CN111415823B - Ni-Sn-S composite material and preparation method and application thereof - Google Patents
Ni-Sn-S composite material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 229910020212 Na2SnO3 Inorganic materials 0.000 claims abstract description 16
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 79
- 239000000243 solution Substances 0.000 claims description 35
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 34
- 239000006260 foam Substances 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 29
- 229910052759 nickel Inorganic materials 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 20
- -1 polytetrafluoroethylene Polymers 0.000 claims description 16
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 16
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 16
- 239000006229 carbon black Substances 0.000 claims description 13
- 238000001291 vacuum drying Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
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- 239000002904 solvent Substances 0.000 claims description 4
- 239000003990 capacitor Substances 0.000 abstract description 9
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 18
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- 238000010277 constant-current charging Methods 0.000 description 9
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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
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
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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
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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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- 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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Abstract
The invention relates to a Ni-Sn-S composite material and a preparation method and application thereof, wherein the preparation method of the composite material comprises the following steps: 1) mixing Na2SnO3Solution and Ni (CH)3COO)2Uniformly mixing the solution, adding thioacetamide and carrying out hydrothermal reaction; 2) after the hydrothermal reaction is finished, carrying out post-treatment to obtain the Ni-Sn-S composite material; the composite material is prepared into a working electrode for being used in a super capacitor. Compared with the prior art, the Ni-Sn-S composite material is synthesized by a one-step hydrothermal method, the composite material has good electrochemical performance, and the preparation method is simple, environment-friendly and convenient for large-scale production.
Description
Technical Field
The invention belongs to the technical field of electrochemistry and nano materials, and relates to a Ni-Sn-S composite material, a preparation method thereof and application thereof in a super capacitor.
Background
Due to the wide application of high performance energy storage devices in portable electronic products and electric vehicles, their demand is rapidly increasing. In particular, supercapacitors, which have energy and power densities intermediate between conventional capacitors and batteries, have received attention for their unique advantages. The super capacitor has the advantages of high charging speed, long cycle life, good stability, good safety and the like. Supercapacitors are divided into two categories, Electric Double Layer Capacitors (EDLCs) and pseudo-capacitors (PCs), according to their mechanism of operation. Most commercial carbon-based supercapacitors belong to the EDLCs, which show good performance and cost-effectiveness. However, PCs are likely to be superior to EDLCs due to their inherently fast and reversible faradaic redox reactions, with higher energy densities. Therefore, electrode materials for PCs are receiving attention.
Transition metal oxides and metal hydroxides having multiple oxidation states produce higher specific capacitance (Cs) than conductive polymers and carbonaceous materials. However, low conductivity, poor cycling stability and slow ion diffusion worsen the faradaic reaction at its surface, leading to a reduction in power density. In addition, sulfur-containing materials have higher electrical conductivity and more efficient electrochemical activity than oxides. Because of the low electronegativity of sulfur, the substitution of sulfur for oxygen can create an additional flexible structure that provides an easy electron transport pathway in the structure. Among various metal sulfide materials, Sn-based materials are very attractive due to their high theoretical capacity, however, the capacity of tin metal decays faster due to its large volume change during the process of lithium alloying and dealloying, which limits its application.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a Ni-Sn-S composite material, a preparation method thereof and application thereof in a super capacitor. The composite material has good electrochemical performance, and the preparation method is simple, environment-friendly and convenient for large-scale production.
The purpose of the invention can be realized by the following technical scheme:
a method of making a Ni-Sn-S composite, the method comprising the steps of:
1) mixing Na2SnO3Solution and Ni (CH)3COO)2Uniformly mixing the solution, adding thioacetamide and carrying out hydrothermal reaction;
2) and after the hydrothermal reaction is finished, carrying out post-treatment to obtain the Ni-Sn-S composite material.
Further, in step 1), the Na is2SnO3Solution and Ni (CH)3COO)2In the solution, the solvent is a mixed solution of water and glycol; in the solvent, the volume ratio of water to glycol is 3 (1-9).
Further, in step 1), the Na is2SnO3In solution, Na2SnO3Has a molar concentration of 1-2mmol/40mL, and the Ni (CH)3COO)2In solution, Ni (CH)3COO)2The molar concentration of (b) is 1-2mmol/40 mL.
Further, in the step 1), the mixing process is that Na is firstly mixed under the condition of vigorous stirring2SnO3Solution and Ni (CH)3COO)2The solution was mixed and then stirred magnetically.
Further, in step 1), Na2SnO3、Ni(CH3COO)2The addition amount ratio of the thioacetamide to the thioacetamide is 2mmol (1-4) mmol (0.1-0.5) g.
Further, in the step 1), the temperature in the hydrothermal reaction is 120-200 ℃, and the time is 12-24 h.
Further, in the step 2), the post-treatment comprises cooling, centrifuging, washing and drying, wherein the drying is vacuum drying, and the temperature is 55-65 ℃ in the vacuum drying process for 10-14 h.
The Ni-Sn-S composite material is prepared by the method.
The application of the Ni-Sn-S composite material is to prepare the composite material into a working electrode for a super capacitor.
Further, the preparation process of the working electrode comprises the following steps: grinding the composite material, uniformly mixing the ground composite material with carbon black and polytetrafluoroethylene, then pressing the mixture on a foam nickel sheet, and drying to obtain the working electrode; the mass ratio of the composite material, the carbon black and the polytetrafluoroethylene is 8 (0.8-1.2) to (0.8-1.2).
The electrochemical performance of the Sn-based material is improved by adopting the M-Sn alloy (M is transition metal) to replace pure metal, so that the electrochemical performance of the composite material is improved. Compared with a single metal sulfide, the Ni-Sn-S composite material of the invention shows more effective pseudocapacitive behavior, which is caused by the fact that two constituent metals enhance the redox reaction.
Compared with the prior art, the invention has the following characteristics:
1) the Ni-Sn-S composite material is synthesized by one-step hydrothermal synthesis, has rich pore channel structures, can provide more electrochemical active sites, and simultaneously provides a rapid ion transportation way to improve the electrochemical performance;
2) the working electrode prepared by the Ni-Sn-S composite material has high specific capacitance (600--1) And power density (800--1) The electrochemical performance is good, and the method can be used in a super capacitor.
Drawings
FIG. 1 is a TEM image of a Ni-Sn-S composite material prepared in example 1;
FIG. 2 is a CV diagram of the Ni-Sn-S composite material prepared in example 1 at different sweep rates;
FIG. 3 is a graph of GCD of the Ni-Sn-S composite material prepared in example 1 at different current densities.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
The raw materials used in the examples are commercially available unless otherwise specified.
Example 1:
a preparation method of a Ni-Sn-S composite material comprises the following steps:
first, 2mmol of Na2SnO3And 2mmol of Ni (CH)3COO)2Respectively dissolving the two solutions in a mixed solution of 30mL of water and 10mL of ethylene glycol, mixing the two solutions under a vigorous stirring condition, adding 0.3g of thioacetamide after magnetic stirring is uniform, transferring the mixed solution into an 80mL polytetrafluoroethylene-lined stainless steel autoclave, carrying out a first-step hydrothermal reaction at 160 ℃ for 16h, taking out a sample after hydrothermal reaction, cooling, centrifuging, washing, and carrying out vacuum drying at 60 ℃ for 12h to obtain the Ni-Sn-S composite material. As can be seen from FIG. 1, the material has rich pore structure, can provide rich electrochemical active sites, and simultaneously provides a rapid ion transport way, thereby improving the electrochemical performance; grinding the composite material, uniformly mixing the ground composite material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and drying the foam nickel sheet in a drying oven at the temperature of 60 ℃ for 12 hours to obtain the Ni-Sn-S working electrode (recorded as NNS-1).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: the method comprises the following steps of taking a foam nickel sheet of NNS-1 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 754.92F/g under the conditions of 2mol/LKOH solution and 1A/g current density, and the energy density is 21.38Wh kg-1The power density is 800W kg-1。
FIG. 2 is a CV diagram of the prepared Ni-Sn-S composite material at different sweep rates, wherein the sweep rates are respectively 5mV/S, 10mV/S, 15mV/S, 20mV/S and 40 mV/S. As can be seen from FIG. 2, in the voltage range of 0 to 0.6V, there are a pair of symmetrical redox peaks, and as the sweep rate increases, the oxidation peak and the reduction peak move to the right and left, respectively. The phenomenon shows that the prepared Ni-Sn-S composite material has good reversibility and stability.
FIG. 3 is a GCD curve of the prepared Ni-Sn-S composite material under different current densities. The specific capacitance is 754.92F/g, 670.54F/g, 554.17F/g, 487.39F/g and 419.33F/g when the current density is 1A/g, 2A/g, 5A/g, 10A/g and 20A/g respectively. As can be seen in fig. 3, the GCD curve contains two voltage plateaus, showing the faradaic behavior of the cell-type electrode.
Example 2:
a preparation method of a Ni-Sn-S composite material comprises the following steps:
first, 2mmol of Na2SnO3And 1mmol of Ni (CH)3COO)2Dissolving the two solutions in a mixed solution of 30mL of water and 10mL of ethylene glycol respectively, mixing the two solutions under a violent stirring condition, adding 0.3g of thioacetamide after magnetic stirring is uniform, transferring the mixed solution into an 80mL polytetrafluoroethylene-lined stainless steel autoclave, carrying out a first-step hydrothermal reaction at 160 ℃ for 16h, taking out a sample after hydrothermal reaction, cooling, centrifuging, washing, and carrying out vacuum drying at 60 ℃ for 12h to obtain a Ni-Sn-S composite material; grinding the composite material, uniformly mixing the ground composite material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and drying the foam nickel sheet in a drying oven at the temperature of 60 ℃ for 12 hours to obtain a Ni-Sn-S working electrode (recorded as NNS-2).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: the method comprises the following steps of taking a foam nickel sheet of NNS-2 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. Under the conditions of 2mol/LKOH solution and 1A/g current density, the specific capacitance of the composite material reaches 645F/g, and the energy density is 18.56Wh kg-1The power density is 800W kg-1。
Example 3:
a preparation method of a Ni-Sn-S composite material comprises the following steps:
first, 1mmol of Na2SnO3And 2mmol of Ni (CH)3COO)2Respectively dissolving in a mixed solution of 30mL of water and 10mL of glycol, mixing the two solutions under the condition of vigorous stirring, uniformly stirring by magnetic force,adding 0.3g of thioacetamide, transferring the mixed solution into a 80mL stainless steel autoclave with a polytetrafluoroethylene lining, carrying out a first-step hydrothermal reaction at 160 ℃ for 16h, taking out a sample after hydrothermal reaction, cooling, centrifuging, washing, and vacuum drying at 60 ℃ for 12h to obtain a Ni-Sn-S composite material; grinding the composite material, uniformly mixing the ground composite material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and drying the foam nickel sheet in a drying oven at the temperature of 60 ℃ for 12 hours to obtain a Ni-Sn-S working electrode (recorded as NNS-3).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: the method comprises the following steps of taking a foam nickel sheet of NNS-3 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. Under the conditions of 2mol/LKOH solution and 1A/g current density, the specific capacitance of the composite material reaches 712F/g, and the energy density is 15.4Wh kg-1The power density is 800W kg-1。
Example 4:
a preparation method of a Ni-Sn-S composite material comprises the following steps:
first, 2mmol of Na2SnO3And 2mmol of Ni (CH)3COO)2Dissolving the two solutions in a mixed solution of 20mL of water and 20mL of ethylene glycol respectively, mixing the two solutions under a violent stirring condition, adding 0.3g of thioacetamide after magnetic stirring is uniform, transferring the mixed solution into an 80mL polytetrafluoroethylene-lined stainless steel autoclave, carrying out a first-step hydrothermal reaction at 160 ℃ for 16h, taking out a sample after hydrothermal reaction, cooling, centrifuging, washing, and vacuum-drying at 55 ℃ for 14h to obtain a Ni-Sn-S composite material; grinding the composite material, uniformly mixing the ground composite material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and drying the foam nickel sheet in a drying oven at the temperature of 60 ℃ for 12 hours to obtain a Ni-Sn-S working electrode (recorded as NNS-4).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: the method comprises the following steps of taking a foam nickel sheet of NNS-4 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability.
Example 5:
a preparation method of a Ni-Sn-S composite material comprises the following steps:
first, 2mmol of Na2SnO3And 2mmol of Ni (CH)3COO)2Dissolving the two solutions in a mixed solution of 10mL of water and 30mL of ethylene glycol respectively, mixing the two solutions under a violent stirring condition, adding 0.3g of thioacetamide after magnetic stirring is uniform, transferring the mixed solution into an 80mL polytetrafluoroethylene-lined stainless steel autoclave, carrying out a first-step hydrothermal reaction at 160 ℃ for 16h, taking out a sample after hydrothermal reaction, cooling, centrifuging, washing, and vacuum-drying at 65 ℃ for 10h to obtain a Ni-Sn-S composite material; grinding the composite material, uniformly mixing the ground composite material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and drying the foam nickel sheet in a drying oven at the temperature of 60 ℃ for 12 hours to obtain a Ni-Sn-S working electrode (recorded as NNS-5).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: the method comprises the following steps of taking a foam nickel sheet of NNS-5 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability.
Example 6:
a preparation method of a Ni-Sn-S composite material comprises the following steps:
first, 2mmol of Na2SnO3And 2mmol of Ni (CH)3COO)2Respectively dissolving in a mixed solution of 30mL of water and 10mL of ethylene glycol, and vigorously stirringMixing the two solutions obtained under the condition, adding 0.5g of thioacetamide after magnetic stirring uniformly, transferring the mixed solution into a 80mL stainless steel autoclave with a polytetrafluoroethylene lining, carrying out a first-step hydrothermal reaction at 160 ℃ for 16h, taking out a sample after hydrothermal reaction, cooling, centrifuging, washing, and carrying out vacuum drying at 60 ℃ for 12h to obtain a Ni-Sn-S composite material; grinding the composite material, uniformly mixing the ground composite material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and drying the foam nickel sheet in a drying oven at the temperature of 60 ℃ for 12 hours to obtain a Ni-Sn-S working electrode (recorded as NNS-6).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: the method comprises the following steps of taking a foam nickel sheet of NNS-6 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability.
Example 7:
a preparation method of a Ni-Sn-S composite material comprises the following steps:
first, 2mmol of Na2SnO3And 2mmol of Ni (CH)3COO)2Dissolving the two solutions in a mixed solution of 30mL of water and 10mL of ethylene glycol respectively, mixing the two solutions under a violent stirring condition, adding 0.3g of thioacetamide after magnetic stirring is uniform, transferring the mixed solution into an 80mL polytetrafluoroethylene-lined stainless steel autoclave, carrying out a first-step hydrothermal reaction at 120 ℃ for 24 hours, taking out a sample after hydrothermal reaction, cooling, centrifuging, washing, and carrying out vacuum drying at 60 ℃ for 12 hours to obtain a Ni-Sn-S composite material; grinding the composite material, uniformly mixing the ground composite material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:0.8:1.2, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and drying the foam nickel sheet in a drying oven at the temperature of 60 ℃ for 12 hours to obtain the Ni-Sn-S working electrode (recorded as NNS-7).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: the foam nickel sheet of NNS-7 is used as a working electrode, an Ag/AgCl electrode is used as a reference electrode, a Pt electrode is used as a counter electrode, and 2mol/L KOH is used as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability.
Example 8:
a preparation method of a Ni-Sn-S composite material comprises the following steps:
first, 1mmol of Na2SnO3And 2mmol of Ni (CH)3COO)2Dissolving the two solutions in a mixed solution of 30mL of water and 10mL of ethylene glycol respectively, mixing the two solutions under a violent stirring condition, adding 0.2g of thioacetamide after magnetic stirring is uniform, transferring the mixed solution into an 80mL polytetrafluoroethylene-lined stainless steel autoclave, carrying out a first-step hydrothermal reaction at 200 ℃ for 12h, taking out a sample after hydrothermal reaction, cooling, centrifuging, washing, and carrying out vacuum drying at 60 ℃ for 12h to obtain a Ni-Sn-S composite material; grinding the composite material, uniformly mixing the ground composite material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1.2:0.8, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and drying the foam nickel sheet in a drying oven at the temperature of 60 ℃ for 12 hours to obtain the Ni-Sn-S working electrode (recorded as NNS-8).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: the method comprises the following steps of taking a foam nickel sheet of NNS-8 as a working electrode, taking an Ag/AgCl electrode as a reference electrode, taking a Pt electrode as a counter electrode and taking 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability.
Example 9:
a preparation method of a Ni-Sn-S composite material comprises the following steps:
first, 2mmol of Na2SnO3And 2mmol of Ni (CH)3COO)2Dissolving in mixed solution of 30mL water and 10mL ethylene glycol, mixing the two solutions under vigorous stirring, adding 0.1g thioacetamide after magnetic stirring, addingTransferring the mixed solution into a 80mL stainless steel autoclave with a polytetrafluoroethylene lining, carrying out a first-step hydrothermal reaction at 160 ℃ for 18h, taking out a sample after hydrothermal reaction, cooling, centrifuging, washing, and vacuum-drying at 60 ℃ for 12h to obtain a Ni-Sn-S composite material; grinding the composite material, uniformly mixing the ground composite material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and drying the foam nickel sheet in a drying oven at the temperature of 60 ℃ for 12 hours to obtain a Ni-Sn-S working electrode (recorded as NNS-9).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: the foam nickel sheet of NNS-9 is used as a working electrode, an Ag/AgCl electrode is used as a reference electrode, a Pt electrode is used as a counter electrode, and 2mol/L KOH is used as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (7)
1. A preparation method of a Ni-Sn-S composite material is characterized by comprising the following steps:
1) mixing Na2SnO3Solution and Ni (CH)3COO)2Uniformly mixing the solution, adding thioacetamide and carrying out hydrothermal reaction;
2) after the hydrothermal reaction is finished, post-treating to obtain the Ni-Sn-S composite material;
in step 1), the Na2SnO3Solution and Ni (CH)3COO)2In the solution, the solvent is water and BA mixed solution of glycol; in the solvent, the volume ratio of water to glycol is 3 (1-9);
in the step 1), the mixing process is that Na is firstly mixed under the condition of vigorous stirring2SnO3Solution and Ni (CH)3COO)2Mixing the solution, and then uniformly stirring by magnetic force;
in the step 1), the temperature in the hydrothermal reaction is 120-.
2. The method for preparing Ni-Sn-S composite material according to claim 1, wherein in step 1), Na is added2SnO3In solution, Na2SnO3Has a molar concentration of 1-2mmol/40mL, and the Ni (CH)3COO)2In solution, Ni (CH)3COO)2The molar concentration of (b) is 1-2mmol/40 mL.
3. The method for preparing Ni-Sn-S composite material according to claim 1, wherein in step 1), Na is added2SnO3、Ni(CH3COO)2The addition amount ratio of the thioacetamide to the thioacetamide is 2mmol (1-4) mmol (0.1-0.5) g.
4. The method for preparing Ni-Sn-S composite material of claim 1, wherein in the step 2), the post-treatment comprises cooling, centrifuging, washing and drying, the drying is vacuum drying, and the temperature in the vacuum drying process is 55-65 ℃ and the time is 10-14 h.
5. A Ni-Sn-S composite material, characterized in that it is produced by a method according to any one of claims 1 to 4.
6. Use of the Ni-Sn-S composite material according to claim 5 to prepare a working electrode for use in a supercapacitor.
7. The use of the Ni-Sn-S composite material as claimed in claim 6, wherein the working electrode is prepared by the following steps: grinding the composite material, uniformly mixing the ground composite material with carbon black and polytetrafluoroethylene, then pressing the mixture on a foam nickel sheet, and drying to obtain the working electrode; the mass ratio of the composite material, the carbon black and the polytetrafluoroethylene is 8 (0.8-1.2) to (0.8-1.2).
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