CN113130905A - Ultra-small cobalt sulfide nanosheet/carbon cloth composite material and preparation method thereof - Google Patents

Ultra-small cobalt sulfide nanosheet/carbon cloth composite material and preparation method thereof Download PDF

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Publication number
CN113130905A
CN113130905A CN202110408426.0A CN202110408426A CN113130905A CN 113130905 A CN113130905 A CN 113130905A CN 202110408426 A CN202110408426 A CN 202110408426A CN 113130905 A CN113130905 A CN 113130905A
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carbon cloth
ultra
powder
composite material
cobalt sulfide
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Inventor
黄剑锋
何枢薇
李嘉胤
曹丽云
王瑜航
张金津
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581Chalcogenides or intercalation compounds thereof
    • H01M4/5815Sulfides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/054Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
    • H01M4/625Carbon or graphite
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M2004/021Physical characteristics, e.g. porosity, surface area
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M2004/026Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027Negative electrodes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention discloses a preparation method of an ultra-small cobalt sulfide nanosheet/carbon cloth composite material, which comprises the following steps of (1) (0.7-1.1) weighing analytically pure cobalt acetate, tetrahydrate and sulfur powder according to the mass ratio, adding the cobalt acetate, the tetrahydrate and the sulfur powder into an ethanol solution, and stirring to obtain a solution A with the cobalt acetate concentration of 0.15-0.2 mol/L; standing the solution A, performing suction filtration to collect powder, cleaning and drying to obtain powder A; cutting the carbon cloth into small pieces, completely soaking the small pieces in a concentrated nitric acid solution, reacting for 2-4h in an oven at 90 ℃, cooling and then cleaning to obtain the pretreated carbon cloth; step four, respectively placing the pretreated carbon cloth and the powder A at two ends of the magnetic field, placing the pretreated carbon cloth and the powder A into a tubular furnace together, calcining the mixture to 800 ℃ in the protection of argon atmosphere, keeping the temperature for 1 to 3 hours at the heating rate of 3 to 7 ℃/min, and taking out a sample after cooling to room temperature to obtain the ultra-small cobalt sulfide nanosheet/carbon cloth composite material; the invention effectively improves the electrochemical activity and rate capability of the cobalt sulfide electrode material.

Description

Ultra-small cobalt sulfide nanosheet/carbon cloth composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of electrochemistry, relates to a sodium ion battery cathode material and a preparation method thereof, and particularly relates to an ultra-small cobalt sulfide nanosheet/carbon cloth composite material and a preparation method thereof.
Technical Field
With the popularization of portable electronic products and the rapid development of electric automobiles, the requirements on energy storage technology are higher and higher. The carbon-based material is a host material widely used in secondary batteries, such as carbon nanotubes, porous carbon, graphene nanoribbons, carbon fibers, and the like. Cobalt sulfide belongs to transition metal sulfide, belongs to a conversion reaction type cathode material in a secondary battery, but has poor cycle performance due to large volume expansion, and causes electrode pulverization; slower kinetics lead to poorer rate performance. Carbon cloth is widely used as a substrate of a flexible electrode material due to its good mechanical strength, electrical conductivity and flexibility. In recent years, many researchers have used flexible electrode materials by growing active materials such as metal oxides, metal sulfides, etc. on carbon cloth. The flexible electrode material does not need to add a binder and a conductive agent in the preparation process, so that the preparation steps are reduced, and the quality and the cost of the electrode material are reduced. In addition, the carbon cloth can effectively relieve the volume change of the active material in the charging and discharging process, thereby improving the performance of the active material. Therefore, the research on the flexible electrode material taking the carbon cloth as the substrate has important significance for the development of flexible energy storage devices.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide an ultra-small cobalt sulfide nanosheet/carbon cloth composite material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of an ultra-small cobalt sulfide nanosheet/carbon cloth composite material comprises the following steps:
weighing analytically pure cobalt acetate, tetrahydrate and sulfur powder according to the mass ratio of 1 (0.7-1.1), adding the cobalt acetate, the tetrahydrate and the sulfur powder into an ethanol solution, and stirring to obtain a solution A with the cobalt acetate concentration of 0.15-0.2 mol/L;
standing the solution A, performing suction filtration to collect powder, cleaning and drying to obtain powder A;
cutting the carbon cloth into small pieces, completely soaking the small pieces in a concentrated nitric acid solution, reacting for 2-4h in an oven at 90 ℃, cooling and then cleaning to obtain the pretreated carbon cloth;
and step four, respectively placing the pretreated carbon cloth and the powder A at two ends of the magnetic field, placing the pretreated carbon cloth and the powder A into a tubular furnace together, calcining the mixture in the protection of argon atmosphere to 800 ℃, keeping the temperature at the rate of 3-7 ℃/min for 1-3h, and taking out a sample after cooling to room temperature to obtain the ultra-small cobalt sulfide nanosheet/carbon cloth composite material.
The invention also has the following technical characteristics:
preferably, the standing method in the second step is standing for 4-7 hours at normal temperature in a dark place.
Preferably, the cleaning method in the second step is to repeatedly and alternately clean the substrate with deionized water and absolute ethyl alcohol for 3-5 times.
Preferably, the drying method in the second step is drying for 5-10h at 70 ℃ in a vacuum drying oven.
Preferably, the carbon cloth is cut into small pieces with the size of 2cm by 3cm in the third step.
Preferably, the cleaning method in the third step is to repeatedly and alternately clean the substrate for 3 to 5 times by using deionized water and absolute ethyl alcohol.
The invention also provides the ultra-small cobalt sulfide nanosheet/carbon cloth composite material prepared by the preparation method of the ultra-small cobalt sulfide nanosheet/carbon cloth composite material.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the carbon cloth is added to be compounded with the cobalt sulfide, and a conductive network formed by carbon fibers in the conductive carbon cloth is beneficial to the diffusion of electrolyte and can improve the conductivity of the cobalt sulfide; meanwhile, the carbon cloth as a self-supporting body can avoid adding a conductive agent and a binder in the preparation process of the electrode, simplify the process flow, improve the capacity contribution of the cobalt sulfide, and further improve the electrochemical activity and the rate capability of the electrode material;
the cobalt sulfide particle size is in the nanometer size range, and the composite material can remarkably improve the integrity of a microstructure, is beneficial to ion transmission and electron transfer and improves the electrochemical performance of the composite material due to the advantage of a nanometer structure;
the raw materials used in the invention are common materials, are cheap and easy to obtain, have low cost, do not need post treatment, are environment-friendly, have simple process and easy operation, and can be suitable for large-scale production.
Drawings
FIG. 1 is an XRD diffractogram of the product obtained in example 1 of the present invention
FIG. 2 is an SEM topography of the product obtained in example 1 of the invention
FIG. 3 is a graph showing the cycle performance of the product obtained in example 1 of the present invention
Detailed Description
Example 1:
1) a certain amount of analytically pure cobalt acetate, tetrahydrate and sulfur powder are added into an ethanol solution together, and a clear solution A is obtained by stirring. The concentration of the cobalt acetate is 0.15mol/L, and the mass ratio of the cobalt acetate to the sulfur powder is 1: 0.7;
2) standing the clear solution A at normal temperature in a dark place for 4h, performing suction filtration, collecting powder, repeatedly and alternately cleaning with deionized water and absolute ethyl alcohol for 3-5 times, and drying in a vacuum drying oven at 70 ℃ for 5h to obtain powder A;
3) cutting the carbon cloth into 2cm by 3cm, completely soaking the carbon cloth in a concentrated nitric acid solution, reacting for 2 hours in an oven at 90 ℃, and repeatedly and alternately cleaning for 3-5 times by using deionized water and absolute ethyl alcohol after cooling to obtain pretreated carbon cloth;
4) placing the pretreated carbon cloth and the powder A at two ends of the magnetic field respectively, placing the pretreated carbon cloth and the powder A into a tubular furnace together, calcining the mixture to 700 ℃ under the protection of argon atmosphere, raising the temperature at a rate of 7 ℃/min, and preserving the heat for 1 h. And after the temperature is reduced to the room temperature, taking out the sample to obtain the ultra-small cobalt sulfide nanosheet/carbon cloth composite material.
Example 2:
1) a certain amount of analytically pure cobalt acetate, tetrahydrate and sulfur powder are added into an ethanol solution together, and a clear solution A is obtained by stirring. The concentration of the cobalt acetate is 0.18mol/L, and the mass ratio of the cobalt acetate to the sulfur powder is 1: 0.9;
2) standing the clear solution A at normal temperature in a dark place for 5h, performing suction filtration, collecting powder, repeatedly and alternately cleaning with deionized water and absolute ethyl alcohol for 3-5 times, and drying in a vacuum drying oven at 70 ℃ for 8h to obtain powder A;
3) cutting the carbon cloth into 2cm by 3cm, completely soaking the carbon cloth in a concentrated nitric acid solution, reacting for 3h in an oven at 90 ℃, and repeatedly and alternately cleaning for 3-5 times by using deionized water and absolute ethyl alcohol after cooling to obtain pretreated carbon cloth;
4) placing the pretreated carbon cloth and the powder A at two ends of the magnetic field respectively, placing the pretreated carbon cloth and the powder A into a tubular furnace together, calcining the mixture to 750 ℃ under the protection of argon atmosphere, raising the temperature at a rate of 5 ℃/min, and preserving the heat for 2 hours. And after the temperature is reduced to the room temperature, taking out the sample to obtain the ultra-small cobalt sulfide nanosheet/carbon cloth composite material.
Example 3:
1) a certain amount of analytically pure cobalt acetate, tetrahydrate and sulfur powder are added into an ethanol solution together, and a clear solution A is obtained by stirring. The concentration of the cobalt acetate is 0.2mol/L, and the mass ratio of the cobalt acetate to the sulfur powder is 1: 1.1;
2) standing the clear solution A at normal temperature in a dark place for 7h, performing suction filtration, collecting powder, repeatedly and alternately cleaning with deionized water and absolute ethyl alcohol for 3-5 times, and drying in a vacuum drying oven at 70 ℃ for 10h to obtain powder A;
3) cutting the carbon cloth into 2cm by 3cm, completely soaking the carbon cloth in a concentrated nitric acid solution, reacting for 4 hours in an oven at 90 ℃, and repeatedly and alternately cleaning for 3-5 times by using deionized water and absolute ethyl alcohol after cooling to obtain pretreated carbon cloth;
4) placing the pretreated carbon cloth and the powder A at two ends of the magnetic field respectively, placing the pretreated carbon cloth and the powder A into a tubular furnace together, calcining the mixture to 800 ℃ under the protection of argon atmosphere, heating at a rate of 3 ℃/min, and preserving the heat for 3 hours. And after the temperature is reduced to the room temperature, taking out the sample to obtain the ultra-small cobalt sulfide nanosheet/carbon cloth composite material.
FIG. 1 is an XRD of the product obtained in example 1, and it can be seen that the product phase is comparable to standard card PDF #03-0631Co9S8Correspondingly, the peak of the steamed bun is brought by the carbon cloth, and the successful preparation of the cobalt sulfide/carbon cloth composite material is proved.
FIG. 2 is an SEM image analysis of the product obtained in example 1, and it can be seen from the low-power graph a that the composite material has a uniform appearance and cobalt sulfide is uniformly distributed on the surface of the carbon cloth; from the high power graph b, it can be seen that the cobalt sulfide flakes are in the nanometer scale and are staggered with each other.
FIG. 3 is an electrochemical performance test analysis of the product obtained in example 1, the capacity of the cell was maintained at 650mAh/g for 60 cycles at a current density of 1A/g in the voltage range of 0.3-3V, and the slight performance decay was probably due to the activation process, and the overall cycle stability was good.

Claims (7)

1. A preparation method of an ultra-small cobalt sulfide nanosheet/carbon cloth composite material is characterized by comprising the following steps:
weighing analytically pure cobalt acetate, tetrahydrate and sulfur powder according to the mass ratio of 1 (0.7-1.1), adding the cobalt acetate, the tetrahydrate and the sulfur powder into an ethanol solution, and stirring to obtain a solution A with the cobalt acetate concentration of 0.15-0.2 mol/L;
standing the solution A, performing suction filtration to collect powder, cleaning and drying to obtain powder A;
cutting the carbon cloth into small pieces, completely soaking the small pieces in a concentrated nitric acid solution, reacting for 2-4h in an oven at 90 ℃, cooling and then cleaning to obtain the pretreated carbon cloth;
and step four, respectively placing the pretreated carbon cloth and the powder A at two ends of the magnetic field, placing the pretreated carbon cloth and the powder A into a tubular furnace together, calcining the mixture to 800 ℃ in the protection of argon atmosphere, keeping the temperature rising rate at 3-7 ℃/min, keeping the temperature for 1-3h in a sealed manner, and taking out a sample after the temperature is reduced to room temperature to obtain the ultra-small cobalt sulfide nanosheet/carbon cloth composite material.
2. The method for preparing an ultra-small cobalt sulfide nanosheet/carbon cloth composite material of claim 1, wherein the standing method in step two is standing at normal temperature in a dark place for 4-7 h.
3. The method for preparing ultra-small cobalt sulfide nanosheet/carbon cloth composite material of claim 2, wherein the cleaning in step two is repeated and alternate cleaning with deionized water and absolute ethanol for 3-5 times.
4. The method for preparing ultra-small cobalt sulfide nanosheet/carbon cloth composite material of claim 3, wherein the drying method in step two is drying at 70 ℃ for 5-10h in a vacuum drying oven.
5. A method for preparing ultra-small cobalt sulfide nanosheet/carbon cloth composite material as recited in claim 1 in which the carbon cloth is cut into pieces of 2cm by 3cm in size in step three.
6. The method for preparing ultra-small cobalt sulfide nanosheet/carbon cloth composite material of claim 5, wherein the cleaning in step three is repeated and alternate cleaning with deionized water and absolute ethyl alcohol for 3-5 times.
7. An ultra-small cobalt sulfide nanosheet/carbon cloth composite prepared using the method of preparing an ultra-small cobalt sulfide nanosheet/carbon cloth composite of claims 1-6.
CN202110408426.0A 2021-04-16 2021-04-16 Ultra-small cobalt sulfide nanosheet/carbon cloth composite material and preparation method thereof Pending CN113130905A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN114703505A (en) * 2022-04-04 2022-07-05 昆明理工大学 Preparation method of metal atom electrocatalyst with stable carbon atom coordination

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114703505A (en) * 2022-04-04 2022-07-05 昆明理工大学 Preparation method of metal atom electrocatalyst with stable carbon atom coordination
CN114703505B (en) * 2022-04-04 2023-11-28 昆明理工大学 Preparation method of metal atom electrocatalyst with stable carbon atom coordination

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