CN114843109B - Sea urchin-shaped MoS 2 Foam nickel composite capacitor electrode material and preparation method thereof - Google Patents
Sea urchin-shaped MoS 2 Foam nickel composite capacitor electrode material and preparation method thereof Download PDFInfo
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- CN114843109B CN114843109B CN202210517687.0A CN202210517687A CN114843109B CN 114843109 B CN114843109 B CN 114843109B CN 202210517687 A CN202210517687 A CN 202210517687A CN 114843109 B CN114843109 B CN 114843109B
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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
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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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a sea urchin-shaped MoS 2 Preparation method and application of foam nickel composite capacitor electrode material. Water and n-butanol are used as solvents, cetyl trimethyl ammonium bromide is used as a surfactant and a protective agent, sodium molybdate is used as a molybdenum source, hydrochloric acid provides an acidic environment, thiourea is used as a sulfur source, and a molybdenum precursor is constructed on pretreated foam nickel through a primary hydrothermal reaction; annealing at 400 ℃ in argon for 1h, preparing the sea urchin-shaped MoS 2 Nickel foam composite capacitor electrode material. In the present invention, sea urchin-like MoS 2 And general MoS 2 In contrast, when the surface areas are the same, the sea urchin-like MoS 2 The specific surface area of (2) is larger, more active sites can be provided, and the electrochemical performance is more excellent. The obtained sea urchin-shaped MoS 2 The foam nickel composite capacitor electrode material not only has better conductivity and higher specific capacitance, but also has soft mechanical characteristics, and can be used for super capacitor electrode materials.
Description
Technical Field
The invention belongs to the field of nano materials and electrochemistry, and in particular relates to a sea urchin-shaped MoS 2 Preparation method and application of foam nickel composite capacitor electrode material.
Background
Compared with a battery and an electric double layer capacitor, the super capacitor has the advantages of high power density, high charge and discharge speed, long cycle life and the like, and is an irreplaceable high-efficiency energy storage device. The super capacitor mainly comprises four parts of a current collector, an electrode, an electrolyte and a diaphragm, wherein the structure and the characteristics of an electrode material are key factors for determining the performance of the super capacitor. Hitherto, there have been many reports on metal oxides, metal hydroxides, metal sulfides as electrode materials, such as Co 2 O 3 、NiCo 2 O 4 、Ni(OH) 2 、Co(OH) 2 And NiCo 2 S 4 Etc., but there have been less researches on molybdenum sulfide as an electrode material. A metal sulfide is a metal compound having good electrochemical activity, which exhibits highly reversible redox reactions under alkaline conditions, and has a lower band gap and thus better conductivity than oxides of the same metal species. Among these metal sulfides, moS 2 Compared with NiS, coS 2 、Co 9 S 8 Metal sulfides such as CuS and the like show better oxidation-reduction capability, so that the metal sulfides have rapid electron transfer capability and charge-discharge capability.
The nickel foam is net-shaped, which facilitates the growth of the precursor thereon, and has excellent electrical conductivity. In addition, the network structure leads to large specific surface area of the foam nickel, and can enable the precursor to grow fully and uniformly. The nano-structure metal sulfide constructed on the surface of the foam nickel is beneficial to the diffusion of electrolyte charges on the surface or in the bulk phase of the foam nickel, so that the composite electrode material has larger specific capacitance and energy density, and the overall structural stability of the electrode material is more excellent.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art and providing a sea urchin-shaped MoS 2 Preparation method and application of foam nickel composite capacitor electrode material. By constructing nano-structure MoS on the surface of foam nickel 2 The composite electrode material has larger specific capacitance and energy density.
In order to achieve the above purpose, the invention adopts the following technical scheme:
sea urchin-shaped MoS prepared by water-oil two-phase method 2 Preparation method of foam nickel composite capacitor electrode material, sea urchin-shaped MoS prepared by water-oil two-phase method 2 The foam nickel composite capacitor electrode material is prepared from sea urchin-shaped MoS 2 The preparation method of the composite material formed by uniformly distributing the composite material on the surface of the foam nickel comprises the following steps:
(1) Pretreating foam nickel;
(2) Dissolving sodium molybdate in deionized water, dissolving cetyl trimethyl ammonium bromide in n-butanol, then dropwise adding the aqueous solution dissolved with sodium molybdate into the n-butanol solution dissolved with cetyl trimethyl ammonium bromide, and fully stirring; then hydrochloric acid is added into the mixed solution drop by drop, and the mixture is fully stirred; then thiourea is added and stirred vigorously; then adding the foam nickel pretreated in the step (1), and continuing to uniformly ultrasonically process;
(3) Carrying out hydrothermal reaction on the system in the step (2) in a polytetrafluoroethylene reaction kettle, wherein the reaction temperature is 180 ℃, and the reaction time is 24 hours;
(4) And (3) centrifuging the product obtained in the step (3) by using deionized water, washing, drying in vacuum, and annealing in argon for 1h at 400 ℃.
The pretreatment process of the foam nickel in the step (1) comprises the following steps: ultrasonic cleaning foam nickel with sodium hydroxide, hydrochloric acid, ethanol and deionized water for 4h, and vacuum drying at 60deg.C for 24h.
The amount of sodium molybdate added in the step (2) is 0.5 to 2.5mmol, the amount of cetyltrimethylammonium bromide added is 15mmol, and the amount of hydrochloric acid added is 1ml.
The molar ratio of the cetyl trimethyl ammonium bromide to the thiourea is 1:1.
Sea urchin-like MoS prepared by the preparation method 2 The foam nickel composite capacitor electrode material is used as a supercapacitor electrode material.
The invention has the beneficial effects that:
(1) In the invention, sea urchin-shaped MoS is obtained through one-time hydrothermal reaction and one-time high-temperature calcination 2 The preparation process is simple, the secondary hydrothermal reaction is not needed, the preparation process is simple, and the time is saved;
(2) Sea urchin-like MoS 2 And general MoS 2 In contrast, when the surface areas are the same, the sea urchin-like MoS 2 Is larger because of the sea urchin-like MoS 2 The ball body can be regarded as being full of thorns outside the ball body, the thorns also have the outer surfaces of the ball body, and more active sites can be provided for electrochemical tests, so that the electrochemical performance of the ball body is more excellent;
(3) Prepared sea urchin-like MoS 2 In the foam nickel composite capacitor electrode material, the specific surface area is larger, the active sites are more, and therefore, ions in the electrolyte can be matched with sea urchin-shaped MoS during charging and discharging in the electrolyte 2 The oxidation-reduction reaction sufficiently occurs. During charging, ions in the electrolyte enter sea urchin-shaped MoS 2 Is subjected to a reduction reaction; during discharge, ions in the electrolyte are extracted from sea urchin-like MoS 2 Is evolved, and oxidation reaction occurs.
Drawings
FIG. 1 shows a sea urchin-like MoS prepared according to the present invention 2 SEM image of nickel foam composite capacitor electrode material;
FIG. 2 shows sea urchin-like MoS prepared according to the present invention 2 Constant current charge-discharge curve of the foam nickel composite capacitor electrode material;
FIG. 3 is a block MoS prepared in comparative example 2 SEM image of the nickel foam composite capacitor electrode material.
Detailed Description
The invention is further illustrated below in connection with specific examples, but the invention is not limited to these examples only.
Example 1
Sea urchin-shaped MoS 2 The preparation method of the foam nickel composite capacitor electrode material comprises the following specific processes:
(1) Pretreatment of foam nickel
The nickel foam was sheared into L-shape 1cm x 1cm, ultrasonically cleaned with sodium hydroxide, hydrochloric acid, ethanol and deionized water, respectively, for 4 hours, and vacuum dried at 60 ℃ for 24h.
(2) Loaded molybdenum precursor
Dissolving 0.5mmol of sodium molybdate in 60ml of deionized water to form sodium molybdate aqueous solution; 15mmol of cetyltrimethylammonium bromide are dissolved in 20ml of n-butanol to which 1ml of hydrochloric acid is added; then dropwise adding the aqueous solution of sodium molybdate into n-butanol solution of hydrochloric acid dissolved with cetyltrimethylammonium bromide, and fully stirring for 2h; then 15mmol of thiourea is added and stirred vigorously for 2h; then adding the foam nickel pretreated in the step (1), and continuing to carry out ultrasonic treatment for 1h;
pouring the system into a polytetrafluoroethylene reaction kettle with the volume of 80mL, performing hydrothermal reaction for 24 hours at 180 ℃, and controlling the heating rate to be 2 ℃/min. And after the reaction is finished, washing the obtained product by deionized water and ethanol, and vacuum drying at 60 ℃ to obtain the foam nickel loaded with the molybdenum precursor.
(3) Load MoS 2
And (3) annealing the dried product in an argon atmosphere at 400 ℃ for 1h.
Through testing, the obtained sea urchin-shaped MoS 2 Foam nickel compositeThe specific capacitance of the composite capacitor electrode material is as high as 888.89F/g.
Example 2
Sea urchin-shaped MoS 2 The preparation method of the foam nickel composite capacitor electrode material comprises the following specific processes:
(1) Pretreatment of foam nickel
The nickel foam was sheared into L-shape 1cm x 1cm, ultrasonically cleaned with sodium hydroxide, hydrochloric acid, ethanol and deionized water, respectively, for 4 hours, and vacuum dried at 60 ℃ for 24h.
(2) Loaded molybdenum precursor
1mmol of sodium molybdate was dissolved in 60ml of deionized water to form an aqueous sodium molybdate solution; 15mmol of cetyltrimethylammonium bromide are dissolved in 20ml of n-butanol to which 1ml of hydrochloric acid is added; then dropwise adding the aqueous solution of sodium molybdate into n-butanol solution of hydrochloric acid dissolved with cetyltrimethylammonium bromide, and fully stirring for 2h; then 15mmol of thiourea is added and stirred vigorously for 2h; then adding the foam nickel pretreated in the step (1), and continuing to carry out ultrasonic treatment for 1h;
pouring the system into a polytetrafluoroethylene reaction kettle with the volume of 80mL, performing hydrothermal reaction for 24 hours at 180 ℃, and controlling the heating rate to be 2 ℃/min. And after the reaction is finished, washing the obtained product by deionized water and ethanol, and vacuum drying at 60 ℃ to obtain the foam nickel loaded with the molybdenum precursor.
(3) Load MoS 2
And (3) annealing the dried product in an argon atmosphere at 400 ℃ for 1h.
Through testing, the obtained sea urchin-shaped MoS 2 The specific capacitance of the electrode material of the foam nickel composite capacitor is as high as 884F/g.
Example 3
Sea urchin-shaped MoS 2 The preparation method of the foam nickel composite capacitor electrode material comprises the following specific processes:
(1) Pretreatment of foam nickel
The nickel foam was sheared into L-shape 1cm x 1cm, ultrasonically cleaned with sodium hydroxide, hydrochloric acid, ethanol and deionized water, respectively, for 4 hours, and vacuum dried at 60 ℃ for 24h.
(2) Loaded molybdenum precursor
1.5mmol of sodium molybdate was dissolved in 60ml of deionized water to form an aqueous sodium molybdate solution; 15mmol of cetyltrimethylammonium bromide are dissolved in 20ml of n-butanol to which 1ml of hydrochloric acid is added; then dropwise adding the aqueous solution of sodium molybdate into n-butanol solution of hydrochloric acid dissolved with cetyltrimethylammonium bromide, and fully stirring for 2h; then 15mmol of thiourea is added and stirred vigorously for 2h; then adding the foam nickel pretreated in the step (1), and continuing to carry out ultrasonic treatment for 1h;
pouring the system into a polytetrafluoroethylene reaction kettle with the volume of 80mL, performing hydrothermal reaction for 24 hours at 180 ℃, and controlling the heating rate to be 2 ℃/min. And after the reaction is finished, washing the obtained product by deionized water and ethanol, and vacuum drying at 60 ℃ to obtain the foam nickel loaded with the molybdenum precursor.
(3) Load MoS 2
And (3) annealing the dried product in an argon atmosphere at 400 ℃ for 1h.
Through testing, the obtained sea urchin-shaped MoS 2 The specific capacitance of the foam nickel composite capacitor electrode material is as high as 886.6F/g.
Example 4
Sea urchin-shaped MoS 2 The preparation method of the foam nickel composite capacitor electrode material comprises the following specific processes:
(1) Pretreatment of foam nickel
The nickel foam was sheared into L-shape 1cm x 1cm, ultrasonically cleaned with sodium hydroxide, hydrochloric acid, ethanol and deionized water, respectively, for 4 hours, and vacuum dried at 60 ℃ for 24h.
(2) Loaded molybdenum precursor
2mmol of sodium molybdate was dissolved in 60ml of deionized water to form an aqueous sodium molybdate solution; 15mmol of cetyltrimethylammonium bromide are dissolved in 20ml of n-butanol to which 1ml of hydrochloric acid is added; then dropwise adding the aqueous solution of sodium molybdate into n-butanol solution of hydrochloric acid dissolved with cetyltrimethylammonium bromide, and fully stirring for 2h; then 15mmol of thiourea is added and stirred vigorously for 2h; then adding the foam nickel pretreated in the step (1), and continuing to carry out ultrasonic treatment for 1h;
pouring the system into a polytetrafluoroethylene reaction kettle with the volume of 80mL, performing hydrothermal reaction for 24 hours at 180 ℃, and controlling the heating rate to be 2 ℃/min. And after the reaction is finished, washing the obtained product by deionized water and ethanol, and vacuum drying at 60 ℃ to obtain the foam nickel loaded with the molybdenum precursor.
(3) Load MoS 2
And (3) annealing the dried product in an argon atmosphere at 400 ℃ for 1h.
Through testing, the obtained sea urchin-shaped MoS 2 The specific capacitance of the foam nickel composite capacitor electrode material is as high as 882.5F/g.
Example 5
Sea urchin-shaped MoS 2 The preparation method of the foam nickel composite capacitor electrode material comprises the following specific processes:
(1) Pretreatment of foam nickel
The nickel foam was sheared into L-shape 1cm x 1cm, ultrasonically cleaned with sodium hydroxide, hydrochloric acid, ethanol and deionized water, respectively, for 4 hours, and vacuum dried at 60 ℃ for 24h.
(2) Loaded molybdenum precursor
2.5mmol of sodium molybdate was dissolved in 60ml of deionized water to form an aqueous sodium molybdate solution; 15mmol of cetyltrimethylammonium bromide are dissolved in 20ml of n-butanol to which 1ml of hydrochloric acid is added; then dropwise adding the aqueous solution of sodium molybdate into n-butanol solution of hydrochloric acid dissolved with cetyltrimethylammonium bromide, and fully stirring for 2h; then 15mmol of thiourea is added and stirred vigorously for 2h; then adding the foam nickel pretreated in the step (1), and continuing to carry out ultrasonic treatment for 1h;
pouring the system into a polytetrafluoroethylene reaction kettle with the volume of 80mL, performing hydrothermal reaction for 24 hours at 180 ℃, and controlling the heating rate to be 2 ℃/min. And after the reaction is finished, washing the obtained product by deionized water and ethanol, and vacuum drying at 60 ℃ to obtain the foam nickel loaded with the molybdenum precursor.
(3) Load MoS 2
And (3) annealing the dried product in an argon atmosphere at 400 ℃ for 1h.
Through testing, the obtained sea urchin-shaped MoS 2 The specific capacitance of the foam nickel composite capacitor electrode material is as high as 873.22F/g.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Comparative example
Blocky MoS 2 The preparation method of the foam nickel composite capacitor electrode material comprises the following specific processes:
(1) Pretreatment of foam nickel
The nickel foam was sheared into L-shape 1cm x 1cm, ultrasonically cleaned with sodium hydroxide, hydrochloric acid, ethanol and deionized water, respectively, for 4 hours, and vacuum dried at 60 ℃ for 24h.
(2) Loaded molybdenum precursor
2.5mmol of sodium molybdate was dissolved in 60ml of deionized water to form an aqueous sodium molybdate solution; 15mmol of ammonium fluoride was dissolved in 20ml of deionized water; then dropwise adding the aqueous solution of sodium molybdate into deionized water dissolved with ammonium fluoride, and fully stirring for 2 hours; then 15mmol of thiourea is added and stirred vigorously for 2h; then adding the foam nickel pretreated in the step (1), and continuing to carry out ultrasonic treatment for 1h;
pouring the system into a polytetrafluoroethylene reaction kettle with the volume of 80mL, performing hydrothermal reaction for 24 hours at 180 ℃, and controlling the heating rate to be 2 ℃/min. And after the reaction is finished, washing the obtained product with deionized water and ethanol, vacuum drying at 60 ℃, and annealing in argon for 1h at 400 ℃ to obtain the foam nickel loaded with the molybdenum precursor.
As can be seen from FIG. 3, SEM of comparative example was in the form of a block, and in examples 1 to 6, sea urchin-like MoS could be obtained after the treatment of step (2) 2 It can be seen that step (2) is to prepare sea urchin-like MoS 2 The essential operations. By comparison of the comparative example and the example, the surfactant used in comparative example 1 was ammonium fluoride, which forms a homogeneous solution with an aqueous sodium molybdate solution after being dissolved in water; examples surface usedThe active agent is cetyl trimethyl ammonium bromide dissolved in n-butanol and can form spherical water-oil two-phase suspension with sodium molybdate aqueous solution. Also as a surfactant, since comparative example 1 formed a homogeneous solution, ammonium fluoride was allowed to act throughout the homogeneous solution, forming a block shape; in the examples, a spherical water-oil two-phase suspension was formed, and cetyltrimethylammonium bromide dissolved in n-butanol acted on the interface between the water-oil two phases, and acted on the surface of the spherical water-oil two-phase to modify the surface, thereby forming a sea urchin shape.
While the foregoing description illustrates and describes the preferred embodiments of the present invention, as noted above, it is to be understood that the invention is not limited to the forms disclosed herein but is not to be construed as excluding other embodiments, and that various other combinations, modifications and environments are possible and may be made within the scope of the inventive concepts described herein, either by way of the foregoing teachings or by those of skill or knowledge of the relevant art. And that modifications and variations which do not depart from the spirit and scope of the invention are intended to be within the scope of the appended claims.
Claims (7)
1. Sea urchin-shaped MoS 2 The preparation method of the foam nickel composite capacitor electrode material is characterized by comprising the following steps of: the sea urchin-shaped MoS 2 The foam nickel composite capacitor electrode material is prepared from MoS 2 The preparation method of the composite material formed by uniformly distributing the composite material on the surface of the foam nickel comprises the following steps:
(1) Pretreating foam nickel;
(2) Dissolving sodium molybdate in deionized water, dissolving cetyl trimethyl ammonium bromide in a mixed solution of hydrochloric acid and n-butanol, then dropwise adding the aqueous solution dissolved with sodium molybdate into the mixed solution of hydrochloric acid and n-butanol dissolved with cetyl trimethyl ammonium bromide, and fully stirring; then thiourea is added and stirred vigorously; then adding the foam nickel pretreated in the step (1), and continuing to uniformly ultrasonically process;
(3) Carrying out hydrothermal reaction on the system in the step (2) in a polytetrafluoroethylene reaction kettle, wherein the reaction temperature is 180 ℃, and the reaction time is 24 hours;
(4) And (3) centrifuging the product obtained in the step (3) by using deionized water, washing, drying in vacuum, and annealing in argon for 1h at 400 ℃.
2. Sea urchin-like MoS according to claim 1 2 The preparation method of the foam nickel composite capacitor electrode material is characterized by comprising the following steps of: the pretreatment process of the foam nickel in the step (1) comprises the following steps: ultrasonic cleaning foam nickel with sodium hydroxide, hydrochloric acid, ethanol and deionized water for 4h, and vacuum drying at 60deg.C for 24h.
3. The method of manufacturing according to claim 1, characterized in that: the amount of sodium molybdate added in the step (2) is 0.5 to 2.5mmol.
4. The method of manufacturing according to claim 1, characterized in that: the addition amount of the cetyl trimethyl ammonium bromide is 15mmol.
5. The method of manufacturing according to claim 1, characterized in that: the addition amount of the hydrochloric acid is 1ml.
6. The method of manufacturing according to claim 1, characterized in that: the molar ratio of the cetyl trimethyl ammonium bromide to the thiourea is 1:1.
7. Sea urchin-like MoS prepared by the method of claim 1 2 The application of the foam nickel composite capacitor electrode material is characterized in that: the composite capacitor electrode material is used as a supercapacitor electrode material.
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