CN113643903A - NF @ Ni-Mo-S @ NiCo-LDH composite material and preparation method and application thereof - Google Patents

NF @ Ni-Mo-S @ NiCo-LDH composite material and preparation method and application thereof Download PDF

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CN113643903A
CN113643903A CN202110796686.XA CN202110796686A CN113643903A CN 113643903 A CN113643903 A CN 113643903A CN 202110796686 A CN202110796686 A CN 202110796686A CN 113643903 A CN113643903 A CN 113643903A
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electrodeposition
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foamed nickel
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CN113643903B (en
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蒋继波
黄星
孙冉
许文秀
李明晶
李雨露
魏影
陈晓敏
李婷婷
周少博
王云云
丛海山
宣宇娜
唐佳斌
韩生
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Shanghai Institute of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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    • H01G11/30—Electrodes characterised by their material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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Abstract

The invention relates to an NF @ Ni-Mo-S @ NiCo-LDH composite material and a preparation method and application thereof. The preparation method comprises the following steps: mixing ammonium molybdate tetrahydrate and Ni (NO)3)2·6H2Mixing O, thiourea and water, stirring and uniformly dispersing by ultrasound to completely dissolve the O, thiourea and water to obtain a mixed solution A; taking the mixed solution A as electrodeposition liquid, taking foamed nickel treated by acetone, ethanol and water in sequence as a deposition carrier, washing by adopting a one-step electrodeposition method, and drying to prepare NF @ Ni-Mo-S; mixing Ni (NO)3)2·6H2O、Co(NO3)3·6H2Adding O into water, fully stirring and uniformly dispersing to obtain a mixed solution B; the mixed solution B is taken as electrodeposition liquid, NF @ Ni-Mo-S is taken as a deposition carrier, and a one-step electrodeposition method is adopted for washing and dryingAnd drying to obtain the NF @ Ni-Mo-S @ NiCo-LDH composite material. Compared with the prior art, the NF @ Ni-Mo-S @ NiCo-LDH composite material prepared by the invention has a multi-layer flaky nano structure, can provide a large number of effective active sites, and thus has excellent electrochemical performance; in addition, the preparation method is two-step electrodeposition, is simple and easy to operate, is environment-friendly and is convenient for large-scale industrial production.

Description

NF @ Ni-Mo-S @ NiCo-LDH composite material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of electrochemistry and nano materials, and relates to an NF @ Ni-Mo-S @ NiCo-LDH composite material, and a preparation method and application thereof.
Background
At present, the human demand for green and sustainable energy continues to grow rapidly due to the energy scarcity and accelerated environmental distress consequences of natural fossil fuel combustion. Many renewable resources are currently being developed, but the intermittent nature of these resources limits their practical applications. Therefore, the development of economical, sustainable and high performance energy storage devices is crucial to ensure future sustainable energy. In energy storage devices, supercapacitors are receiving attention due to their greater specific power, fast charge and discharge capability, long life and environmental friendliness, which make supercapacitors applicable to many potential fields, such as hybrid vehicles, portable electronic devices, power grids, etc. Pseudocapacitors (PSCs) are a class of supercapacitors that exhibit rapid multi-electron reversible faradaic redox reactions at the electrode surface, resulting in higher specific capacities compared to Electrochemical Double Layer Capacitors (EDLCs).
Disclosure of Invention
The invention aims to provide an NF @ Ni-Mo-S @ NiCo-LDH composite material as well as a preparation method and application thereof.
The effect of enhancing the electrochemical performance is achieved by compounding Ni-Mo-S and NiCo-LDH, so that the problems of application limitation and the like of Ni-Mo-S and NiCo-LDH in the aspect of electrode materials of a supercapacitor are solved.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a preparation method of an NF @ Ni-Mo-S @ NiCo-LDH composite material, which comprises the following steps:
s1: mixing ammonium molybdate tetrahydrate and Ni (NO)3)2·6H2Mixing O, thiourea and water to completely dissolve the O, the thiourea and the water to obtain a mixed solution A;
s2: the mixed solution A is used as electrodeposition liquid, foamed nickel is used as a deposition carrier, and a one-step electrodeposition method is adopted to wash and dry the mixed solution A to prepare NF @ Ni-Mo-S;
s3: mixing Ni (NO)3)2·6H2O、Co(NO3)3·6H2Adding O into water, fully stirring and uniformly dispersing to obtain a mixed solution B;
s4: and (2) taking the mixed solution B as an electrodeposition solution, taking NF @ Ni-Mo-S as a deposition carrier, washing and drying by adopting a one-step electrodeposition method to prepare the NF @ Ni-Mo-S @ NiCo-LDH composite material.
In one embodiment of the present invention, in step S1, the ammonium molybdate tetrahydrate, Ni (NO)3)2·6H2The molar weight ratio of O to thiourea is (0.1-0.3) mmol to 2mmol (6-8) mmol.
In one embodiment of the present invention, in step S1, the volume of water is 40-60 mL.
In one embodiment of the present invention, in step S1, the mixture is stirred and ultrasonically dispersed uniformly to completely dissolve, the stirring and ultrasonically dispersing temperature is room temperature, the ultrasonic time is 5-10min, and the clear mixed solution a is obtained after the ultrasonic dispersing.
In one embodiment of the present invention, in step S2, the nickel foam is prepared by sequentially treating acetone, ethanol, and water.
In one embodiment of the present invention, in step S2, the one-step electrodeposition process is performed at room temperature, the voltage range for electrodeposition is-1.2-0.2V, the scan rate is 10-20mV/S, and the scan period is 10-20.
In one embodiment of the present invention, in step S3, Ni (NO)3)2·6H2O、Co(NO3)3·6H2The molar charge ratio of O is 1mmol (2-4 mmol).
In one embodiment of the present invention, in step S3, the volume of water is 45-55 mL.
In one embodiment of the present invention, in step S4, the one-step electrodeposition process is performed at room temperature, the voltage range for electrodeposition is-1.2-0.2V, the scan rate is 5-10mV/S, and the scan period is 3-8.
In one embodiment of the present invention, the drying processes in steps S2 and S4 are vacuum drying, the drying temperature is 60-80 ℃, and the drying time is 12-24 h.
The invention also provides the NF @ Ni-Mo-S @ NiCo-LDH composite material obtained based on the preparation method.
The invention also provides an application of the NF @ Ni-Mo-S @ NiCo-LDH composite material obtained based on the preparation method in a super capacitor.
In one embodiment of the invention, the NF @ Ni-Mo-S @ NiCo-LDH composite material prepared by the method is applied to a working electrode of a supercapacitor in the following way: grinding the NF @ Ni-Mo-S @ NiCo-LDH composite material, uniformly mixing the material with carbon black and polytetrafluoroethylene, and then pressing the mixture on a foamed nickel sheet to obtain the working electrode.
In one embodiment of the invention, the mass ratio of the NF @ Ni-Mo-S @ NiCo-LDH composite material to the carbon black to the polytetrafluoroethylene is 8 (0.8-1.2) to (0.8-1.2).
Metal Sulfides (MSs) such as CuS, Co9S8、Ni3S2、FeS2、WS2And MoS2The metal sulfide serving as a substitute of metal oxide is considered as a novel pseudo-capacitance electrode material in SCs, and has high conductivity, excellent oxidation-reduction reversibility, low electronegativity and high catalytic activity, and the specific capacitance capacity, energy and power density are enhanced. Meanwhile, additional metal atoms Ni are doped to adjust the morphology of the required nano structure so as to obtain high electrochemical performance.
Layered Double Hydroxides (LDHs), due to their novel layered structure, superior capacitance, high redox activity and environmental friendliness, have become competitive materials for supercapacitor applications. Because of the synergistic effect of the two elements cobalt and nickel, different electrochemical active sites are provided through the several oxidation states of the elements, and NiCo-LDH has outstanding capacitance characteristics, the composite material of Ni-Mo-S is selected by the invention, so that the active sites of the composite material are fully utilized.
According to the invention, the effect of enhancing the electrochemical performance is achieved by compounding Ni-Mo-S and NiCo-LDH, and the problems of application limitation and the like of Ni-Mo-S and NiCo-LDH in the aspect of electrode materials of a supercapacitor are further solved.
Compared with the prior art, the invention has the following advantages:
1. the NF @ Ni-Mo-S @ NiCo-LDH composite material prepared by the invention has a unique multilayer flaky nano structure, MoS2The doped Ni obviously increases the electric active sites and makes full use of the sulfurationThe sulfur vacancy in the matter and the shortening of the ion diffusion length can effectively make up the defect of low conductivity of the NiCo-LDH, and the NiCo-LDH is compounded with the sulfur vacancy and the ion diffusion length, so that the high specific capacitance of the NiCo-LDH is fully utilized.
2. The NF @ Ni-Mo-S @ NiCo-LDH composite material prepared by the invention is used as a working electrode in a super capacitor, and a cyclic voltammetry curve chart of the composite material has an obvious redox peak pair and good stability; meanwhile, the constant current charging and discharging curve diagram shows that the specific capacitance can reach 2425F/g at least, and an alternating current impedance spectrogram can prove that the conductivity is good and the internal resistance is low.
3. The preparation method has the advantages of low cost of raw materials, no pollution, no toxicity of solvents generated in the preparation process, and realization of large-scale industrial popularization.
Drawings
FIG. 1 is a cyclic voltammogram at different sweep rates for the product samples obtained in example 1.
Figure 2 is a graph of GCD at different current densities for samples of the product obtained in example 1.
FIG. 3 is an EIS plot of a sample of the product obtained in example 1.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
The raw materials used in the examples of the present invention are commercially available unless otherwise specified.
Example 1:
an NF @ Ni-Mo-S @ NiCo-LDH composite material and a preparation method and application thereof comprise the following steps:
in the first step, 0.1mmol ammonium molybdate tetrahydrate, 2mmol Ni (NO)3)2·6H2Mixing O, 8mmol of thiourea and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the thiourea to obtain a mixed solution A;
and secondly, placing the mixed solution A as an electrodeposition solution in an electrodeposition device, using 8mm multiplied by 1cm foamed nickel which is treated by acetone, ethanol and water for 3 times in sequence as a working electrode, using a platinum wire as a counter electrode, using Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 10mV/s, and the scanning period is 10. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to prepare NF @ Ni-Mo-S;
thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2Adding O into 50mL of water, and fully stirring and uniformly dispersing to obtain a mixed solution B;
and fourthly, taking the mixed solution B as an electrodeposition solution, placing the mixed solution B in an electrodeposition device, taking NF @ Ni-Mo-S as a working electrode, a platinum wire as a counter electrode and Ag/AgCl as a reference electrode, and maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 5mV/S, and the scanning period is 3. And (3) taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, then putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain the NF @ Ni-Mo-S @ NiCo-LDH. The foamed nickel loaded composite material is used as a working electrode, namely a Ni-Mo-S @ NiCo-LDH working electrode (NMS @ NC-1).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: the foam nickel sheet of NMS @ NC-1 is used as a working electrode, an Ag/AgCl electrode is used as a reference electrode, a Pt electrode is used as a counter electrode, and 2mol/L KOH is used as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 3105.9F/g in 2mol/L KOH solution and at a current density of 1A/g.
FIG. 1 is a CV diagram of the prepared NF @ Ni-Mo-S @ NiCo-LDH composite material at different sweep rates, wherein the sweep rates are respectively 5, 10, 15, 20, 30, 40, 50, 80 and 100 mV/S. As can be seen from the figure, at a voltage range of-0.1 to 0.7V, there are a pair of symmetrical redox peaks, and as the sweep rate increases, the oxidation peak and the reduction peak move to the right and left, respectively. The phenomenon shows that the prepared NF @ Ni-Mo-S @ NiCo-LDH composite material has good reversibility and stability.
FIG. 2 is a GCD curve of the prepared NF @ Ni-Mo-S @ NiCo-LDH composite material at current densities of 1, 2, 5, 10 and 20A/g.
FIG. 3 is an EIS diagram of the prepared NF @ Ni-Mo-S @ NiCo-LDH composite material at 100000Hz and 0.01 Hz.
Example 2:
an NF @ Ni-Mo-S @ NiCo-LDH composite material and a preparation method and application thereof comprise the following steps:
in the first step, 0.2mmol ammonium molybdate tetrahydrate, 2mmol Ni (NO)3)2·6H2Mixing O, 8mmol of thiourea and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the thiourea to obtain a mixed solution A;
and secondly, placing the mixed solution A as an electrodeposition solution in an electrodeposition device, using 8mm multiplied by 1cm foamed nickel which is treated by acetone, ethanol and water for 3 times in sequence as a working electrode, using a platinum wire as a counter electrode, using Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 10mV/s, and the scanning period is 10. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to prepare NF @ Ni-Mo-S;
thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2Adding O into 50mL of water, and fully stirring and uniformly dispersing to obtain a mixed solution B;
and fourthly, taking the mixed solution B as an electrodeposition solution, placing the mixed solution B in an electrodeposition device, taking NF @ Ni-Mo-S as a working electrode, a platinum wire as a counter electrode and Ag/AgCl as a reference electrode, and maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 5mV/S, and the scanning period is 3. And (3) taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, then putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain the NF @ Ni-Mo-S @ NiCo-LDH. The foamed nickel loaded composite material is used as a working electrode, namely a Ni-Mo-S @ NiCo-LDH working electrode (NMS @ NC-2).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: and taking a foam nickel sheet of NMS @ NC-2 as a working electrode, an Ag/AgCl electrode as a reference electrode, a Pt electrode as a counter electrode and 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 2975.3F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 3:
an NF @ Ni-Mo-S @ NiCo-LDH composite material and a preparation method and application thereof comprise the following steps:
in the first step, 0.3mmol ammonium molybdate tetrahydrate, 2mmol Ni (NO)3)2·6H2Mixing O, 8mmol of thiourea and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the thiourea to obtain a mixed solution A;
and secondly, placing the mixed solution A as an electrodeposition solution in an electrodeposition device, using 8mm multiplied by 1cm foamed nickel which is treated by acetone, ethanol and water for 3 times in sequence as a working electrode, using a platinum wire as a counter electrode, using Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 10mV/s, and the scanning period is 10. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to prepare NF @ Ni-Mo-S;
thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2Adding O into 50mL of water, and fully stirring and uniformly dispersing to obtain a mixed solution B;
and fourthly, taking the mixed solution B as an electrodeposition solution, placing the mixed solution B in an electrodeposition device, taking NF @ Ni-Mo-S as a working electrode, a platinum wire as a counter electrode and Ag/AgCl as a reference electrode, and maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 5mV/S, and the scanning period is 3. And (3) taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, then putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain the NF @ Ni-Mo-S @ NiCo-LDH. The foamed nickel loaded composite material is used as a working electrode, namely a Ni-Mo-S @ NiCo-LDH working electrode (NMS @ NC-3).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: and taking a foam nickel sheet of NMS @ NC-3 as a working electrode, an Ag/AgCl electrode as a reference electrode, a Pt electrode as a counter electrode and 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 2425F/g in 2mol/L KOH solution and at a current density of 2A/g.
Example 4:
an NF @ Ni-Mo-S @ NiCo-LDH composite material and a preparation method and application thereof comprise the following steps:
in the first step, 0.1mmol ammonium molybdate tetrahydrate, 2mmol Ni (NO)3)2·6H2Mixing O, 6mmol thiourea and 50mL water, stirring and uniformly dispersing by ultrasound to completely dissolve the thiourea to obtain a mixed solution A;
and secondly, placing the mixed solution A as an electrodeposition solution in an electrodeposition device, using 8mm multiplied by 1cm foamed nickel which is treated by acetone, ethanol and water for 3 times in sequence as a working electrode, using a platinum wire as a counter electrode, using Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 10mV/s, and the scanning period is 10. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to prepare NF @ Ni-Mo-S;
thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2Adding O into 50mL of water, and fully stirring and uniformly dispersing to obtain a mixed solution B;
and fourthly, taking the mixed solution B as an electrodeposition solution, placing the mixed solution B in an electrodeposition device, taking NF @ Ni-Mo-S as a working electrode, a platinum wire as a counter electrode and Ag/AgCl as a reference electrode, and maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 5mV/S, and the scanning period is 3. And (3) taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, then putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain the NF @ Ni-Mo-S @ NiCo-LDH. The foamed nickel loaded composite material is used as a working electrode, namely a Ni-Mo-S @ NiCo-LDH working electrode (NMS @ NC-4).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: and taking a foam nickel sheet of NMS @ NC-4 as a working electrode, an Ag/AgCl electrode as a reference electrode, a Pt electrode as a counter electrode and 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 2837.8F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 5:
an NF @ Ni-Mo-S @ NiCo-LDH composite material and a preparation method and application thereof comprise the following steps:
in the first step, 0.1mmol ammonium molybdate tetrahydrate, 2mmol Ni (NO)3)2·6H2Mixing O, 7mmol thiourea and 50mL water, stirring and uniformly dispersing by ultrasound to completely dissolve the thiourea to obtain a mixed solution A;
and secondly, placing the mixed solution A as an electrodeposition solution in an electrodeposition device, using 8mm multiplied by 1cm foamed nickel which is treated by acetone, ethanol and water for 3 times in sequence as a working electrode, using a platinum wire as a counter electrode, using Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 10mV/s, and the scanning period is 10. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to prepare NF @ Ni-Mo-S;
thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2Adding O into 50mL of water, fully stirring and uniformly dispersing to obtain a mixtureMixing the solution B;
and fourthly, taking the mixed solution B as an electrodeposition solution, placing the mixed solution B in an electrodeposition device, taking NF @ Ni-Mo-S as a working electrode, a platinum wire as a counter electrode and Ag/AgCl as a reference electrode, and maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 5mV/S, and the scanning period is 3. And (3) taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, then putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain the NF @ Ni-Mo-S @ NiCo-LDH. The foamed nickel loaded composite material is used as a working electrode, namely a Ni-Mo-S @ NiCo-LDH working electrode (NMS @ NC-5).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: and taking a foam nickel sheet of NMS @ NC-5 as a working electrode, an Ag/AgCl electrode as a reference electrode, a Pt electrode as a counter electrode and 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 2639.5F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 6:
an NF @ Ni-Mo-S @ NiCo-LDH composite material and a preparation method and application thereof comprise the following steps:
in the first step, 0.1mmol ammonium molybdate tetrahydrate, 2mmol Ni (NO)3)2·6H2Mixing O, 8mmol of thiourea and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the thiourea to obtain a mixed solution A;
and secondly, placing the mixed solution A as an electrodeposition solution in an electrodeposition device, using 8mm multiplied by 1cm foamed nickel which is treated by acetone, ethanol and water for 3 times in sequence as a working electrode, using a platinum wire as a counter electrode, using Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 10mV/s, and the scanning period is 20. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to prepare NF @ Ni-Mo-S;
thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2Adding O into 50mL of water, and fully stirring and uniformly dispersing to obtain a mixed solution B;
and fourthly, taking the mixed solution B as an electrodeposition solution, placing the mixed solution B in an electrodeposition device, taking NF @ Ni-Mo-S as a working electrode, a platinum wire as a counter electrode and Ag/AgCl as a reference electrode, and maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 5mV/S, and the scanning period is 3. And (3) taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, then putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain the NF @ Ni-Mo-S @ NiCo-LDH. The foamed nickel loaded composite material is used as a working electrode, namely a Ni-Mo-S @ NiCo-LDH working electrode (NMS @ NC-6).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: and taking a foam nickel sheet of NMS @ NC-6 as a working electrode, an Ag/AgCl electrode as a reference electrode, a Pt electrode as a counter electrode and 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 2706.9F/g in 2mol/L KOH solution and at a current density of 5A/g.
Example 7:
an NF @ Ni-Mo-S @ NiCo-LDH composite material and a preparation method and application thereof comprise the following steps:
in the first step, 0.1mmol ammonium molybdate tetrahydrate, 2mmol Ni (NO)3)2·6H2Mixing O, 8mmol of thiourea and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the thiourea to obtain a mixed solution A;
and secondly, placing the mixed solution A as an electrodeposition solution in an electrodeposition device, using 8mm multiplied by 1cm foamed nickel which is treated by acetone, ethanol and water for 3 times in sequence as a working electrode, using a platinum wire as a counter electrode, using Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 10mV/s, and the scanning period is 10. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to prepare NF @ Ni-Mo-S;
thirdly, 1mmol of Ni (NO)3)2·6H2O、4mmol Co(NO3)3·6H2Adding O into 50mL of water, and fully stirring and uniformly dispersing to obtain a mixed solution B;
and fourthly, taking the mixed solution B as an electrodeposition solution, placing the mixed solution B in an electrodeposition device, taking NF @ Ni-Mo-S as a working electrode, a platinum wire as a counter electrode and Ag/AgCl as a reference electrode, and maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 5mV/S, and the scanning period is 3. And (3) taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, then putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain the NF @ Ni-Mo-S @ NiCo-LDH. The foamed nickel loaded composite material is used as a working electrode, namely a Ni-Mo-S @ NiCo-LDH working electrode (NMS @ NC-7).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: and taking a foam nickel sheet of NMS @ NC-7 as a working electrode, an Ag/AgCl electrode as a reference electrode, a Pt electrode as a counter electrode and 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 2849.8F/g in 2mol/L KOH solution and at a current density of 10A/g.
Example 8:
an NF @ Ni-Mo-S @ NiCo-LDH composite material and a preparation method and application thereof comprise the following steps:
in the first step, 0.1mmol ammonium molybdate tetrahydrate, 2mmol Ni (NO)3)2·6H2Mixing O, 8mmol of thiourea and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the thiourea to obtain a mixed solution A;
and secondly, placing the mixed solution A as an electrodeposition solution in an electrodeposition device, using 8mm multiplied by 1cm foamed nickel which is treated by acetone, ethanol and water for 3 times in sequence as a working electrode, using a platinum wire as a counter electrode, using Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 10mV/s, and the scanning period is 10. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to prepare NF @ Ni-Mo-S;
thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2Adding O into 50mL of water, and fully stirring and uniformly dispersing to obtain a mixed solution B;
and fourthly, taking the mixed solution B as an electrodeposition solution, placing the mixed solution B in an electrodeposition device, taking NF @ Ni-Mo-S as a working electrode, a platinum wire as a counter electrode and Ag/AgCl as a reference electrode, and maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 5mV/S, and the scanning period is 5. And (3) taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, then putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain the NF @ Ni-Mo-S @ NiCo-LDH. The foamed nickel loaded composite material is used as a working electrode, namely a Ni-Mo-S @ NiCo-LDH working electrode (NMS @ NC-8).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: and taking a foam nickel sheet of NMS @ NC-8 as a working electrode, an Ag/AgCl electrode as a reference electrode, a Pt electrode as a counter electrode and 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 2631.8F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 9:
an NF @ Ni-Mo-S @ NiCo-LDH composite material and a preparation method and application thereof comprise the following steps:
in the first step, 0.1mmol ammonium molybdate tetrahydrate, 2mmol Ni (NO)3)2·6H2O, 8mmol of thiourea and 50mL of water are mixed, stirred and dispersed uniformly with the assistance of ultrasonicUniformly dissolving the mixture completely to obtain a mixed solution A;
and secondly, placing the mixed solution A as an electrodeposition solution in an electrodeposition device, using 8mm multiplied by 1cm foamed nickel which is treated by acetone, ethanol and water for 3 times in sequence as a working electrode, using a platinum wire as a counter electrode, using Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 10mV/s, and the scanning period is 10. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to prepare NF @ Ni-Mo-S;
thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2Adding O into 50mL of water, and fully stirring and uniformly dispersing to obtain a mixed solution B;
and fourthly, taking the mixed solution B as an electrodeposition solution, placing the mixed solution B in an electrodeposition device, taking NF @ Ni-Mo-S as a working electrode, a platinum wire as a counter electrode and Ag/AgCl as a reference electrode, and maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 10mV/S, and the scanning period is 3. And (3) taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, then putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain the NF @ Ni-Mo-S @ NiCo-LDH. The foamed nickel loaded composite material is used as a working electrode, namely a Ni-Mo-S @ NiCo-LDH working electrode (NMS @ NC-9).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: and taking a foam nickel sheet of NMS @ NC-9 as a working electrode, an Ag/AgCl electrode as a reference electrode, a Pt electrode as a counter electrode and 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. The specific capacitance of the composite material reaches 2715.2F/g in 2mol/L KOH solution and at a current density of 2A/g.
Example 10:
an NF @ Ni-Mo-S @ NiCo-LDH composite material and a preparation method and application thereof comprise the following steps:
in the first step, 0.1mmol ammonium molybdate tetrahydrate, 2mmol Ni (NO)3)2·6H2Mixing O, 8mmol of thiourea and 50mL of water, stirring and uniformly dispersing by ultrasound to completely dissolve the thiourea to obtain a mixed solution A;
and secondly, placing the mixed solution A as an electrodeposition solution in an electrodeposition device, using 8mm multiplied by 1cm foamed nickel which is treated by acetone, ethanol and water for 3 times in sequence as a working electrode, using a platinum wire as a counter electrode, using Ag/AgCl as a reference electrode, maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 10mV/s, and the scanning period is 10. Taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to prepare NF @ Ni-Mo-S;
thirdly, 1mmol of Ni (NO)3)2·6H2O、2mmol Co(NO3)3·6H2Adding O into 50mL of water, and fully stirring and uniformly dispersing to obtain a mixed solution B;
and fourthly, taking the mixed solution B as an electrodeposition solution, placing the mixed solution B in an electrodeposition device, taking NF @ Ni-Mo-S as a working electrode, a platinum wire as a counter electrode and Ag/AgCl as a reference electrode, and maintaining the electrodeposition solution at room temperature, wherein the scanning voltage range is-1.2-0.2V, the scanning rate is 10mV/S, and the scanning period is 5. And (3) taking out the foamed nickel after the electrodeposition is finished, washing the foamed nickel for three times by deionized water, then putting the washed foamed nickel into a vacuum oven, and drying the foamed nickel for 12 hours at the temperature of 60 ℃ to obtain the NF @ Ni-Mo-S @ NiCo-LDH. The foamed nickel loaded composite material is used as a working electrode, namely a Ni-Mo-S @ NiCo-LDH working electrode (NMS @ NC-10).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system for electrochemical test: and taking a foam nickel sheet of NMS @ NC-10 as a working electrode, an Ag/AgCl electrode as a reference electrode, a Pt electrode as a counter electrode and 2mol/L KOH as an electrolyte solution. The specific capacitance and the cyclic stability of the composite material are detected, and cyclic voltammetry tests show that the composite material has excellent redox capability. Under the condition of 2mol/L KOH solution and the current density of 1A/g, the specific capacitance of the composite material reaches 2619F/g.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (10)

1. A preparation method of NF @ Ni-Mo-S @ NiCo-LDH composite material is characterized by comprising the following steps:
s1: mixing ammonium molybdate tetrahydrate and Ni (NO)3)2·6H2Mixing O, thiourea and water to completely dissolve the O, the thiourea and the water to obtain a mixed solution A;
s2: the mixed solution A is used as electrodeposition liquid, foamed nickel is used as a deposition carrier, and a one-step electrodeposition method is adopted to wash and dry the mixed solution A to prepare NF @ Ni-Mo-S;
s3: mixing Ni (NO)3)2·6H2O、Co(NO3)3·6H2Adding O into water, fully stirring and uniformly dispersing to obtain a mixed solution B;
s4: and (2) taking the mixed solution B as an electrodeposition solution, taking NF @ Ni-Mo-S as a deposition carrier, washing and drying by adopting a one-step electrodeposition method to prepare the NF @ Ni-Mo-S @ NiCo-LDH composite material.
2. The process of claim 1, wherein in step S1, ammonium molybdate tetrahydrate, Ni (NO), is added to said composite material3)2·6H2The molar weight ratio of O to thiourea is (0.1-0.3) mmol to 2mmol (6-8) mmol.
3. The preparation method of the NF @ Ni-Mo-S @ NiCo-LDH composite material as claimed in claim 1, wherein in step S1, the mixture is stirred and dispersed by ultrasound uniformly to be dissolved completely, the stirring and ultrasonic dispersion are assisted at room temperature for 5-10min, and a clear mixed solution A is obtained after ultrasonic dispersion.
4. The process of claim 1, wherein in step S3, Ni (NO) is added3)2·6H2O、Co(NO3)3·6H2The molar charge ratio of O is 1mmol (2-4 mmol).
5. The process of claim 1, wherein in step S2, the one-step electrodeposition is performed at room temperature, with the electrodeposition being performed at a voltage ranging from-1.2V to 0.2V, a scan rate of 10mV/S to 20mV/S, and a scan period of 10 to 20;
in step S4, the one-step electrodeposition process is performed at room temperature, the voltage range used for electrodeposition is-1.2-0.2V, the scanning rate is 5-10mV/S, and the scanning period is 3-8.
6. The preparation method of the NF @ Ni-Mo-S @ NiCo-LDH composite material as claimed in claim 1, wherein the drying processes in the steps S2 and S4 are vacuum drying, the drying temperature is 60-80 ℃, and the drying time is 12-24 h.
7. An NF @ Ni-Mo-S @ NiCo-LDH composite material, characterized in that the NF @ Ni-Mo-S @ NiCo-LDH composite material is obtained by the production method described in any one of claims 1 to 6.
8. The use of the NF @ Ni-Mo-S @ NiCo-LDH composite material of claim 7 in a supercapacitor.
9. The use of the NF @ Ni-Mo-S @ NiCo-LDH composite material of claim 8 in a supercapacitor, wherein the NF @ Ni-Mo-S @ NiCo-LDH composite material is ground, uniformly mixed with carbon black and polytetrafluoroethylene, and then pressed onto a foamed nickel sheet to obtain a supercapacitor working electrode.
10. The use of the NF @ Ni-Mo-S @ NiCo-LDH composite material of claim 9 in a supercapacitor, wherein the mass ratio of the NF @ Ni-Mo-S @ NiCo-LDH composite material to the carbon black to the polytetrafluoroethylene is 8 (0.8-1.2) to (0.8-1.2).
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