CN110136975B - Preparation method and application of amorphous cobalt tetrathiomolybdate/nickel selenide nanosheet array composite material - Google Patents

Preparation method and application of amorphous cobalt tetrathiomolybdate/nickel selenide nanosheet array composite material Download PDF

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CN110136975B
CN110136975B CN201910394958.6A CN201910394958A CN110136975B CN 110136975 B CN110136975 B CN 110136975B CN 201910394958 A CN201910394958 A CN 201910394958A CN 110136975 B CN110136975 B CN 110136975B
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amorphous
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nise
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composite material
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CN110136975A (en
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范乐庆
顾芸
吴季怀
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Huaqiao University
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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
    • 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
    • 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
    • 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 amorphous CoMoS4The preparation method of the NiSe nanosheet array composite material comprises the following steps: (1) under the hydrothermal condition, cobalt nitrate hexahydrate and sodium molybdate heptahydrate react to grow CoMoO on foamed nickel4A nanosheet array; (2) mixing sodium sulfide with CoMoO4Hydrothermal reaction is carried out on the nanosheet array to form amorphous CoMoS4A nanosheet array; (3) under hydrothermal conditions, nickel chloride hexahydrate, selenium dioxide and urea react to form amorphous NiSe and deposit on amorphous CoMoS4The amorphous CoMoS is finally obtained on the surface of the nano-sheet array4The NiSe nano sheet array composite material. The preparation method is simple and low in cost, and the prepared amorphous CoMoS4The NiSe nanosheet array composite material has high specific capacitance and good cycling stability, can be applied to a supercapacitor electrode material, and has a good application prospect.

Description

Preparation method and application of amorphous cobalt tetrathiomolybdate/nickel selenide nanosheet array composite material
Technical Field
The invention relates to the technical field of super capacitors, in particular to a preparation method of an amorphous cobalt tetrathiomolybdate/nickel selenide nanosheet array composite material and application of the composite material as a super capacitor electrode material.
Background
The super capacitor is composed of electrodes, electrolyte, a current collector and a diaphragm, and is a novel electrochemical energy storage device. Compared with a lithium ion battery, the lithium ion battery has lower energy density. But has its own advantages such as high power density, fast charge and discharge speed, and long cycle life, etc., and thus has become one of the current research hotspots.
Supercapacitors are classified into pseudocapacitors and electric double layer capacitors. The pseudocapacitor depends on the Faraday redox reaction on the surface of the electrode material to store energy, and the double-electric-layer capacitor depends on the adsorption charges on the surface of the electrode material to store energy. The energy storage mechanism of the pseudo capacitor is different from that of the double electric layer capacitor, so that the energy density of the pseudo capacitor is far higher than that of the double electric layer capacitor, but the difference is larger compared with the lithium ion battery. Common pseudocapacitive materials include transition metal oxides, transition metal hydroxides, and conductive polymers, as well as transition metal sulfides that have been newly developed in recent years, and the like. At present, most of pseudocapacitance materials are crystalline materials, but the crystalline materials are not favorable for rapid ion diffusion due to the anisotropic characteristics of the crystalline materials, and a high specific capacitance is difficult to obtain, so that a super capacitor with high energy density is difficult to form. In addition, a binder is usually added in the preparation of the supercapacitor electrode, and the binder plays a role in binding an electrode material and a current collector; however, the binder will block the pores of the electrode material to some extent, and will reduce the energy storage capacity of the super capacitor.
Disclosure of Invention
The invention aims to provide amorphous cobalt tetrathiomolybdate/nickel selenide (namely CoMoS)4Preparation method of/NiSe) nanosheet array composite material is simple and low in cost, and prepared amorphous CoMoS4The NiSe nanosheet array composite material has high specific capacitance and good cycling stability, can be applied to a supercapacitor electrode material, and has a good application prospect.
In order to achieve the above purpose, the solution of the invention is:
amorphous CoMoS4The preparation method of the NiSe nanosheet array composite material comprises the step of preparing CoMoO4Preparation of nanosheet array, amorphous CoMoS4Preparation of nanosheet array and amorphous CoMoS4Preparing the NiSe nanosheet array composite material;
the CoMoO4Firstly, immersing cleaned foamed nickel into a mixed aqueous solution of cobalt nitrate hexahydrate and sodium molybdate heptahydrate at room temperature, sealing and heating to 80-180 ℃ for hydrothermal reaction, preserving heat for 4-10 h, and cooling to room temperature to obtain a reaction product A; then the reaction product A is cleaned and dried to obtain the CoMoO growing on the foamed nickel4A nanosheet array;
the amorphous CoMoS4The preparation method of the nano-sheet array is that the C grows at room temperatureoMoO4Placing foamed nickel of a nanosheet array in a sodium sulfide solution, sealing and heating to 60-120 ℃ for hydrothermal reaction, keeping the temperature for 4-10 h, cooling to room temperature to obtain a reaction product B, cleaning and drying the reaction product B to obtain amorphous CoMoS growing on the foamed nickel4A nanosheet array;
the amorphous CoMoS4The preparation method of the/NiSe nanosheet array composite material comprises the following step of growing the amorphous CoMoS at room temperature4Placing the foamed nickel of the nanosheet array in a mixed aqueous solution of nickel chloride hexahydrate, selenium dioxide and urea, sealing and heating to 100-200 ℃ for hydrothermal reaction, preserving heat for 5-20 hours, and then cooling to room temperature to obtain a reaction product C;
finally, cleaning and drying the reaction product C to obtain the amorphous CoMoS4The NiSe nano sheet array composite material.
In the mixed aqueous solution of cobalt nitrate hexahydrate and sodium molybdate heptahydrate, the molar ratio of cobalt nitrate hexahydrate to sodium molybdate heptahydrate is 1: 0.5-2, wherein the dosage ratio of the cobalt nitrate hexahydrate to the deionized water is 1 mmol: 10-15 mL.
In the sodium sulfide solution, the dosage ratio of sodium sulfide to deionized water is 1 mmol: 25-35 mL.
In the mixed aqueous solution of nickel chloride hexahydrate, selenium dioxide and urea, the molar ratio of nickel chloride hexahydrate, selenium dioxide and urea is 1: 1-4: 5-20, and the dosage ratio of nickel chloride hexahydrate and deionized water is 1 mmol: 50-70 mL.
The cleaning step is to clean for a plurality of times by sequentially adopting deionized water and ethanol.
The drying is vacuum drying.
The amorphous CoMoS4The application of the NiSe nanosheet array composite material as an electrode material of a super capacitor.
After the technical scheme is adopted, the amorphous CoMoS is4The preparation method of the NiSe nanosheet array composite material has the following advantages:
(1) the preparation method is simple, low in cost and good in repeatability;
(2) amorphous CoMoS4The NiSe nanosheet array composite material directly grows on the foamed nickel substrate, so that the use of a binder is effectively avoided;
(3) preparation of the resulting amorphous CoMoS4The NiSe nanosheet array composite material can form an open pore structure, and promotes the contact between electrolyte and electrodes;
(4) the amorphous CoMoS4CoMoS in NiSe nanosheet array composite material4And NiSe are both amorphous structures, can provide rich channels for ion diffusion, and thus have high specific capacitance and high cycling stability.
Drawings
FIG. 1 shows the CoMoO obtained in example 1 of the present invention4Nanosheet array, amorphous CoMoS4Nanosheet array and CoMoS4An X-ray diffraction pattern of the NiSe nanosheet array composite material;
FIG. 2 shows the amorphous CoMoS obtained in example 1 of the present invention4Nanosheet array and amorphous CoMoS4A selected area electron diffraction pattern of the NiSe nanosheet array composite material;
FIG. 3 shows the amorphous CoMoS obtained in example 1 of the present invention4An energy spectrum of the NiSe nanosheet array composite material;
FIG. 4 shows the amorphous CoMoS obtained in example 1 of the present invention4A photoelectron energy spectrum of the NiSe nanosheet array composite material;
FIG. 5 shows the CoMoO obtained in example 1 of the present invention4Nanosheet array, amorphous CoMoS4Nanosheet array and amorphous CoMoS4A scanning electron microscope image of the NiSe nanosheet array composite material;
FIG. 6 shows the amorphous CoMoS obtained in example 1 of the present invention4Nanosheet array and amorphous CoMoS4A specific capacitance relation diagram of the NiSe nanosheet array composite material under different current densities;
FIG. 7 shows CoMoS in example 1 of the present invention4The energy density-power density relation graph of the/NiSe// AC asymmetric super capacitor;
FIG. 8 is a schematic representation of the practice of the present inventionCoMoS in example 14Cycle stability profiles for/NiSe// AC asymmetric supercapacitors.
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
Example 1
Preparation of composite material
Amorphous CoMoS4The preparation method of the NiSe nanosheet array composite material comprises the following steps:
step 1, adding 5mmol of cobalt nitrate hexahydrate, 2.5mmol of sodium molybdate heptahydrate and 50mL of deionized water into a 100mL high-pressure kettle at room temperature, and stirring for dissolving to obtain a mixed aqueous solution A;
step 2, immersing the cleaned foamed nickel into the mixed aqueous solution A, sealing and heating the high-pressure kettle to 80 ℃ for hydrothermal reaction, preserving heat for 10 hours, and cooling to room temperature to obtain a reaction product A;
step 3, washing the reaction product A with deionized water and ethanol for several times in sequence, and drying for 12 hours in vacuum at the temperature of 60 ℃ to obtain the CoMoO growing on the foamed nickel4A nanosheet array;
step 4, adding 2mmol of sodium sulfide and 50mL of deionized water into a 100mL autoclave at room temperature, and stirring for dissolving to obtain a sodium sulfide solution;
step 5, growing the CoMoO obtained in the step 34Placing the foamed nickel of the nanosheet array into a sodium sulfide solution, sealing and heating the high-pressure kettle to 60 ℃ for hydrothermal reaction, preserving heat for 10 hours, and cooling to room temperature to obtain a reaction product B;
step 6, washing the reaction product B with deionized water and ethanol for several times in sequence, and drying the reaction product B for 12 hours in vacuum at the temperature of 60 ℃ to obtain amorphous CoMoS growing on the foamed nickel4A nanosheet array;
step 7, adding 1mmol of nickel chloride hexahydrate, 1mmol of selenium dioxide, 5mmol of urea and 50mL of deionized water into a 100mL high-pressure kettle at room temperature, and stirring for dissolving to obtain a mixed aqueous solution B of nickel chloride hexahydrate, selenium dioxide and urea;
step 8, the amorphous CoMoS obtained in the step 6 is grown4Placing the foamed nickel with the nanosheet array into the mixed aqueous solution B, sealing and heating the high-pressure kettle to 100 ℃ for hydrothermal reaction, keeping the temperature for 20 hours, reacting nickel chloride hexahydrate, selenium dioxide and urea to form amorphous NiSe under the hydrothermal condition, and depositing the amorphous NiSe on amorphous CoMoS4Cooling the surface of the nanosheet array to room temperature to obtain a reaction product C;
step 9, washing the reaction product C with deionized water and ethanol for several times in sequence, and drying for 12 hours in vacuum at 60 ℃ to obtain amorphous CoMoS4The NiSe nano sheet array composite material.
II, structural characterization
XRD measurements As shown in FIG. 1, CoMoO4The nanosheet array is crystalline, while the CoMoS4Nanosheet array and CoMoS4The X-ray diffraction pattern of the/NiSe nanosheet array composite material does not have diffraction peaks, which indicates that CoMoS4Nanosheet array and CoMoS4the/NiSe nano sheet array composite material has an amorphous structure.
FIG. 2 is an amorphous CoMoS4Nanosheet array and amorphous CoMoS4The selected area electron diffraction patterns of the NiSe nanosheet array composite material both present wide and fuzzy circular rings, and further illustrate that the two are amorphous structures.
By testing amorphous CoMoS4The energy spectrum (shown in figure 3) and the photoelectron spectrum (shown in figure 4) of the NiSe nanosheet array composite material confirm that the composite material is prepared from CoMoS4And NiSe.
Scanning electron microscopy results are shown in FIG. 5, which illustrates CoMoO growth on nickel foam4、CoMoS4And CoMoS4the/NiSe composite material presents a nano-sheet array and has an open pore structure.
Third, performance test
1. Directly in amorphous CoMoS4Nanosheet array and amorphous CoMoS4The NiSe nanosheet array composite material is used as a working electrode, the Hg/HgO electrode is used as a reference electrode, and 3mol/L KOH aqueous solution is used as electrolyte, so that three-electrode testing is performed. The test results are shown in FIG. 6Amorphous CoMoS at a current density of 1A/g4The specific capacitance of the NiSe nanosheet array composite material is up to 5757F/g, which exceeds that of amorphous CoMoS4Specific capacitance of the nanosheet array (2776F/g); amorphous CoMoS when the current density was raised to 10A/g4The specific capacitance of the NiSe nanosheet array composite material can still be maintained at a high specific capacitance (3120F/g), which indicates that the material has good rate capability.
2. In amorphous CoMoS4The NiSe nanosheet array composite material is used as a positive electrode, Activated Carbon (AC) is used as a negative electrode, and 3mol/L KOH aqueous solution is used as an electrolyte to assemble the CoMoS4And measuring the charge-discharge curves of the NiSe// AC asymmetric super capacitor under different current densities so as to obtain a relation curve graph of energy density-power density. As shown in FIG. 7, the energy density of the capacitor was as high as 69Wh/kg at a watt density of 875W/kg.
Under the condition that the current density is 5A/g, the asymmetric super capacitor is subjected to a charge-discharge cycle stability test, and the test result is shown in FIG. 8: after 10000 cycles, the capacitor can still maintain the specific capacitance of about 86 percent, which shows that the capacitor has good cycle stability, and the prepared amorphous CoMoS4The NiSe nanosheet array composite material can be applied as a supercapacitor material.
Example 2
Amorphous CoMoS4The preparation method of the NiSe nanosheet array composite material comprises the following steps:
step 1, adding 5mmol of cobalt nitrate hexahydrate, 10mmol of sodium molybdate heptahydrate and 75mL of deionized water into a 100mL high-pressure kettle at room temperature, and stirring for dissolving to obtain a mixed aqueous solution A;
step 2, immersing the cleaned foamed nickel into the mixed aqueous solution A, sealing and heating the high-pressure kettle to 180 ℃ for hydrothermal reaction, preserving heat for 4 hours, and cooling to room temperature to obtain a reaction product A;
step 3, washing the reaction product A with deionized water and ethanol for several times in sequence, and drying for 12 hours in vacuum at the temperature of 60 ℃ to obtain the CoMoO growing on the foamed nickel4A nanosheet array;
step 4, adding 2mmol of sodium sulfide and 70mL of deionized water into a 100mL autoclave at room temperature, and stirring for dissolving to obtain a sodium sulfide solution;
step 5, growing the CoMoO obtained in the step 34Placing the foamed nickel of the nanosheet array into a sodium sulfide solution, sealing and heating the high-pressure kettle to 120 ℃ for hydrothermal reaction, preserving heat for 4 hours, and cooling to room temperature to obtain a reaction product B;
step 6, washing the reaction product B with deionized water and ethanol for several times in sequence, and drying the reaction product B for 12 hours in vacuum at the temperature of 60 ℃ to obtain amorphous CoMoS growing on the foamed nickel4A nanosheet array;
step 7, adding 1mmol of nickel chloride hexahydrate, 4mmol of selenium dioxide, 20mmol of urea and 70mL of deionized water into a 100mL high-pressure kettle at room temperature, and stirring for dissolving to obtain a mixed aqueous solution B of nickel chloride hexahydrate, selenium dioxide and urea;
step 8, the amorphous CoMoS obtained in the step 6 is grown4Placing the foamed nickel with the nanosheet array into the mixed aqueous solution B, sealing and heating the high-pressure kettle to 200 ℃ for hydrothermal reaction, keeping the temperature for 5 hours, reacting nickel chloride hexahydrate, selenium dioxide and urea to form amorphous NiSe under the hydrothermal condition, and depositing the amorphous NiSe on amorphous CoMoS4Cooling the surface of the nanosheet array to room temperature to obtain a reaction product C;
step 9, washing the reaction product C with deionized water and ethanol for several times in sequence, and drying for 12 hours in vacuum at 60 ℃ to obtain amorphous CoMoS4The NiSe nano sheet array composite material.
The above embodiments and drawings are not intended to limit the form and style of the present invention, and any suitable changes or modifications thereof by those skilled in the art should be considered as not departing from the scope of the present invention.

Claims (7)

1. Amorphous CoMoS4The preparation method of the NiSe nanosheet array composite material is characterized by comprising the following steps of: including CoMoO4Preparation of nanosheet array, amorphous CoMoS4Preparation of nanosheet array and amorphous CoMoS4NiSe nano sheetPreparing an array composite material;
the CoMoO4Firstly, immersing cleaned foamed nickel into a mixed aqueous solution of cobalt nitrate hexahydrate and sodium molybdate heptahydrate at room temperature, sealing and heating to 80-180 ℃ for hydrothermal reaction, preserving heat for 4-10 h, and cooling to room temperature to obtain a reaction product A; then the reaction product A is cleaned and dried to obtain the CoMoO growing on the foamed nickel4A nanosheet array;
the amorphous CoMoS4The preparation method of the nano-sheet array comprises the steps of firstly growing the CoMoO at room temperature4Placing foamed nickel of a nanosheet array in a sodium sulfide solution, sealing and heating to 60-120 ℃ for hydrothermal reaction, keeping the temperature for 4-10 h, cooling to room temperature to obtain a reaction product B, cleaning and drying the reaction product B to obtain amorphous CoMoS growing on the foamed nickel4A nanosheet array;
the amorphous CoMoS4The preparation method of the/NiSe nanosheet array composite material comprises the following step of growing the amorphous CoMoS at room temperature4Placing the foamed nickel of the nanosheet array in a mixed aqueous solution of nickel chloride hexahydrate, selenium dioxide and urea, sealing and heating to 100-200 ℃ for hydrothermal reaction, preserving heat for 5-20 hours, and then cooling to room temperature to obtain a reaction product C;
finally, cleaning and drying the reaction product C to obtain the amorphous CoMoS4/NiSe nanosheet array composite, the amorphous CoMoS4CoMoS in NiSe nanosheet array composite material4And NiSe are both amorphous structures.
2. An amorphous CoMoS according to claim 14The preparation method of the NiSe nanosheet array composite material is characterized by comprising the following steps of: in the mixed aqueous solution of cobalt nitrate hexahydrate and sodium molybdate heptahydrate, the molar ratio of cobalt nitrate hexahydrate to sodium molybdate heptahydrate is 1: 0.5-2, wherein the dosage ratio of the cobalt nitrate hexahydrate to the deionized water is 1 mmol: 10-15 mL.
3. An amorphous CoMoS according to claim 14The preparation method of the NiSe nanosheet array composite material is characterized by comprising the following steps of: in the sodium sulfide solution, the dosage ratio of sodium sulfide to deionized water is 1 mmol: 25-35 mL.
4. An amorphous CoMoS according to claim 14The preparation method of the NiSe nanosheet array composite material is characterized by comprising the following steps of: in the mixed aqueous solution of nickel chloride hexahydrate, selenium dioxide and urea, the molar ratio of nickel chloride hexahydrate, selenium dioxide and urea is 1: 1-4: 5-20, and the dosage ratio of nickel chloride hexahydrate and deionized water is 1 mmol: 50-70 mL.
5. An amorphous CoMoS according to claim 14The preparation method of the NiSe nanosheet array composite material is characterized by comprising the following steps of: the cleaning step is to clean for a plurality of times by sequentially adopting deionized water and ethanol.
6. An amorphous CoMoS according to claim 14The preparation method of the NiSe nanosheet array composite material is characterized by comprising the following steps of: the drying is vacuum drying.
7. An amorphous CoMoS according to claim 14Amorphous CoMoS prepared by preparation method of NiSe nanosheet array composite material4The application of the NiSe nanosheet array composite material as an electrode material of a super capacitor.
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