50 to 200sccm, and calcination conditions are as follows: firstly, preserving heat for 2-4h at the temperature of 400 ℃ of 300-; then heating to 700-800 ℃ at the heating rate of 2-5 ℃/min, and keeping the temperature for 1-3 h; 1-3mol/L hydrochloric acid or 1-3mol/L sulfuric acid is adopted for the acid treatment; and finally, washing with deionized water.
6. A flexible all-solid-state asymmetric supercapacitor electrode obtained by the preparation method of any one of claims 1 to 5, wherein the positive electrode material and the negative electrode material are prepared from a precursor composite material at the same time.
7. A flexible all-solid-state asymmetric supercapacitor assembled by the electrodes of claim 6, wherein a carbon cloth @ nickel oxide nanosheet array electrode is used as a positive electrode, a carbon cloth @ graphene nano-sieve array electrode is used as a negative electrode, PVA/KOH is used as a solid electrolyte, and an interlayer diaphragm is arranged in the middle of the carbon cloth @ nickel oxide nanosheet array electrode.
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