CN109003832B - Preparation method and application of three-dimensional porous graphene/nickel cobalt sulfide composite material - Google Patents
Preparation method and application of three-dimensional porous graphene/nickel cobalt sulfide composite material Download PDFInfo
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- CN109003832B CN109003832B CN201810843976.3A CN201810843976A CN109003832B CN 109003832 B CN109003832 B CN 109003832B CN 201810843976 A CN201810843976 A CN 201810843976A CN 109003832 B CN109003832 B CN 109003832B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/84—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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention belongs to the field of nano materials and electrochemistry, and particularly relates to a preparation method of a three-dimensional porous graphene/nickel cobalt sulfide composite material. Deionized water and n-octane are used as solvents, sulfur, nickel nitrate and cobalt nitrate are used as a sulfur source, a nickel source and a cobalt source, cetyl trimethyl ammonium bromide is used as a surfactant, the materials are reacted in a stainless steel high-pressure reaction kettle for a period of time to obtain a three-dimensional porous graphene/nickel cobalt sulfide composite material, the three-dimensional porous graphene/nickel cobalt sulfide composite material is coated on the surface of foamed nickel, and the three-dimensional porous graphene/nickel cobalt sulfide composite material is dried in vacuum and then pressed into an electrode material. According to the invention, the morphology of the composite material is regulated, so that the composite electrode material has a larger specific surface area, and is fully contacted with the electrolyte, and the electrochemical performance is improved.
Description
Technical Field
The invention belongs to the field of nano materials and electrochemistry, and particularly relates to a preparation method and application of a three-dimensional porous graphene/nickel cobalt sulfide composite material.
Background
In the 21 st century, "energy" has become the focus of competition among countries. In the face of the upcoming energy crisis, scientists are actively developing energy-saving and efficient energy storage devices while trying to find new energy. In a new energy storage device, a super capacitor is receiving more and more attention due to its advantages of large power density, fast charge and discharge speed, long cycle life, and the like. Among the many components of supercapacitors, the characteristics and combination of electrode materials have a large impact on the performance of the supercapacitor.
Graphene is a two-dimensional allotrope of carbon, and integrates a plurality of excellent characteristics such as high theoretical specific surface area, high carrier mobility, good light transmission, high thermal conductivity, high mechanical strength, high electrochemical stability and the like. The most surprising feature of the graphene is the electrical properties of the unique electronic structure of graphene, such as electron ballistic transport at room temperature, abnormal quantum hall effect, quantum tunneling effect, and the like. However, when pure graphene is used as an electrode material of a supercapacitor, the performance of the graphene cannot meet the requirements of people, and on one hand, the graphene prepared by a chemical method is easy to agglomerate due to pi-pi acting force between sheet layers, so that the specific surface area of the graphene is reduced; on the other hand, it exhibits a specific capacitance that is not comparable to the faradaic capacitance, subject to the double layer capacitance mechanism. Therefore, the agglomeration of the graphene is reduced by preparing the three-dimensional porous graphene, and the introduction of the super-capacitance characteristic of the Faraday pseudocapacitance improving material is particularly important.
Disclosure of Invention
The invention aims to provide a preparation method and application of a three-dimensional porous graphene/nickel cobalt sulfide composite material aiming at the defects of the prior art. By regulating the morphology of the composite material, the composite electrode material has a larger specific surface area, so that the composite electrode material is in full contact with electrolyte, and the electrochemical performance is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a three-dimensional porous graphene/nickel cobalt sulfide composite material comprises the following steps:
(1) weighing graphene oxide and hexadecyl trimethyl ammonium bromide, respectively dissolving the graphene oxide and the hexadecyl trimethyl ammonium bromide in deionized water, mixing the graphene oxide and the hexadecyl trimethyl ammonium bromide and performing ultrasonic treatment;
(2) weighing sulfur, ultrasonically dispersing the sulfur in n-octane to obtain n-octane mixed liquid, dropwise adding the obtained n-octane mixed liquid into the solution obtained in the step (1), and magnetically stirring;
(3) weighing nickel nitrate and cobalt nitrate, dissolving in deionized water, dropwise adding into the mixed solution obtained in the step (2), and magnetically stirring;
(4) transferring the mixture obtained in the step (3) into a stainless steel high-pressure reaction kettle with a Teflon lining, and placing the stainless steel high-pressure reaction kettle in an oven for reaction;
(5) and (4) naturally cooling the product obtained by the reaction in the step (4) to room temperature, centrifuging, washing, vacuum drying, and calcining at high temperature to obtain the three-dimensional porous graphene/nickel cobalt sulfide composite material.
According to the mass ratio, the graphene oxide, the sulfur and the hexadecyl trimethyl ammonium bromide are =1:3 and (5 ~ 10).
In the step (1), the technological parameters of the ultrasound are that the ultrasound power is 200W, the ultrasound temperature is 25 ℃, and the ultrasound time is 1 ~ 2 h.
The volume ratio of the n-octane in the step (2) to the deionized water in the step (1) is 1 (1 ~ 5).
In the step (3), the molar ratio of cobalt nitrate to nickel nitrate =1 (0.5 ~ 2).
In the step (4), the technological parameters for the reaction in the oven are that the reaction temperature is 160 ℃, ~ 240 ℃ and the reaction time is 12 ~ 24 h.
In the step (5), the calcination process parameters are that the calcination atmosphere is argon, the calcination temperature is 500 ℃, and the calcination time is 1 ~ 3 h.
Uniformly mixing the prepared three-dimensional porous graphene/nickel cobalt sulfide with acetylene black serving as a conductive agent and PVDF serving as a binder, then dropwise adding a proper amount of N-methylpyrrolidone (NMP) solvent to prepare uniform viscous slurry, uniformly coating the viscous slurry on a processed foamed nickel current collector, performing vacuum drying and pressing into a sheet to obtain a working electrode for testing; according to the mass ratio, the three-dimensional porous graphene/nickel cobalt sulfide composite material comprises the following components: conductive agent acetylene black: binder PVDF =80:15: 5.
The pretreatment process of the foamed nickel comprises the following steps: cutting foamed nickel with the thickness of 0.5mm into L-shaped strips with the thickness of 1 cm multiplied by 1 cm, washing the L-shaped strips with dilute hydrochloric acid, acetone and ethanol in sequence to remove oxides and other pollutants on the surface, finally washing the L-shaped strips with a large amount of deionized water by ultrasound, and finally drying the L-shaped strips for 24 hours under the vacuum condition at the temperature of 60 ℃.
The invention has the beneficial effects that:
according to the invention, n-octane is used as a soft membrane, graphene oxide is wrapped around the n-octane, and when the n-octane is evaporated, a pore channel with three-dimensional stacked graphene can be obtained, and defects can be remained on a two-dimensional base surface of the graphene under the high-temperature and high-pressure environment. In addition, under the synergy of the surfactant, granular nickel-cobalt sulfide grows on the basal plane of the graphene. The obtained electrode has higher specific capacitance and can be used as an electrode material of a super capacitor.
Drawings
Fig. 1 is an XRD spectrum of a three-dimensional porous graphene/nickel cobalt sulfide composite material prepared by the present invention;
FIG. 2 is a scanning electron microscope picture of a three-dimensional porous graphene/nickel cobalt sulfide composite material prepared by the invention;
FIG. 3 is a cyclic voltammetry curve of a three-dimensional porous graphene/nickel cobalt sulfide composite material prepared by the present invention;
fig. 4 is a cycle stability curve diagram of the three-dimensional porous graphene/nickel cobalt sulfide composite material prepared by the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.
Example 1
A preparation method of a three-dimensional porous graphene/nickel cobalt sulfide composite material comprises the following specific steps:
(1) weighing 0.1g of graphene oxide and 1g of hexadecyl trimethyl ammonium bromide, respectively dissolving in 20mL of deionized water, mixing the graphene oxide and the hexadecyl trimethyl ammonium bromide, and carrying out ultrasonic treatment on the graphene oxide and the hexadecyl trimethyl ammonium bromide, wherein the ultrasonic power is 200W, the ultrasonic temperature is 25 ℃, and the ultrasonic treatment time is 2 hours;
(2) weighing 0.3g of sulfur, ultrasonically dispersing the sulfur in 20mL of n-octane, dropwise adding the obtained n-octane mixed liquid into the solution obtained in the step (1), and magnetically stirring for 60 minutes;
(3) weighing 0.2g of nickel nitrate and 0.1g of cobalt nitrate, dissolving in deionized water, dropwise adding into the mixed solution obtained in the step (2), and magnetically stirring for 30 minutes;
(4) transferring the mixture obtained in the step (3) into a stainless steel high-pressure reaction kettle with a 100mL teflon lining, placing the stainless steel high-pressure reaction kettle into an oven, and preserving heat for 24 hours at 180 ℃;
(5) taking out the high-pressure reaction kettle, naturally cooling to room temperature, centrifuging, washing and vacuum drying the obtained product, and calcining for 2 hours at 500 ℃ under the protection atmosphere of argon to obtain the three-dimensional porous graphene/nickel-cobalt sulfide composite material;
(6) uniformly mixing 3.2mg of three-dimensional porous graphene/nickel cobalt sulfide, 0.6mg of conductive agent acetylene black and 0.2mg of binder PVDF according to the proportion of 80:15:5, and then dropwise addingOne drop of the liquidN-methyl pyrrolidone (NMP) solvent, preparing into uniform viscous slurry, and homogenizingUniformly coating the mixture on a pretreated foamed nickel current collector, drying in vacuum and pressing into a sheet to obtain a working electrode for testing; the pretreatment process of the foamed nickel comprises the following steps: cutting foamed nickel with the thickness of 0.5mm into L-shaped strips with the thickness of 1 cm multiplied by 1 cm, washing the L-shaped strips with dilute hydrochloric acid, acetone and ethanol in sequence to remove oxides and other pollutants on the surface, finally washing the L-shaped strips with a large amount of deionized water by ultrasound, and finally drying the L-shaped strips for 24 hours under the vacuum condition at the temperature of 60 ℃.
Example 2
A preparation method of a three-dimensional porous graphene/nickel cobalt sulfide composite material comprises the following specific steps:
(1) weighing 0.1g of graphene oxide and 1g of hexadecyl trimethyl ammonium bromide, respectively dissolving in 20mL of deionized water, mixing the graphene oxide and the hexadecyl trimethyl ammonium bromide, and carrying out ultrasonic treatment on the graphene oxide and the hexadecyl trimethyl ammonium bromide, wherein the ultrasonic power is 200W, the ultrasonic temperature is 25 ℃, and the ultrasonic treatment time is 2 hours;
(2) weighing 0.3g of sulfur, ultrasonically dispersing the sulfur in 20mL of n-octane, dropwise adding the obtained n-octane mixed liquid into the solution obtained in the step (1), and magnetically stirring for 60 minutes;
(3) weighing 0.15g of nickel nitrate and 0.15g of cobalt nitrate, dissolving in deionized water, dropwise adding into the mixed solution obtained in the step (2), and magnetically stirring for 30 minutes;
(4) transferring the mixture obtained in the step (3) into a stainless steel high-pressure reaction kettle with a 100mL teflon lining, placing the stainless steel high-pressure reaction kettle into an oven, and preserving heat for 24 hours at 180 ℃;
(5) taking out the high-pressure reaction kettle, naturally cooling to room temperature, centrifuging, washing and vacuum drying the obtained product, and calcining for 2 hours at 500 ℃ under the protection atmosphere of argon to obtain the three-dimensional porous graphene/nickel-cobalt sulfide composite material;
(6) uniformly mixing 3.2mg of three-dimensional porous graphene/nickel cobalt sulfide, 0.6mg of conductive electrode agent acetylene black and 0.2mg of binder PVDF according to the proportion of 80:15:5, then dropwise adding a drop of N-methyl pyrrolidone (NMP) solvent to prepare uniform viscous slurry, uniformly coating the slurry on a pretreated foamed nickel current collector, drying in vacuum and pressing into a sheet to obtain a working electrode for testing; the pretreatment process of the foamed nickel comprises the following steps: cutting foamed nickel with the thickness of 0.5mm into L-shaped strips with the thickness of 1 cm multiplied by 1 cm, washing the L-shaped strips with dilute hydrochloric acid, acetone and ethanol in sequence to remove oxides and other pollutants on the surface, finally washing the L-shaped strips with a large amount of deionized water by ultrasound, and finally drying the L-shaped strips for 24 hours under the vacuum condition at the temperature of 60 ℃.
Example 3
A preparation method of a three-dimensional porous graphene/nickel cobalt sulfide composite material comprises the following specific steps:
(1) weighing 0.1g of graphene oxide and 1g of hexadecyl trimethyl ammonium bromide, respectively dissolving in 20mL of deionized water, mixing the graphene oxide and the hexadecyl trimethyl ammonium bromide, and carrying out ultrasonic treatment on the graphene oxide and the hexadecyl trimethyl ammonium bromide, wherein the ultrasonic power is 200W, the ultrasonic temperature is 25 ℃, and the ultrasonic treatment time is 2 hours;
(2) weighing 0.3g of sulfur, ultrasonically dispersing the sulfur in 20mL of n-octane, dropwise adding the obtained n-octane mixed liquid into the solution obtained in the step (1), and magnetically stirring for 60 minutes;
(3) weighing 0.1g of nickel nitrate and 0.2g of cobalt nitrate, dissolving in deionized water, dropwise adding into the mixed solution obtained in the step (2), and magnetically stirring for 30 minutes;
(4) transferring the mixture obtained in the step (3) into a stainless steel high-pressure reaction kettle with a 100mL teflon lining, placing the stainless steel high-pressure reaction kettle into an oven, and preserving heat for 24 hours at 180 ℃;
(5) taking out the high-pressure reaction kettle, naturally cooling to room temperature, centrifuging, washing and vacuum drying the obtained product, and calcining for 2 hours at 500 ℃ under the protection atmosphere of argon to obtain the three-dimensional porous graphene/nickel-cobalt sulfide composite material;
(6) uniformly mixing 3.2mg of three-dimensional porous graphene/nickel cobalt sulfide, 0.6mg of conductive electrode agent acetylene black and 0.2mg of binder PVDF according to the proportion of 80:15:5, then dropwise adding a drop of N-methyl pyrrolidone (NMP) solvent to prepare uniform viscous slurry, uniformly coating the slurry on a pretreated foamed nickel current collector, drying in vacuum and pressing into a sheet to obtain a working electrode for testing; the pretreatment process of the foamed nickel comprises the following steps: cutting foamed nickel with the thickness of 0.5mm into L-shaped strips with the thickness of 1 cm multiplied by 1 cm, washing the L-shaped strips with dilute hydrochloric acid, acetone and ethanol in sequence to remove oxides and other pollutants on the surface, finally washing the L-shaped strips with a large amount of deionized water by ultrasound, and finally drying the L-shaped strips for 24 hours under the vacuum condition at the temperature of 60 ℃.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (4)
1. A preparation method of a three-dimensional porous graphene/nickel cobalt sulfide composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing graphene oxide and hexadecyl trimethyl ammonium bromide, respectively dissolving the graphene oxide and the hexadecyl trimethyl ammonium bromide in deionized water, mixing the graphene oxide and the hexadecyl trimethyl ammonium bromide and performing ultrasonic treatment;
(2) weighing sulfur, ultrasonically dispersing the sulfur in n-octane to obtain n-octane mixed liquid, dropwise adding the obtained n-octane mixed liquid into the solution obtained in the step (1), and magnetically stirring;
(3) weighing nickel nitrate and cobalt nitrate, dissolving in deionized water, dropwise adding into the mixed solution obtained in the step (2), and magnetically stirring;
(4) transferring the mixed solution obtained in the step (3) into a stainless steel high-pressure reaction kettle with a Teflon lining, and placing the stainless steel high-pressure reaction kettle in an oven for reaction;
(5) naturally cooling the product obtained by the reaction in the step (4) to room temperature, centrifuging, washing, vacuum drying, and finally calcining to obtain the three-dimensional porous graphene/nickel cobalt sulfide composite material;
according to the mass ratio, the graphene oxide comprises sulfur, hexadecyl trimethyl ammonium bromide =1:3 and (5 ~ 10);
in the step (4), the technological parameters for reaction in the oven are that the reaction temperature is 160 ℃, ~ 240 ℃ and the reaction time is 12 ~ 24 h;
in the step (5), the calcination process parameters are that the calcination atmosphere is argon, the calcination temperature is 500 ℃, and the calcination time is 1 ~ 3 h.
2. The preparation method of the three-dimensional porous graphene/nickel cobalt sulfide composite material according to claim 1, wherein in the step (1), the ultrasonic process parameters are that the ultrasonic power is 200W, the ultrasonic temperature is 25 ℃, and the ultrasonic time is 1 ~ 2 h.
3. The method for preparing the three-dimensional porous graphene/nickel cobalt sulfide composite material according to claim 1, wherein the volume ratio of n-octane in the step (2) to the deionized water in the step (1) is 1 (1 ~ 5).
4. The method for preparing the three-dimensional porous graphene/nickel cobalt sulfide composite material according to claim 1, wherein in the step (3), the molar ratio of cobalt nitrate to nickel nitrate is =1 (0.5 ~ 2).
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