CN114334471B - CeO (CeO) 2 /CuCo 2 S 4 Nano-NF composite material and preparation method and application thereof - Google Patents
CeO (CeO) 2 /CuCo 2 S 4 Nano-NF composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a CeO 2 /CuCo 2 S 4 The @ NF composite material and the preparation method and application thereof, wherein the composite material is prepared by adopting the following preparation method: (1) Dispersing cerium source, ammonium fluoride and urea in deionized water, adding foam nickel, hydrothermal, washing and drying to obtain CeO 2 An @ NF material; (2) Dispersing a cobalt source, a copper source and a sulfur source in water to obtain a copper-cobalt-sulfur aqueous solution, and then taking the copper-cobalt-sulfur aqueous solution as an electrolyte to obtain CeO 2 The target product is obtained by respectively taking an @ NF material, an Ag/AgCl electrode and a platinum electrode as a working electrode, a reference electrode and a counter electrode, and performing electrodeposition, washing and drying. The composite material can be used as a working electrode for a super capacitor. Compared with the prior art, the composite material has higher specific capacitance, and the preparation method is simpler and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of super capacitors, and relates to CeO 2 /CuCo 2 S 4 An @ NF composite material, a preparation method and application thereof.
Background
Global energy crisis and its associated environmental problems have created an urgent need for clean, economical sustainable energy. Supercapacitors are widely studied as electrochemical energy storage devices with the most application prospects at present, and electrode materials of the supercapacitors are divided into electric double layer electrode materials and pseudo-capacitor electrode materials according to different electrochemical energy storage principles. Generally, the electric double layer electrode material has high conductivity, high charge and discharge speed, good electrochemical stability, but small capacitance. The pseudo-capacitor electrode material has the advantages of good capacitance performance, high energy density, low charge and discharge rate and poor stability. Therefore, the two materials are compounded, and the advantages of the two materials are combined, especially the nanometer materials are selected, and the synergistic effect of the nanometer materials is used as a current research hot spot.
There are a series of problems in production and application based on supercapacitors. Firstly, the preparation process of the composite electrode material is complex; second, the composite material is single in type, and the micro-nano structure is unfavorable for metal ion embedding, so that the capacitance performance is affected.
CeO 2 In conventional supercapacitor applications, the energy density is low and there is no relatively regular topography.
Disclosure of Invention
The invention aims to provide CeO 2 /CuCo 2 S 4 @NF composite material, preparation method and application thereof, so as to overcome the defect of composite electrode material in the prior artComplex preparation process and CeO 2 Low energy density or random and integral morphology and the like.
The aim of the invention can be achieved by the following technical scheme:
one of the technical proposal of the invention provides a CeO 2 /CuCo 2 S 4 A method of preparing an @ NF composite comprising the steps of:
(1) Dispersing cerium source, ammonium fluoride and urea in deionized water, adding foam Nickel (NF), hydrothermal, washing and drying to obtain CeO 2 An @ NF material;
(2) Dispersing a cobalt source, a copper source and a sulfur source in water to obtain a copper-cobalt-sulfur aqueous solution, and then taking the copper-cobalt-sulfur aqueous solution as an electrolyte to obtain CeO 2 The target product is obtained by respectively taking an @ NF material, an Ag/AgCl electrode and a platinum electrode as a working electrode, a reference electrode and a counter electrode, and performing electrodeposition, washing and drying.
Further, in step (1), the cerium source is cerium nitrate hexahydrate.
Further, the molar ratio of the cerium nitrate hexahydrate, the ammonium fluoride and the urea is 1:1:4.
further, the size of the foam nickel is 1cm multiplied by 0.5mm, and the corresponding added amount of cerium nitrate hexahydrate and deionized water is (1-2) mmol and 20ml respectively.
Further, in the step (1), the hydrothermal temperature is 100 ℃, and the hydrothermal time is 6-8 hours.
Further, in the step (2), the cobalt source is cobalt nitrate hexahydrate, the copper source is copper nitrate hexahydrate, and the sulfur source is thiourea.
Still further, the molar ratio of cobalt nitrate hexahydrate, copper nitrate hexahydrate and thiourea was 2:1:4.
further, ceO 2 The size of the @ NF material is 1cm multiplied by 0.5mm, and the corresponding amounts of added cobalt nitrate hexahydrate and deionized water are (2-4) mmol and 15ml respectively.
Further, in the step (2), during the electrodeposition process, the temperature is 25 ℃, the voltage is-1.2-0.2V, the scanning rate is 5mV/s, and the scanning period is 15.
Further, the washing process is as follows:
the water and ethanol solution are used for washing alternately, and the total washing times are not less than 2 times and not more than 4 times.
Further, the drying is vacuum drying, the temperature of the vacuum drying is 60-90 ℃, and the drying time is 8-24 hours.
The second technical proposal of the invention provides a CeO 2 /CuCo 2 S 4 The @ NF composite material is prepared by the preparation method.
The third technical scheme of the invention provides application of the composite material, and the composite material can be used as a working electrode for a super capacitor.
The transition metal sulfide has excellent electrochemical activity, thermal stability and small electric resistance. Sulfur atoms are less electronegative than oxygen atoms, and thus the resulting sulfide has a more stable microstructure, which facilitates electron transport. In addition, there is a synergistic effect between the two metals and a large number of redox reactions occur, so that binary metal sulfides have better electrochemical properties than single metal sulfides.
The CeO prepared by the simple and quick method 2 /CuCo 2 S 4 The @ NF composite material is assembled to obtain the high-performance pseudo-capacitor all-solid super capacitor, and has high research significance and commercial value.
The preparation method disclosed by the invention is simple in preparation process and low in cost, can realize the structural design of the pseudo-capacitor electrode material on the nanometer level, fully exerts the advantages of the rare earth cerium material, and obtains the full-solid supercapacitor with excellent comprehensive performance and based on cerium oxide.
The invention controls the raw material ratio to enable CeO 2 /CuCo 2 S 4 the@NF composite material has good morphology, and the CeO 2 /CuCo 2 S 4 The electrochemical performance and the cycle performance of the @ NF composite material are very excellent, and the traditional CeO is overcome 2 The energy density of the super capacitor is low.
CeO of the invention 2 /CuCo 2 S 4 In the preparation process of the@NF composite material, urea is used as an alkaline reagent to provide an alkaline source for the reaction; the pH value of the solution plays a key role in the generation of mesoporous phases, and particularly has great influence on the pore channel shape and arrangement characteristics of mesoporous materials. According to the invention, ammonium fluoride is used as a surfactant, and under the alkaline condition of ammonium salt action, the cationic surfactant regulates and controls the appearance of the hexagonal cerium oxide nano-sheet on the surface of the foam nickel at a certain temperature. The temperature is set to 100 c because the temperature affects the structure and amount formed, and thus the specific surface area of the cerium oxide material. In the preparation process of the cerium oxide nano-sheet, the concentration of a cerium source, the pH value of a reaction solution, the reaction time and the reaction temperature all influence the synthesis of materials, so that ordered or disordered cerium oxide with high and low specific surface areas is formed.
At CeO 2 The nanometer sheet surface is formed into a layer of small nanometer sheet by means of electrodeposition method, and the main component of said nanometer sheet is CuCo 2 S 4 . The redox reaction equations mainly involved in the electrodeposition process are as follows:
compared with the prior art, the invention has the following advantages:
(1) The invention uses CeO 2 CuCo was used as the precursor 2 S 4 Modifying to make the final product CeO 2 /CuCo 2 S 4 the@NF composite material has a regular and uniform structure of electrode materials and a large specific surface area of sulfide, so that the specific capacitance of the material is fundamentally improved, and the composite material has application prospect in the field of energy storageThe range is wide;
(2) The preparation method of the invention is simple, has low cost and is suitable for large-scale production.
Drawings
FIG. 1 shows CeO obtained in example 1 2 /CuCo 2 S 4 A transmission electron microscope image of the @ NF composite material;
FIG. 2 shows CeO obtained in example 1 2 /CuCo 2 S 4 CV diagram of @ NF composite;
FIG. 3 shows CeO obtained in example 1 2 /CuCo 2 S 4 GCD diagram of @ NF composite;
FIG. 4 shows CeO obtained in example 1 2 /CuCo 2 S 4 EIS diagram of @ NF composite.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
In the following examples, unless otherwise specified, the raw materials or processing techniques are indicated as being conventional commercially available raw material products or conventional processing techniques in the art.
Example 1:
cerium nitrate hexahydrate 2.0mmol
Ammonium fluoride 2.0mmol
Urea 8.0mmol
Cobalt nitrate hexahydrate 4.0mmol
Copper nitrate hexahydrate 2.0mmol
Thiourea 8.0mmol
CeO 2 /CuCo 2 S 4 The @ NF composite material is prepared by a preparation method comprising the following steps:
2.0mmol of cerium nitrate hexahydrate, 2.0mmol of ammonium fluoride and 8.0mmol of urea were dissolved in 20ml of deionized water, and stirred for 30min to obtain a uniformly mixed pale white solution. 1 cm. Times.1 cm. Times.0.5 mm of nickel foam was immersed in the solution for 1h and then transferred to a hydrothermal kettle for 6h at 100deg.C. After the cooling to the room temperature, the mixture was cooled,washing with deionized water for one time, washing with absolute ethyl alcohol for three times, and drying in a vacuum drying oven at 60 ℃ for 8 hours to obtain CeO 2 @ NF material. CeO is added with 2 The @ NF material, saturated silver/silver chloride electrode and platinum wire electrode were used as working electrode, reference electrode, counter electrode, respectively. 4.0mmol of cobalt nitrate hexahydrate, 2.0mmol of copper nitrate hexahydrate, and 8.0mmol of thiourea were dissolved in deionized water (15 ml) as an electrolyte. CuCo 2 S 4 Depositing on cerium oxide nano-sheet by electrochemical codeposition method, then washing three times with deionized water, and placing in vacuum drying oven at 60 deg.C for 8 hr to obtain CeO 2 /CuCo 2 S 4 @nf composite material. In the electrodeposition process, the temperature is 25 ℃, the voltage range is-1.2-0.2V, the scanning speed is 5mV/s, and the scanning period is 15.
The CeO obtained is then treated 2 /CuCo 2 S 4 The @ NF composite was used as a working electrode, and a counter electrode (platinum wire electrode) and a reference electrode (saturated silver/silver chloride electrode) were prepared. Preparing 2.0M potassium hydroxide solution as electrolyte, introducing nitrogen to drive air, cleaning the electrode surface of Ag/AgCl electrode with 2.0M potassium hydroxide solution, connecting the working electrode, ag/AgCl electrode and platinum electrode with electrochemical workstation, and measuring the CeO in alkaline solution 2 /CuCo 2 S 4 Electrochemical performance of NF composites. At a current density of 1 A.g -1 When the specific capacitance of the material is 2100 F.g -1 。
FIG. 1 is CeO 2 /CuCo 2 S 4 The transmission electron microscope image of the @ NF composite material can clearly see the surface of the template which takes the large nano-sheet cerium oxide, and a plurality of CuCo can be grown uniformly 2 S 4 A nano-sheet.
FIGS. 2-4 evaluate CeO 2 /CuCo 2 S 4 Electrochemical behavior of the @ NF composite in a three electrode configuration in 2M KOH electrolyte. FIG. 2 is a graph of between 5 and 50 mV.s -1 CeO at the scanning rate of (2) 2 /CuCo 2 S 4 CV diagram of the @ NF composite material under a potential window of-0.2-0.5V, obvious oxidation-reduction peaks exist in the diagram, which indicates CeO 2 /CuCo 2 S 4 The @ NF composite material was characterized asPseudocapacitive characteristics. When the scanning speed is gradually increased to 50 mV.s -1 When CeO 2 /CuCo 2 S 4 The shape of the CV curve of the @ NF composite can be maintained.
FIG. 3 shows the current density at different current densities (1-40 A.g -1 )CeO 2 /CuCo 2 S 4 GCD curve of the @ NF composite, in order to reduce the water splitting reaction during low current density measurements, the most suitable voltage window measured in GCD was between 0 and 0.3V. According to GCD curve, when the current density is 1 A.g -1 、2A·g -1 、5A·g -1 、10A·g -1 、20A·g -1 And 40 A.g -1 When the CeO is measured 2 /CuCo 2 S 4 The corresponding capacitance of the @ NF composite material is 2100 F.g respectively -1 、1701F·g -1 、1653F·g -1 、1597F·g -1 、1554F·g -1 、1489F·g -1 。
To further investigate CeO 2 /CuCo 2 S 4 The reason that the @ NF composite material has good electrochemical performance is that CeO is subjected to EIS 2 /CuCo 2 S 4 The electron and ion transfer properties of the @ NF composite were evaluated. FIG. 4 shows CeO 2 /CuCo 2 S 4 Nyquist plot (EIS curve) for NF composite, nyquist plot in electrode shows linear component in low frequency region and semicircle in high frequency region. As can be seen, ceO 2 /CuCo 2 S 4 The volume resistance of the @ NF composite material is in a high frequency region, indicating CeO 2 /CuCo 2 S 4 The charge transfer resistance (Rct) of the @ NF composite is small, only 0.25 Ω. Further shows that the porous nano-sheet structure shortens the diffusion distance of electrolyte ions and improves the conductivity.
Example 2:
cerium nitrate hexahydrate 1.0mmol
Ammonium fluoride 1.0mmol
Urea 4.0mmol
Cobalt nitrate hexahydrate 2.0mmol
Copper nitrate hexahydrate 1.0mmol
Thiourea 4.0mmol
CeO 2 /CuCo 2 S 4 The @ NF composite material is prepared by a preparation method comprising the following steps:
1.0mmol of cerium nitrate hexahydrate, 1.0mmol of ammonium fluoride and 4.0mmol of urea were dissolved in 20ml of deionized water, and stirred for 30min to obtain a uniformly mixed pale white solution. 1 cm. Times.1 cm. Times.0.5 mm of nickel foam was immersed in the solution for 1h and then transferred to a hydrothermal kettle for 6h at 100deg.C. After cooling to room temperature, washing with deionized water and then absolute ethyl alcohol for three times, and drying in a vacuum drying oven at 60 ℃ for 8 hours to obtain CeO 2 @ NF material. CeO is added with 2 The @ NF material, saturated silver/silver chloride electrode and platinum wire electrode were used as working electrode, reference electrode, counter electrode, respectively. 2.0mmol of cobalt nitrate hexahydrate, 1.0mmol of copper nitrate hexahydrate, and 4.0mmol of thiourea were dissolved in deionized water (15 ml) as an electrolyte. CuCo 2 S 4 Depositing on cerium oxide nano-sheet by electrochemical codeposition method, then washing three times with deionized water, and placing in vacuum drying oven at 60 deg.C for 8 hr to obtain CeO 2 /CuCo 2 S 4 @nf composite material. In the electrodeposition process, the temperature is 25 ℃, the voltage range is-1.2-0.2V, the scanning speed is 5mV/s, and the scanning period is 15.
The CeO obtained is then treated 2 /CuCo 2 S 4 The @ NF composite was used as a working electrode, and a counter electrode (platinum wire electrode) and a reference electrode (saturated silver/silver chloride electrode) were prepared. Preparing 2.0M potassium hydroxide solution as electrolyte, introducing nitrogen to drive air, cleaning the electrode surface of Ag/AgCl electrode with 2.0M potassium hydroxide solution, connecting the working electrode, ag/AgCl electrode and platinum electrode with electrochemical workstation, and measuring the CeO in alkaline solution 2 /CuCo 2 S 4 Electrochemical performance of NF composites. At a current density of 1 A.g -1 When the specific capacitance of the material is 830 F.g -1 . The cerium nitrate hexahydrate in the precursor solution is obviously reduced, so that the obtained CeO 2 /CuCo 2 S 4 The @ NF composite had a significant decrease in specific capacitance compared to example 1.
Example 3:
cerium nitrate hexahydrate 2.0mmol
Ammonium fluoride 2.0mmol
Urea 8.0mmol
Cobalt nitrate hexahydrate 2.0mmol
Copper nitrate hexahydrate 1.0mmol
Thiourea 4.0mmol
The composite material is prepared by a preparation method comprising the following steps:
2.0mmol of cerium nitrate hexahydrate, 2.0mmol of ammonium fluoride and 8.0mmol of urea were dissolved in 20ml of deionized water, and stirred for 30min to obtain a uniformly mixed pale white solution. 1 cm. Times.1 cm. Times.0.5 mm of nickel foam was immersed in the solution for 1h and then transferred to a hydrothermal kettle for 6h at 100deg.C. After cooling to room temperature, washing with deionized water and then absolute ethyl alcohol for three times, and drying in a vacuum drying oven at 60 ℃ for 8 hours to obtain CeO 2 @ NF material. CeO is added with 2 The @ NF material, saturated silver/silver chloride electrode and platinum wire electrode were used as working electrode, reference electrode, counter electrode, respectively. 2.0mmol of cobalt nitrate hexahydrate, 1.0mmol of copper nitrate hexahydrate, and 4.0mmol of thiourea were dissolved in deionized water (15 ml) as an electrolyte. CuCo 2 S 4 Depositing on cerium oxide nano-sheet by electrochemical codeposition method, then washing three times with deionized water, and placing in vacuum drying oven at 60 deg.C for 8 hr to obtain CeO 2 /CuCo 2 S 4 @nf composite material. In the electrodeposition process, the temperature is 25 ℃, the voltage range is-1.2-0.2V, the scanning speed is 5mV/s, and the scanning period is 15.
The CeO obtained is then treated 2 /CuCo 2 S 4 The @ NF composite was used as a working electrode, and a counter electrode (platinum wire electrode) and a reference electrode (saturated silver/silver chloride electrode) were prepared. Preparing 2.0M potassium hydroxide solution as electrolyte, introducing nitrogen to drive air, cleaning the electrode surface of Ag/AgCl electrode with 2.0M potassium hydroxide solution, connecting the working electrode, ag/AgCl electrode and platinum electrode with electrochemical workstation, and measuring the CeO in alkaline solution 2 /CuCo 2 S 4 Electrochemical performance of NF composites. At a current density of 1 A.g -1 When the specific capacitance of the material is 2100 F.g -1 。
Example 4:
most of the same as in example 1 except that 2.0mmol of cerium nitrate hexahydrate was changed to 1.5mmol of cerium nitrate hexahydrate in this example.
Example 5:
most of the same as in example 1 except that in this example, 4.0mmol of cobalt nitrate hexahydrate was changed to 3mmol of cobalt nitrate hexahydrate.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments 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-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. CeO (CeO) 2 /CuCo 2 S 4 The preparation method of the @ NF composite material is characterized by comprising the following steps:
(1) Dispersing cerium source, ammonium fluoride and urea in deionized water, adding foam nickel, hydrothermal, washing and drying to obtain CeO 2 An @ NF material;
(2) Dispersing a cobalt source, a copper source and a sulfur source in water to obtain a copper-cobalt-sulfur aqueous solution, and then taking the copper-cobalt-sulfur aqueous solution as an electrolyte to obtain CeO 2 The target product is obtained by respectively taking an @ NF material, an Ag/AgCl electrode and a platinum electrode as a working electrode, a reference electrode and a counter electrode, and performing electrodeposition, washing and drying.
2. A CeO according to claim 1 2 /CuCo 2 S 4 The preparation method of the @ NF composite material is characterized in that in the step (1), the cerium source is cerium nitrate hexahydrate.
3. A kind of CeO according to claim 2 2 /CuCo 2 S 4 The preparation method of the @ NF composite material is characterized in that the molar ratio of cerium nitrate hexahydrate, ammonium fluoride and urea is 1:1:4.
4. a CeO according to claim 3 2 /CuCo 2 S 4 The preparation method of the @ NF composite material is characterized in that the size of the foam nickel is 1cm multiplied by 0.5mm, and the corresponding added amounts of cerium nitrate hexahydrate and deionized water are (1-2) mmol and 20ml respectively.
5. A CeO according to claim 1 2 /CuCo 2 S 4 The preparation method of the @ NF composite material is characterized in that in the step (1), the hydrothermal temperature is 100 ℃, and the hydrothermal time is 6-8 hours.
6. A CeO according to claim 1 2 /CuCo 2 S 4 The preparation method of the@NF composite material is characterized in that in the step (2), the cobalt source is cobalt nitrate hexahydrate, the copper source is copper nitrate hexahydrate, and the sulfur source is thiourea.
7. A kind of CeO according to claim 6 2 /CuCo 2 S 4 The preparation method of the @ NF composite material is characterized in that the mole ratio of cobalt nitrate hexahydrate, copper nitrate hexahydrate and thiourea is 2:1:4, a step of;
CeO 2 the size of the @ NF material is 1cm multiplied by 0.5mm, and the corresponding amounts of added cobalt nitrate hexahydrate and deionized water are (2-4) mmol and 15ml respectively.
8. A CeO according to claim 1 2 /CuCo 2 S 4 The preparation method of the @ NF composite material is characterized in that in the step (2), the temperature is 25 ℃, the voltage is-1.2-0.2V, the scanning rate is 5mV/s, and the scanning period is 15.
9. CeO (CeO) 2 /CuCo 2 S 4 An NF composite material, characterized in that it is produced by the preparation method according to any one of claims 1 to 8.
10. A kind of CeO according to claim 9 2 /CuCo 2 S 4 Use of an NF composite material, characterized in that the composite material is used as a working electrode for a supercapacitor.
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| CN108597893A (en) * | 2018-05-28 | 2018-09-28 | 江苏大学 | A kind of preparation method based on the composite electrode material for super capacitor in nickel foam |
| CN109402660A (en) * | 2018-09-18 | 2019-03-01 | 天津大学 | Fabricated in situ transition metal oxide/Ni-based sulfide composite material preparation method |
| CN109806879A (en) * | 2019-02-28 | 2019-05-28 | 北京化工大学 | A kind of CeO2-NiCo2O4/ NF composite electro catalytic material and its preparation method and application |
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| CN103643265A (en) * | 2013-12-25 | 2014-03-19 | 昆明理工大学 | Electroplating liquid for electrically depositing Cu-W-Co alloy coating and method thereof |
| CN108597893A (en) * | 2018-05-28 | 2018-09-28 | 江苏大学 | A kind of preparation method based on the composite electrode material for super capacitor in nickel foam |
| CN109402660A (en) * | 2018-09-18 | 2019-03-01 | 天津大学 | Fabricated in situ transition metal oxide/Ni-based sulfide composite material preparation method |
| CN109806879A (en) * | 2019-02-28 | 2019-05-28 | 北京化工大学 | A kind of CeO2-NiCo2O4/ NF composite electro catalytic material and its preparation method and application |
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