CN109741962B - FeNi-S @ N-RGO nanosheet supercapacitor electrode material and preparation method thereof - Google Patents
FeNi-S @ N-RGO nanosheet supercapacitor electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a FeNi-S @ N-RGO nanosheet supercapacitor electrode material and a preparation method thereof. The preparation method comprises the following steps: the first step is as follows: mixing nickel chloride hexahydrate, ferric nitrate nonahydrate, urea, trisodium citrate dihydrate and deionized water, carrying out hydrothermal reaction in a hydrothermal kettle, centrifuging after the reaction is finished, washing and drying; the second step is that: adding the FeNi LDH and thioacetamide which are obtained in the first step through hydrothermal reaction into an ethanol solution, then carrying out hydrothermal reaction, and centrifuging, washing and drying after the reaction is finished to obtain a FeNi-S sample; the third step: mixing a FeNi-S sample and RGO, and calcining in a tubular furnace to prepare the FeNi-S @ N-RGO nanosheet electrode material. The preparation method is environment-friendly, simple and convenient for large-scale production.
Description
Technical Field
The invention belongs to the technical field of electrochemistry and nano materials, and particularly relates to a FeNi-S @ N-RGO nanosheet supercapacitor electrode material and a preparation method thereof.
Background
With the exhaustion of fossil energy and the severe environmental problems, the development and utilization of renewable clean energy becomes more and more important. Solar energy and wind energy are the most abundant and important renewable clean energy, and due to the natural characteristics of changeability and instability of the solar energy and the wind energy, the power generation output of the solar energy and the wind energy also has the characteristics of intermittence and changeability. In order to integrate these energy products into the power grid, it becomes important to construct a smart power grid by using the energy storage system and the new energy products together. The application research of the energy storage device with high power density and high energy density has important significance for constructing an advanced energy storage system in the future. In addition, the increasing popularization of portable electronic products and the vigorous development of new energy industries represented by electric vehicles provide unprecedented development opportunities for the research and application of energy storage devices, and also provide high requirements for the performance of the energy storage devices.
The super capacitor with ultra-high power density is a characteristic that all other energy storage devices do not have, and is the core competitiveness of the super capacitor. While lithium-sulfur batteries are one of the most promising and desirable high energy densities beyond the currently widely used lithium ion batteries. In order for an electrode material to have improved capacitance properties, the electrode material must have both a large specific surface area, a suitable pore size distribution, and high electrical conductivity. Amorphous carbon materials have a high specific surface area, but are poorly conductive; graphene has excellent conductivity and high specific surface area, and thus is not fully developed.
The development of efficient but low cost supercapacitor materials is the key to sustainable energy conversion technology. In this process, the ultra-thin nano-sheet of iron-nickel sulfide is synthesized. When tested for her electrochemical properties, these nanoflakes exhibit excellent activity and stability in alkaline solutions, which is an attractive alternative to precious Ru and other precious metals.
The graphene energy bands have no gaps, and the conductivity of the graphene energy bands cannot be completely controlled like the conductivity of a traditional semiconductor. The graphene does not have active functional groups on the surface, and is difficult to be compounded with other materials (such as metal particles), so that the application of the graphene in wider fields is hindered. In order to improve the defect that graphene has no energy band, a large amount of work on the functionalization of graphene has been carried out, and currently successful functionalization methods are as follows: the method comprises the steps of adding graphene surface functional groups, preparing graphene derivatives, chemically modifying, doping elements and the like. Wherein element doping is an effective way to optimize the chemical properties and electronic structure of graphene. Other atoms enter into the graphene crystal lattice, so that a band gap can be effectively introduced, and the defects and the reaction activity of the graphene can be increased, thereby improving the performance. According to research, nitrogen, oxygen, sulfur and other elements can be doped into graphene crystal lattices to change the performance of the graphene crystal lattices, wherein nitrogen atoms are introduced into the graphene to cremate carbon atoms adjacent to benzene rings, and the adsorption effect and the reaction activity of an oxidant are enhanced.
Disclosure of Invention
The invention aims to provide an environment-friendly FeNi-S @ N-RGO nanosheet supercapacitor electrode material which is simple in preparation method, greatly shortens the synthesis time and is convenient for large-scale production of high-purity FeNi-S @ N-RGO nanosheets and a preparation method thereof.
The technical scheme of the invention is specifically introduced as follows.
The invention provides a preparation method of a FeNi-S @ N-RGO nanosheet supercapacitor electrode material, which comprises the following specific steps:
the first step is as follows: adding nickel chloride hexahydrate, ferric nitrate nonahydrate, urea and trisodium citrate dihydrate into deionized water, transferring the mixture into a hydrothermal kettle after the nickel chloride hexahydrate, ferric nitrate nonahydrate, urea and trisodium citrate dihydrate are completely dissolved to perform hydrothermal reaction, and centrifuging, washing and drying the mixture after the reaction is finished to obtain a FeNi LDH sample;
the second step is that: dissolving a FeNi LDH sample in ethanol, adding thioacetamide, transferring the mixture into a hydrothermal kettle after the mixture is completely dissolved for hydrothermal reaction, and centrifuging, washing and drying the mixture after the reaction is finished to obtain a FeNi-S sample;
and thirdly, placing the FeNi-S sample and 4-6 mg/ml RGO aqueous solution in a quartz boat, and calcining in a tube furnace under the nitrogen atmosphere to prepare the FeNi-S @ N-RGO nanosheet electrode material.
In the first step, the hydrothermal reaction temperature for preparing the FeNi LDH sample is 140-160 ℃; the hydrothermal reaction time is 20-30 h.
In the first step, the molar ratio of nickel chloride hexahydrate, iron nitrate nonahydrate, urea and trisodium citrate dihydrate is 1: (18-21): (4-6): (1-3); the feeding mass ratio of the nickel chloride hexahydrate to the deionized water is 1: 200-1: 2500.
In the second step, the hydrothermal reaction temperature for preparing the FeNi-S sample is 110-130 ℃; the hydrothermal reaction time is 4-8 h.
In the second step, the feeding mass ratio of FeNi LDH, ethanol and thioacetamide is 1: (380-450): (1-2).
In the third step, the feeding mass ratio of the FeNi-S sample to the RGO is 1: 8-1: 10.
In the third step, the calcination temperature is 300-600 ℃ and the calcination time is 50-110 min under the nitrogen atmosphere.
The invention also provides the FeNi-S @ N-RGO nanosheet supercapacitor electrode material prepared by the preparation method.
In the invention, during electrochemical test, a FeNi-S @ N-RGO sample, carbon black and polytetrafluoroethylene are uniformly mixed and pressed on a foam nickel sheet (1cm multiplied by 1cm) according to the mass ratio of 8:1:1, and the mixture is dried for 12 hours in a drying oven at the temperature of 60 ℃ to prepare the working electrode.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention synthesizes FeNi-S @ N-RGO by two-step hydrothermal one-step calcination, greatly simplifies the reaction steps, improves the reaction rate and efficiency, and improves some physical and chemical properties of the synthesized product.
2. The FeNi-S @ N-RGO prepared by the method has better product dispersibility and no obvious cluster, and the structure can improve the electrochemical property of the substance.
3. The FeNi-S @ N-RGO nano material prepared by the method has stable electrochemical properties.
Drawings
FIG. 1 is an SEM photograph of FeNi-S @ N-RGO at 5 μm in example 1.
FIG. 2 is an SEM photograph of FeNi-S @ N-RGO at 10 μm in example 2.
FIG. 3 is a TEM image at RGO 100nm in example 1.
FIG. 4 is a TEM image at RGO 50nm in example 1.
FIG. 5 is a TEM image at RGO 0.5 μm in example 1.
FIG. 6 is a TEM image at RGO 200nm in example 1.
Detailed Description
The following examples are presented to enable one of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any manner.
Example 1
A preparation method of an FeNi-S @ N-RGO nanosheet supercapacitor electrode material comprises the following steps: first, 0.29ml of 1M NiCl was put in order2·6H2O, 2.9ml of 1M Fe (NO)3)3·9H2O, 11.2ml of 0.5M CH4N2O, 4ml of 0.1M C6H5Na3O7(molar ratio 1: 20: 5: 2) in a 250ml beaker and 160ml deionized water was injected. Transferring the mixture into a 200ml stainless steel autoclave lined with polytetrafluoroethylene after the mixture is completely dissolved, and carrying out a first-step hydrothermal reaction at the temperature of 150 ℃; the hydrothermal reaction time is 24 h. And centrifuging the obtained FeNi LDH sample, washing with water for three times, and drying. Weighing 80mg of FeNi LDH sample, dissolving in 40ml of ethanol, adding 0.1125g of thioacetamide, uniformly mixing, transferring to a 200ml polytetrafluoroethylene-lined stainless steel autoclave, and carrying out a second hydrothermal reaction at 120 ℃; and (3) cooling after the reaction is finished for 6 hours, centrifuging, washing with ethanol for three times, and drying in a 60-DEG C oven to obtain the FeNi-S ultrathin nanosheet. 10ml of 5mg/ml RGO aqueous solution is added into an obtained 80mg FeNi-S sample, wherein RGO is synthesized by Hummer (the shape and structure of the RGO are shown in figures 3-6), the completely mixed solution is placed into a quartz boat, the quartz boat is placed into a tube furnace to be heated in nitrogen atmosphere, the nitrogen flow rate is 50ml/min, the heating rate is 5 ℃/min, the temperature is slowly heated to 300 ℃ from the room temperature, and the carbonization time is 50 min. Fully grinding the obtained FeNi-S @ N-RGO active material (the SME figure of the material is shown in figure 1), mixing the FeNi-S @ N-RGO active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1, uniformly stirring, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and baking the foam nickel sheet for 12 hours at the temperature of 60 ℃ to obtain the working electrode.
Application example 1
The Chenhua CHI760e electrochemical workstation adopts cyclic voltammetry and constant-current charging and discharging methods to detect the specific capacitance and cyclic stability of the material, and cyclic voltammetry tests show that the material has excellent redox capability. The high specific surface area of the metamaterial is provided with a foundation by using an electron scanning microscope (for representing the surface microstructure of the electrode material). In 2mol/L KOH solution and under the current density of 1A/g, the voltage range selected by the cyclic Foam test is 0-0.6V, a pair of redox peaks exist, the highest charging and discharging voltage is 0.4V, and the measured specific capacitance of the electrode material reaches 273.6F/g.
Example 2
A FeNi-S @ N-RGO nanosheet supercapacitor electrode material and a preparation method thereof comprise the following steps: first, 0.29ml of 1M NiCl was put in order2·6H2O, 2.9ml of 1M Fe (NO)3)3·9H2O, 11.2ml of 0.5M CH4N2O, 4ml of 0.1MC6H5Na3O7(molar ratio 1: 20: 5: 2) in a 250ml beaker and 160ml deionized water was injected. Transferring the mixture into a 200ml stainless steel autoclave lined with polytetrafluoroethylene after the mixture is completely dissolved, and carrying out a first-step hydrothermal reaction at the temperature of 150 ℃; the hydrothermal reaction time is 24 h. And centrifuging the obtained FeNi LDH sample, washing with water for three times, and drying. Weighing 80mg of FeNi LDH sample, dissolving in 40ml of ethanol, adding 0.1125g of thioacetamide, uniformly mixing, transferring to a 200ml of polytetrafluoroethylene-lined stainless steel autoclave, carrying out a second hydrothermal reaction at 120 ℃ for 6h, cooling after the reaction is finished, centrifuging, washing with ethanol for three times, and drying in a 60 ℃ oven to obtain the FeNi-S ultrathin nanosheet. 10ml of 5mg/ml RGO aqueous solution is added into the obtained 80mg FeNi-S sample, wherein RGO is synthesized by Hummer, the completely mixed solution is put into a quartz boat, the quartz boat is placed in a tube furnace to be heated under nitrogen atmosphere, the nitrogen flow rate is 50ml/min, the temperature rising rate is 5 ℃/min, the temperature is slowly heated to 450 ℃ from room temperature, and the carbonization time is 80 min. Fully grinding the obtained FeNi-S @ N-RGO active material (the SME figure of the material is shown in figure 2), mixing the FeNi-S @ N-RGO active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1, uniformly stirring, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and baking the foam nickel sheet for 12 hours at the temperature of 60 ℃ to obtain the working electrode.
Application example 2
The Chenhua CHI760e electrochemical workstation adopts cyclic voltammetry and constant-current charging and discharging methods to detect the specific capacitance and cyclic stability of the material, and cyclic voltammetry tests show that the material has excellent redox capability. The high specific surface area of the metamaterial is provided with a foundation by using an electron scanning microscope (for representing the surface microstructure of the electrode material). The specific capacitance of the electrode material reaches 312.6F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 3
A FeNi-S @ N-RGO nanosheet supercapacitor electrode material and a preparation method thereof comprise the following steps: first, 0.29ml of 1M NiCl was put in order2·6H2O, 2.9ml of 1M Fe (NO)3)3·9H2O, 11.2ml of 0.5M CH4N2O, 4ml of 0.1M C6H5Na3O7(molar ratio 1: 20: 5: 2) in a 250ml beaker and 160ml deionized water was injected. Transferring the mixture into a 200ml stainless steel autoclave lined with polytetrafluoroethylene after the mixture is completely dissolved, and carrying out a first-step hydrothermal reaction at the temperature of 150 ℃; the hydrothermal reaction time is 24 h. And centrifuging the obtained FeNi LDH sample, washing with water for three times, and drying. Weighing 80mg of FeNi LDH sample, dissolving in 40ml of ethanol, adding 0.1125g of thioacetamide, uniformly mixing, transferring to a 200ml of polytetrafluoroethylene-lined stainless steel autoclave, carrying out a second hydrothermal reaction at 120 ℃ for 6h, cooling after the reaction is finished, centrifuging, washing with ethanol for three times, and drying in a 60 ℃ oven to obtain the FeNi-S ultrathin nanosheet. 10ml of 5mg/ml RGO aqueous solution is added into the obtained 80mg FeNi-S sample, wherein RGO is synthesized by Hummer, the completely mixed solution is put into a quartz boat, the quartz boat is placed in a tube furnace to be heated under nitrogen atmosphere, the nitrogen flow rate is 50ml/min, the temperature rising rate is 5 ℃/min, the temperature is slowly heated to 600 ℃ from room temperature, and the carbonization time is 110 min. Fully grinding the obtained FeNi-S @ N-RGO active material, mixing the FeNi-S @ N-RGO active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1, uniformly stirring, pressing the mixture on a foam nickel sheet (1cm multiplied by 1cm), and baking the foam nickel sheet for 12 hours at the temperature of 60 ℃ to obtain the working electrode.
Application example 3
The Chenhua CHI760e electrochemical workstation adopts cyclic voltammetry and constant-current charging and discharging methods to detect the specific capacitance and cyclic stability of the material, and cyclic voltammetry tests show that the material has excellent redox capability. The high specific surface area of the metamaterial is provided with a foundation by using an electron scanning microscope (for representing the surface microstructure of the electrode material). The specific capacitance of the electrode material of the invention reaches 297.3F/g in 2mol/L KOH solution and at a current density of 1A/g.
Comparative example 1
FeNi-SCThe nano-sheet super capacitor electrode material and the preparation method thereof comprise the following steps: first, 0.29ml of 1M NiCl was put in order2·6H2O, 2.9ml of 1M Fe (NO)3)3·9H2O, 11.2ml of 0.5M CH4N2O, 4ml of 0.1M C6H5Na3O70.1125g of thioacetamide in a 250ml beaker and 160ml of deionized water were poured. Transferring the mixture into a 200ml stainless steel autoclave lined with polytetrafluoroethylene after the mixture is completely dissolved, and carrying out hydrothermal reaction at the temperature of 150 ℃; the hydrothermal reaction time is 24 h. And cooling after the reaction is finished, centrifuging, respectively cleaning with deionized water and ethanol, and drying in a drying oven at 60 ℃ to obtain the FeNi-S ultrathin nanosheet. FeNi-S is obtained1And putting the sample into a quartz boat, putting the quartz boat into a tube furnace, and carrying out carbon burning in a nitrogen atmosphere at the nitrogen flow rate of 50ml/min and the heating rate of 5 ℃/min, slowly heating the sample from room temperature to 450 ℃ and carbonizing the sample for 50 min. The obtained FeNi-SCFully grinding the active material, mixing the active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1, uniformly stirring, pressing on a foam nickel sheet (1cm multiplied by 1cm), and baking for 12 hours at 60 ℃ to obtain the working electrode.
Application performance testing
The Chenhua CHI760e electrochemical workstation adopts cyclic voltammetry and constant-current charging and discharging methods to detect the specific capacitance and cyclic stability of the material, and cyclic voltammetry tests show that the material has excellent redox capability. The high specific surface area of the metamaterial is provided with a foundation by using an electron scanning microscope (for representing the surface microstructure of the electrode material). The specific capacitance of the electrode material reaches 234.2F/g in 2mol/L KOH solution and at a current density of 1A/g.
Claims (8)
1. A preparation method of an FeNi-S @ N-RGO nanosheet supercapacitor electrode material is characterized by comprising the following specific steps:
the first step is as follows: adding nickel chloride hexahydrate, ferric nitrate nonahydrate, urea and trisodium citrate dihydrate into deionized water, transferring the mixture into a hydrothermal kettle after the mixture is completely dissolved for hydrothermal reaction, centrifuging after the reaction is finished, washing and drying to obtain a FeNi LDH sample;
the second step is that: dissolving a FeNi LDH sample in ethanol, adding thioacetamide, transferring the mixture into a hydrothermal kettle after the mixture is completely dissolved for hydrothermal reaction, and centrifuging, washing and drying the mixture after the reaction is finished to obtain a FeNi-S sample;
and thirdly, placing the FeNi-S sample and 4-6 mg/ml RGO aqueous solution in a quartz boat, and calcining in a tube furnace under the nitrogen atmosphere to prepare the FeNi-S @ N-RGO nanosheet electrode material.
2. The preparation method of claim 1, wherein in the first step, the hydrothermal reaction temperature for preparing the FeNi LDH sample is 140-160 ℃; the hydrothermal reaction time is 20-30 h.
3. The method of claim 1, wherein in the first step, the molar ratio of nickel chloride hexahydrate, iron nitrate nonahydrate, urea and trisodium citrate dihydrate is 1: (18-21): (4-6): (1-3); the feeding mass ratio of the nickel chloride hexahydrate to the deionized water is 1: 200-1: 2500.
4. The preparation method according to claim 1, wherein in the second step, the hydrothermal reaction temperature for preparing the FeNi-S sample is 110 to 130 ℃; the hydrothermal reaction time is 4-8 h.
5. The preparation method of claim 1, wherein in the second step, the FeNi LDH sample, ethanol and thioacetamide are fed in a mass ratio of 1: (380-450): (1-2).
6. The method according to claim 1, wherein in the third step, the mass ratio of the FeNi-S sample to the RGO is 1: 8-1: 10.
7. The method according to claim 1, wherein in the third step, the calcination temperature is 300 to 600 ℃ and the calcination time is 50 to 110min under a nitrogen atmosphere.
8. The FeNi-S @ N-RGO nanosheet supercapacitor electrode material prepared according to the preparation method of one of claims 1 to 7.
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| CN106601500A (en) * | 2017-01-19 | 2017-04-26 | 三峡大学 | Vulcanized modification method for Ni-Fe LDH electrode material |
| CN107761128A (en) * | 2017-11-10 | 2018-03-06 | 上海应用技术大学 | A kind of FeNiNC electrode materials, preparation method and applications |
| CN107946089A (en) * | 2017-11-17 | 2018-04-20 | 常州大学 | A kind of MnFe2O4The preparation method of/rGO composite materials and its application as electrode material for super capacitor |
| CN108878167A (en) * | 2018-07-03 | 2018-11-23 | 上海应用技术大学 | A kind of supercapacitor CoNi2S4/ graphene composite material and preparation method thereof |
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| CN106601500A (en) * | 2017-01-19 | 2017-04-26 | 三峡大学 | Vulcanized modification method for Ni-Fe LDH electrode material |
| CN107761128A (en) * | 2017-11-10 | 2018-03-06 | 上海应用技术大学 | A kind of FeNiNC electrode materials, preparation method and applications |
| CN107946089A (en) * | 2017-11-17 | 2018-04-20 | 常州大学 | A kind of MnFe2O4The preparation method of/rGO composite materials and its application as electrode material for super capacitor |
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