阅读说明：本技术 一种双金属硫化物超级电容器电极材料的制备方法 (Preparation method of bimetal sulfide supercapacitor electrode material ) 是由 方林霞 兰梦迪 王茜茜 赵瑞杰 董梦尧 于 2019-10-27 设计创作，主要内容包括：本发明公开了一种双金属硫化物超级电容器电极材料的制备方法,属于新能源材料技术领域。所述超级电容器电极材料的制备是通过一步水热法合成,该材料呈均匀分散的片层结构,片层厚度较薄,纳米片彼此相互连接,形成多孔结构,这种独特的结构可以为电荷及离子的传输提供更多的活性位点,必将产生优异的电化学性能。本发明制备方法简单、生产成本低、技术环保,制得的电极材料具有较高的比电容和良好的电化学稳定性。(The invention discloses a preparation method of a bimetallic sulfide supercapacitor electrode material, and belongs to the technical field of new energy materials. The supercapacitor electrode material is prepared by a one-step hydrothermal method, the supercapacitor electrode material is in a uniformly dispersed lamellar structure, the thickness of the lamellar layer is thin, the nanosheets are mutually connected to form a porous structure, the unique structure can provide more active sites for transmission of charges and ions, and excellent electrochemical performance is certainly generated. The preparation method is simple, the production cost is low, the technology is environment-friendly, and the prepared electrode material has high specific capacitance and good electrochemical stability.)

1. A preparation method of a bimetal sulfide supercapacitor electrode material is characterized by comprising the following steps:

(1) dissolving zinc acetate dihydrate and cobalt acetate tetrahydrate in deionized water, and uniformly stirring to obtain a pink mixed solution;

(2) introducing thiourea into the pink mixed solution obtained in the step (1), and continuously stirring to obtain a dark purple solution;

(3) adding the purple solution obtained in the step (2) into a reaction kettle for hydrothermal reaction;

(4) after the reaction is finished, naturally cooling to room temperature, centrifugally washing by using distilled water and ethanol and drying to obtain Zn_0.76Co_0.24And (4) S nano material.

2. The preparation method of the electrode material of the bimetallic sulfide supercapacitor according to claim 1, characterized in that: the pink solution in the step (1) is as follows: 0.03-0.06g of zinc acetate dihydrate and 0.09-0.18g of cobalt acetate tetrahydrate are dissolved in 30-80mL of deionized water.

3. The preparation method of the electrode material of the bimetallic sulfide supercapacitor according to claim 1, characterized in that: the stirring time in the step (1) is 60-90 minutes.

4. The preparation method of the electrode material of the bimetallic sulfide supercapacitor according to claim 1, characterized in that: in the step (2), 0.08-0.18g of thiourea is used, and the stirring time is 30-60 minutes.

5. The preparation method of the electrode material of the bimetallic sulfide supercapacitor according to claim 1, characterized in that: the hydrothermal reaction conditions in the step (3) are as follows: placing the mixture in an oven to perform hydrothermal reaction at the temperature of 160-200 ℃ for 20-30 h.

6. The preparation method of the electrode material of the bimetallic sulfide supercapacitor according to claim 1, characterized in that: the washing conditions in the step (4) are as follows: washing with deionized water and ethanol for 3-5 times at 60-80 deg.C for 10-24 hr.

7. The electrode material prepared by the preparation method of the bimetallic sulfide supercapacitor electrode material according to claim 1, which is characterized in that: the material is in a uniformly dispersed lamellar structure, the thickness of the lamellar is thin, the nanosheets are mutually connected to form a porous structure, and the unique structure can provide more active sites for the transmission of charges and ions.

Technical Field

The invention relates to preparation of a capacitor electrode material, in particular to a bimetal sulfide super capacitor electrode material Zn_0.76Co_0.24And (5) a preparation method of S.

Background

With the scarcity of petroleum resources and the aggravation of environmental pollution, the search for new energy sources capable of sustainable development is urgent. On the other hand, the fast growing market for portable electronic devices and hybrid electric vehicles has driven research into high performance energy storage systems. Among the many energy storage applications, batteries, fuel cells and electrochemical supercapacitors are mature. The super capacitor draws wide attention of people due to the advantages of high power density, high charging and discharging speed, long cycle life, low cost, environmental friendliness and the like. In view of these advantages, the super capacitor has a wide application prospect in the fields of military affairs, traffic, new energy, electronics, instruments and the like, and has become one of the research hotspots in the field of new energy. However, the energy density of the super capacitor is low, and the problem is still to be solved urgently. Therefore, increasing the energy density without compromising its inherent advantages is the focus of further research. Since the performance of these memory devices depends to a large extent on the electrode materials used, the development of advanced electrode materials with high capacitance, environmental protection, and low cost is still of great significance and challenge.

Generally, the performance of a supercapacitor is affected by electrode materials, electrolyte and assembly processes, wherein the electrode materials are important factors affecting the performance of the electrodes. Currently, research on electrode materials mainly focuses on improving the electrochemical performance of existing materials and developing new high-performance electrode materials. The bimetal sulfide has the advantages of low price, rich reserves, environmental protection and the like, is widely applied to electrode materials of super capacitors, and particularly becomes a new hot point in the field of energy application as a ternary metal sulfide serving as a novel electrode material. Ternary metal sulfides have a richer redox reaction and a higher electron transport rate than single-component metal sulfides, and thus have led to extensive research in supercapacitors.

Disclosure of Invention

The invention provides the bimetallic sulfide supercapacitor electrode which has the advantages of simple preparation method, low production cost, environment-friendly technology, higher capacitance, excellent rate capability and good cycling stability of the prepared materialMaterial Zn_0.76Co_0.24And (5) a preparation method of S.

The purpose of the invention is realized as follows:

bimetal sulfide supercapacitor electrode material Zn_0.76Co_0.24The preparation method of S comprises the following steps:

(1) dissolving zinc acetate dihydrate and cobalt acetate tetrahydrate in deionized water, and uniformly stirring to obtain a pink mixed solution;

(2) introducing thiourea into the pink mixed solution obtained in the step (1), and continuously stirring to obtain a dark purple solution;

(3) adding the purple solution obtained in the step (2) into a reaction kettle for hydrothermal reaction;

(4) after the reaction is finished, naturally cooling to room temperature, centrifugally washing by using distilled water and ethanol and drying to obtain Zn_0.76Co_0.24And (4) S nano material.

The pink solution in the step (1) is as follows: 0.03-0.06g of zinc acetate dihydrate and 0.09-0.18g of cobalt acetate tetrahydrate are dissolved in 30-80mL of deionized water;

the stirring time in the step (1) is 60-90 minutes;

in the step (2), 0.08-0.18g of thiourea is used, and the stirring time is 30-60 minutes;

the hydrothermal reaction conditions in the step (3) are as follows: placing the mixture in an oven to perform hydrothermal reaction at the temperature of 160-200 ℃ for 20-30 h.

The washing conditions in the step (4) are as follows: washing with deionized water and ethanol for 3-5 times at 60-80 deg.C for 10-24 hr;

the material is in a uniformly dispersed lamellar structure, the thickness of the lamellar is thin, the nanosheets are mutually connected to form a porous structure, and the unique structure can provide more active sites for the transmission of charges and ions.

Has the positive and beneficial effects that: the preparation method is simple, the production cost is low, the technology is environment-friendly, the electrode material is prepared by a hydrothermal method, the microstructure of the electrode material is characterized, and the prepared Zn_0.76Co_0.24The S nano material has a uniformly dispersed lamellar structure, and the nano sheets are mutually connected to form a porous structure, so that the material has more active sites, and higher capacitance, excellent rate capability and good cycling stability are shown.

Drawings

FIG. 1 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24An X-ray diffraction pattern of the S electrode material;

FIG. 2 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24An X-ray electron energy spectrum of the S electrode material;

FIG. 3 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24Scanning electron micrographs of S electrode material at different magnifications;

FIG. 4 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24A cyclic voltammogram of the S electrode material in a three-electrode system at different scanning rates;

FIG. 5 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24A charge-discharge curve diagram of the S electrode material under different current densities in a three-electrode system;

FIG. 6 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24A capacitance multiplying power diagram of the S electrode material in a three-electrode system;

FIG. 7 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24An electrode cycle chart of the S electrode material in a three-electrode system;

FIG. 8 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24An electrode alternating current impedance diagram of the S electrode material in a three-electrode system;

FIG. 9 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24The sweep rate of the S electrode material and the activated carbon is 50mV S^-1A comparison graph of cyclic voltammograms over time;

FIG. 10 is a bimetallic vulcanizate prepared in example 1 of the present inventionThe substance Zn_0.76Co_0.24S electrode material and active carbon-composed asymmetric water system two-electrode Zn_0.76Co_0.24Cyclic voltammograms of S// AC at different voltages;

FIG. 11 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24S electrode material and active carbon-composed asymmetric water system two-electrode Zn_0.76Co_0.24Cyclic voltammograms of S// AC at different sweep rates;

FIG. 12 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24S electrode material and active carbon-composed asymmetric water system two-electrode Zn_0.76Co_0.24The constant current discharge curve chart of S// AC under different current densities;

FIG. 13 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24S electrode material and active carbon-composed asymmetric water system two-electrode Zn_0.76Co_0.24A capacitance magnification graph of S// AC;

FIG. 14 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24S electrode material and active carbon-composed asymmetric water system two-electrode Zn_0.76Co_0.24A cycle chart of S// AC;

FIG. 15 shows the bimetallic sulfide Zn prepared in example 1 of the present invention_0.76Co_0.24S electrode material and active carbon-composed asymmetric water system two-electrode Zn_0.76Co_0.24AC impedance plot of S// AC.

Detailed Description

The invention will be further described with reference to the following specific embodiments and the accompanying drawings: