CN110416509B - High-specific-capacity lithium ion battery negative electrode material and preparation method thereof - Google Patents

High-specific-capacity lithium ion battery negative electrode material and preparation method thereof Download PDF

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CN110416509B
CN110416509B CN201910646766.XA CN201910646766A CN110416509B CN 110416509 B CN110416509 B CN 110416509B CN 201910646766 A CN201910646766 A CN 201910646766A CN 110416509 B CN110416509 B CN 110416509B
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sea urchin
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lithium ion
ion battery
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王新
王加义
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Zhaoqing South China Normal University Optoelectronics Industry Research Institute
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    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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Abstract

The invention relates to a lithium ion battery cathode material with high specific capacity and a preparation method thereof. The cathode material of the lithium ion battery is a sea urchin-shaped carbon-coated cobalt oxide, a cobalt chloride precursor is adopted to prepare sea urchin-shaped cobaltosic oxide through hydrothermal synthesis, and carbon deposition is carried out through a vapor deposition method to prepare the sea urchin-shaped carbon-coated cobalt oxide composite cathode material of the lithium ion battery. The cobaltosic oxide is used as an active substance, and the carbon coating is used for providing conductivity for the whole electrode material, and the structural stability of the sea urchin-shaped cobaltosic oxide in the charging and discharging processes is improved. In addition, under the action of hydrogen in the vapor deposition process, the cobalt valence state of the sea urchin-shaped cobaltosic oxide can be changed, and the cobalt with the mixed valence state can provide extra conductivity for the electrode material.

Description

High-specific-capacity lithium ion battery negative electrode material and preparation method thereof
Technical Field
The invention relates to a high-specific-capacity lithium ion battery negative electrode material and a preparation method thereof, belonging to the field of material chemistry.
Background
The economy and scientific technology of the 21 st century are rapidly developed, but the main source of energy is fossil fuels such as petroleum, coal and natural gas which are limited on the earth. It is well known that gases derived from fossil fuel and biomass fuel emissions pollute the atmosphere, causing serious global problems. In the face of increasingly severe energy and environmental problems, the development of renewable clean energy has become an urgent problem to be solved. The new energy refers to unconventional energy developed and utilized on the basis of new technology, and comprises wind energy, solar radiation energy, ocean energy, geothermal energy, biomass energy, ammonia energy, nuclear energy and the like. The new energy resource has great potential, can be continuously utilized, and plays an important role in meeting the energy demand, improving the energy structure, reducing the environmental pollution, promoting the economic development and the like. However, the electric power generated by new energy sources such as wind energy and solar energy has instability and discontinuity, and is difficult to be directly applied to production and living. Therefore, an efficient energy storage and conversion device is established, so that unstable power is collected and can be smoothly released at a proper time, and the device has important significance for development and utilization of new energy.
Compared with other rechargeable batteries (such as lead-acid batteries and nickel-metal hydride batteries), the lithium ion battery has the obvious advantages of high specific capacity, long cycle life, high voltage platform, no memory effect, quick charge and discharge, high safety performance, low self-discharge rate, small environmental pollution, small volume, light weight and the like. At present, lithium ion batteries have been widely used in small digital devices such as mobile phones, cameras, and notebook computers, and are developing into large batteries for electric vehicles and wind and solar energy storage batteries. The demand of the energy storage battery puts higher requirements on the performance of the lithium ion battery, and as an important component of the lithium ion battery, positive and negative electrode materials are key factors determining the performance of the lithium ion battery. Therefore, research and development of high-performance and low-cost lithium ion battery electrode materials are becoming increasingly important.
Disclosure of Invention
The invention provides a lithium ion battery cathode material with high specific capacity and a preparation method thereof, aiming at the problems of small reversible capacity, poor cycle performance and the like of the current lithium ion battery cathode material. The lithium ion battery cathode material with high specific capacity is a sea urchin-shaped carbon-coated cobalt oxide, and is prepared by preparing sea urchin-shaped cobaltosic oxide firstly and then carrying out carbon deposition by a vapor deposition method.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a preparation method of a high-specific-capacity lithium ion battery negative electrode material is characterized in that the lithium ion battery negative electrode material is a sea urchin-shaped carbon-coated cobalt oxide, and the preparation process comprises the following steps:
(1) preparing sea urchin-shaped cobaltosic oxide:
dissolving cobalt chloride and urea in deionized water, magnetically stirring uniformly, placing the mixed solution in a reaction kettle for hydrothermal reaction, naturally cooling after the hydrothermal reaction is finished, washing the product with the deionized water and ethanol for three times, placing the product in an oven for drying at 60 ℃, and placing the dried product in a muffle furnace for calcining to obtain the sea urchin-shaped cobaltosic oxide.
(2) Preparing the urchin-shaped carbon-coated cobalt oxide:
and (2) placing the sea urchin-shaped cobaltosic oxide powder prepared in the step (1) in a tubular furnace, heating to 500-700 ℃ under the argon atmosphere, introducing a mixed gas of acetylene and hydrogen simultaneously after the temperature is constant, continuously introducing for 1-3 min, closing the hydrogen and the acetylene, and naturally cooling under the argon atmosphere to obtain the sea urchin-shaped carbon-coated cobalt oxide composite material.
Preferably, in the step (1), the usage ratio of cobalt chloride, urea and deionized water is as follows: (0.1-0.5) g: (1-5) g: (10-100) mL.
Preferably, in the step (1), the magnetic stirring time is 1-3 h.
Preferably, in the step (1), the temperature of the hydrothermal reaction is 100-150 ℃, and the time of the hydrothermal reaction is 12-24 hours.
Preferably, in the step (1), the calcining temperature is 200-400 ℃, and the calcining time is 6-12h
Preferably, in the step (2), the mass of the sea urchin-shaped cobaltosic oxide powder is 0.1-0.5 g, the hydrogen flow rate is 100-300 mL/min, and the acetylene flow rate is 10-50 mL/min.
Preferably, after the acetylene and hydrogen mixed gas is continuously introduced for 1-3 min in the step (2), the introduction of the acetylene is stopped firstly, and the introduction of the hydrogen is stopped after the introduction of the acetylene is stopped for 5-10 min.
Preferably, in the step (2), the temperature rise rate of the tube furnace is 0.5-1 ℃/min.
The invention has the following beneficial effects:
aiming at the problems of small reversible capacity, poor cycle performance and the like of the current lithium ion battery cathode material, the invention introduces sea urchin-shaped cobaltosic oxide as an active material and deposits a layer of carbon coating on the surface of the active material by a vapor deposition method. The carbon coating can provide conductivity for the whole electrode material, and improve the structural stability of the sea urchin-shaped cobaltosic oxide in the charging and discharging processes, so that the sea urchin-shaped cobaltosic oxide can not collapse in the current impact. In addition, under the action of hydrogen in the vapor deposition process, the hydrogen can react with oxygen in the cobaltosic oxide, so that the valence state of the cobalt is changed, and the cobalt with the mixed valence state can provide additional conductivity for the electrode material.
Drawings
The invention is further illustrated with reference to the following figures and examples:
FIG. 1 is a scanning electron micrograph of a urchin-shaped carbon-coated cobalt oxide obtained in example 1.
Fig. 2 is a discharge specific capacity cycle diagram of the cathode material of the urchin-shaped carbon-coated cobalt oxide lithium ion battery prepared in example 1.
Detailed Description
Example 1:
(1) preparing sea urchin-shaped cobaltosic oxide:
0.3g of cobalt chloride and 2g of urea are dissolved in 50mL of deionized water, the mixture is magnetically stirred for 2 hours, the mixture is uniformly stirred and then transferred to a 150mL reaction kettle, the reaction kettle is placed in a constant temperature furnace, the reaction kettle reacts for 18 hours at 120 ℃, then the reaction kettle is cooled along with the furnace, the mixture is washed three times by using the deionized water and ethanol, and the mixture is placed in an oven to be dried at 60 ℃. And after the reaction is finished, placing the sea urchin-shaped cobaltosic oxide in a muffle furnace, and calcining the sea urchin-shaped cobaltosic oxide at 300 ℃ for 8 hours to obtain the sea urchin-shaped cobaltosic oxide.
(2) Preparing the urchin-shaped carbon-coated cobalt oxide:
and (2) placing 0.2g of the sea urchin-shaped cobaltosic oxide powder prepared in the step (1) in a tubular furnace, heating to 600 ℃ at a heating rate of 1 ℃/min under argon atmosphere, introducing mixed gas of acetylene and hydrogen simultaneously after the temperature is constant, wherein the hydrogen flow rate is 200mL/min, the acetylene flow rate is 30mL/min, continuously introducing for 2min, firstly closing the acetylene after the completion, closing the hydrogen after the acetylene is closed for 5min, and naturally cooling under argon atmosphere to obtain the sea urchin-shaped carbon-coated cobalt oxide.
Example 2:
(1) preparing sea urchin-shaped cobaltosic oxide:
0.1g of cobalt chloride and 1g of urea are dissolved in 10mL of deionized water, the mixture is magnetically stirred for 1h, the mixture is uniformly stirred and then transferred to a 150mL reaction kettle, the reaction kettle is placed in a constant temperature furnace, the reaction kettle reacts for 12h at 100 ℃, then the reaction kettle is cooled along with the furnace, the mixture is washed three times by using the deionized water and ethanol, and the mixture is placed in an oven for drying at 60 ℃. And after the reaction is finished, placing the sea urchin-shaped cobaltosic oxide in a muffle furnace, and calcining the sea urchin-shaped cobaltosic oxide for 6 hours at 200 ℃.
(2) Preparing the urchin-shaped carbon-coated cobalt oxide:
and (2) placing 0.1g of the sea urchin-shaped cobaltosic oxide powder prepared in the step (1) in a tubular furnace, heating to 500 ℃ at a heating rate of 0.5 ℃/min under an argon atmosphere, introducing mixed gas of acetylene and hydrogen simultaneously after the temperature is constant, wherein the hydrogen flow rate is 100mL/min, the acetylene flow rate is 10mL/min, continuously introducing for 1min, firstly closing the acetylene after the completion, closing the hydrogen after the acetylene is closed for 7min, and naturally cooling under the argon atmosphere to obtain the sea urchin-shaped carbon-coated cobalt oxide.
Example 3:
(1) preparing sea urchin-shaped cobaltosic oxide:
0.5g of cobalt chloride and 5g of urea are dissolved in 100mL of deionized water, are magnetically stirred for 3 hours, are uniformly stirred and are transferred to a 150mL reaction kettle, are placed in a constant temperature furnace, react for 24 hours at 150 ℃, are cooled along with the furnace, are respectively washed three times by the deionized water and ethanol, and are placed in an oven for drying at 60 ℃. And after the reaction is finished, placing the sea urchin-shaped cobaltosic oxide in a muffle furnace, and calcining the sea urchin-shaped cobaltosic oxide for 12 hours at 400 ℃.
(2) Preparing the urchin-shaped carbon-coated cobalt oxide:
and (2) placing 0.5g of the sea urchin-shaped cobaltosic oxide powder prepared in the step (1) in a tubular furnace, heating to 700 ℃ at a heating rate of 1 ℃/min under argon atmosphere, introducing mixed gas of acetylene and hydrogen simultaneously after the temperature is constant, wherein the hydrogen flow rate is 300mL/min, the acetylene flow rate is 50mL/min, continuously introducing for 3min, firstly closing the acetylene after the completion, closing the hydrogen after the acetylene is closed for 10min, and naturally cooling under argon atmosphere to obtain the sea urchin-shaped carbon-coated cobalt oxide.

Claims (6)

1. A preparation method of a high-specific-capacity lithium ion battery cathode material is characterized in that the lithium ion battery cathode material is a sea urchin-shaped carbon-coated cobalt oxide composite material, and the preparation method comprises the following steps:
(1) preparing sea urchin-shaped cobaltosic oxide:
dissolving cobalt chloride and urea in deionized water, magnetically stirring uniformly, placing the mixed solution in a reaction kettle for hydrothermal reaction, naturally cooling after the hydrothermal reaction is finished, washing the product with the deionized water and ethanol for three times, placing the product in an oven for drying at 60 ℃, and placing the dried product in a muffle furnace for calcining to obtain sea urchin-shaped cobaltosic oxide;
(2) preparing the urchin-shaped carbon-coated cobalt oxide:
placing the sea urchin-shaped cobaltosic oxide powder prepared in the step (1) in a tubular furnace, heating to 500-700 ℃ under argon atmosphere, introducing a mixed gas of acetylene and hydrogen simultaneously after the temperature is constant, continuously introducing for 1-3 min, closing the hydrogen and the acetylene, and naturally cooling under argon atmosphere to obtain a sea urchin-shaped carbon-coated cobalt oxide composite material;
in the step (2), the mass of the sea urchin-shaped cobaltosic oxide powder is 0.1-0.5 g, the hydrogen flow rate is 100-300 mL/min, and the acetylene flow rate is 10-50 mL/min;
in the step (2), after the acetylene and hydrogen mixed gas is continuously introduced for 1-3 min, firstly stopping the introduction of the acetylene, and stopping the introduction of the acetylene for 5-10min and then stopping the introduction of the hydrogen;
in the step (2), the temperature rise rate of the tubular furnace is 0.5-1 ℃/min.
2. The preparation method according to claim 1, wherein in the step (1), the ratio of the cobalt chloride, the urea and the deionized water is as follows: (0.1-0.5) g: (1-5) g: (10-100) mL.
3. The preparation method according to claim 1, wherein in the step (1), the magnetic stirring time is 1-3 h.
4. The preparation method according to claim 1 or 2, wherein in the step (1), the temperature of the hydrothermal reaction is 100 to 150 ℃ and the time of the hydrothermal reaction is 12 to 24 hours.
5. The preparation method according to any one of claims 1 to 3, wherein in the step (1), the calcination temperature is 200 to 400 ℃ and the calcination time is 6 to 12 hours.
6. The lithium ion battery negative electrode material prepared by the preparation method according to any one of claims 1 to 5.
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CN110416509B (en) * 2019-07-17 2021-05-25 肇庆市华师大光电产业研究院 High-specific-capacity lithium ion battery negative electrode material and preparation method thereof
CN110993941B (en) * 2019-12-11 2022-10-04 肇庆市华师大光电产业研究院 Preparation method of hollow spherical carbon-coated iron sulfide composite potassium ion battery cathode material
CN111470546A (en) * 2020-03-17 2020-07-31 肇庆市华师大光电产业研究院 Coating material for functional interlayer of lithium-sulfur battery and preparation method thereof
CN112875748B (en) * 2021-01-28 2023-03-10 陕西科技大学 Preparation method of sea urchin-shaped titanium dioxide multistage microsphere negative electrode material
CN113526566A (en) * 2021-07-19 2021-10-22 四川轻化工大学 Preparation method of nano carbon sphere composite cobalt oxide negative electrode material
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