CN107492648B - Cotton-based carbon fiber/MnO/C material, preparation method and application - Google Patents
Cotton-based carbon fiber/MnO/C material, preparation method and application Download PDFInfo
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- CN107492648B CN107492648B CN201710714306.7A CN201710714306A CN107492648B CN 107492648 B CN107492648 B CN 107492648B CN 201710714306 A CN201710714306 A CN 201710714306A CN 107492648 B CN107492648 B CN 107492648B
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- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- H01—ELECTRIC ELEMENTS
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
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- H01M4/58—Selection 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A cotton-based carbon fiber/MnO/C material, a preparation method and an application relate to the field of lithium ion batteries, and the preparation method comprises the steps of carrying out hydrothermal treatment on crushed cotton and an aqueous solution of zinc chloride, cooling and then carrying out suction filtration; respectively washing and filtering with dilute acid and pure water; mixing the dried filter residue with molten salt, and carrying out thermal cracking in an inert atmosphere; cleaning and drying the thermal cracking product to obtain a cotton-based carbon fiber material; weighing cotton-based carbon fibers, adding the cotton-based carbon fibers into an ethanol solution of potassium permanganate for soaking, dropwise adding an ethanol solution of pyrrole, and carrying out solvothermal reaction; the thermal reaction product is cleaned, dried and calcined in the inert protective atmosphere, and the preparation method has rich raw materials, low cost and easy industrial production; the prepared cotton-based carbon fiber/MnO/C material is low in cost and has excellent rate capability and cycling stability; the cotton-based carbon fiber/MnO/C material can be used as a lithium ion battery cathode and can improve the performance of the lithium ion battery.
Description
Technical Field
The invention relates to the field of lithium ion batteries, and particularly relates to a cotton-based carbon fiber/MnO/C material, a preparation method and application thereof.
Background
As a chemical power source for energy storage and output, lithium ion batteries have been gaining increasing attention since the last 90 th century, since the market by SONY corporation. After more than 20 years of research and development, the application of lithium ion batteries has penetrated into various fields of human industrial production and life, and plays an increasingly important role in solving the problems of energy shortage, environmental pollution and the like faced by human beings. In recent years, the air pollution caused by fuel vehicles is increasingly emphasized, and research and development of zero-emission electric automobiles are fundamental ways for solving the problem. Therefore, the lithium ion battery serving as a high-power supply is applied to the field of new energy automobiles and is a necessary trend, and future electric automobiles will develop a wider market for the lithium ion battery. As an important component of lithium ion batteries, the performance of the positive, negative and electrolyte materials significantly affects the performance of the overall battery.
However, the existing negative electrode materials, such as graphite, have limited reversible capacity, have certain limitations in application, and are difficult to meet the increasing demand for high-energy lithium ion batteries. Research has found that the use of carbon-containing composite materials as electrode materials is an effective way to achieve higher energy densities. Among numerous transition metal oxide negative electrode materials, the charging potential platform of MnO is only 1.2V, the theoretical specific capacity is 755mAh/g, and manganese resources are rich, cheap, easy to obtain and environment-friendly, so that the material is considered as a lithium ion battery negative electrode material with great prospect. However, similar to other transition metal oxides, MnO also has the disadvantages of low coulombic efficiency, high rate, poor cycle performance, etc. for the first time, limiting its application.
Therefore, an electrode material having a high capacity, an excellent rate capability and a high cycle stability is required.
Disclosure of Invention
The invention aims to provide a preparation method of a cotton-based carbon fiber/MnO/C material, which has the advantages of rich raw materials, low cost and easiness in industrial production.
It is another object of the present invention to provide a cotton-based carbon fiber/MnO/C material that is low cost and has excellent rate capability and cycle stability.
The invention also aims to provide application of the cotton-based carbon fiber/MnO/C material, which can be used as a lithium ion battery cathode and can improve the performance of the lithium ion battery.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a preparation method of a cotton-based carbon fiber/MnO/C material, which comprises the following steps:
carrying out hydrothermal treatment on the crushed cotton and an aqueous solution of zinc chloride, cooling and then carrying out suction filtration; washing the filter residue obtained by suction filtration with dilute acid and pure water respectively until the filter residue is neutral, and drying; mixing the dried filter residue with molten salt, and carrying out thermal cracking in an inert atmosphere; cleaning and drying the thermal cracking product to obtain a cotton-based carbon fiber material;
weighing cotton-based carbon fibers, adding the cotton-based carbon fibers into an ethanol solution of potassium permanganate for soaking, then dropwise adding an ethanol solution of pyrrole, and carrying out solvothermal reaction; and cleaning and drying the thermal reaction product, and calcining under an inert protective atmosphere.
Further, in the preferred embodiment of the present invention, the mass ratio of cotton to zinc chloride is 1: 2-4.
Further, in the preferred embodiment of the present invention, the temperature of the hydrothermal treatment is 140-160 ℃, and the time of the hydrothermal treatment is 12-24 h.
Further, in a preferred embodiment of the present invention, the molten salt is a mixed salt of sodium sulfate and sodium hydroxide or a mixed salt of potassium sulfate and potassium hydroxide, and the molar ratio of sodium sulfate to sodium hydroxide is 1: 7-10, wherein the molar ratio of potassium sulfate to potassium hydroxide is 1: 15-16.
Further, in the preferred embodiment of the present invention, the thermal cracking temperature is 400-.
Further, in a preferred embodiment of the present invention, the mole ratio of the cotton-based carbon fiber to potassium permanganate is 8: 1-3, wherein the dosage ratio of the pyrrole to the potassium permanganate is 1-3 ml: 10-20 mmol.
Further, in the preferred embodiment of the present invention, the temperature of the solvothermal reaction is 120-180 ℃, and the time of the solvothermal reaction is 6-8 h.
Further, in the preferred embodiment of the present invention, the calcination temperature is 700-.
The invention provides a cotton-based carbon fiber/MnO/C material, which is prepared by adopting the preparation method of the cotton-based carbon fiber/MnO/C material.
The invention provides an application of a cotton-based carbon fiber/MnO/C material, wherein the cotton-based carbon fiber/MnO/C material is used as a lithium ion battery cathode material.
The cotton-based carbon fiber/MnO/C material, the preparation method and the application of the invention have the beneficial effects that: the preparation method of the cotton-based carbon fiber/MnO/C material comprises the steps of carrying out hydrothermal treatment on crushed cotton and an aqueous solution of zinc chloride, cooling and carrying out suction filtration; washing the filter residue obtained by suction filtration with dilute acid and pure water respectively until the filter residue is neutral, and drying; mixing the dried filter residue with molten salt, and carrying out thermal cracking in an inert atmosphere; cleaning and drying the thermal cracking product to obtain a cotton-based carbon fiber material; weighing cotton-based carbon fibers, adding the cotton-based carbon fibers into an ethanol solution of potassium permanganate for soaking, then dropwise adding an ethanol solution of pyrrole, and carrying out solvothermal reaction; the thermal reaction product is cleaned, dried and calcined in the inert protective atmosphere, and the preparation method has rich raw materials, low cost and easy industrial production; the prepared cotton-based carbon fiber/MnO/C material is low in cost and has excellent rate capability and cycling stability; the cotton-based carbon fiber/MnO/C material can be used as a lithium ion battery cathode, and the performance of the lithium ion battery is improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The cotton-based carbon fiber/MnO/C material, the preparation method and the application of the invention are specifically described below.
The embodiment of the invention provides a preparation method of a cotton-based carbon fiber/MnO/C material, which comprises the following steps:
(a) preparing cotton-based carbon fibers:
firstly, uniformly mixing crushed cotton with an aqueous solution of zinc chloride, carrying out hydrothermal treatment, and carrying out suction filtration after naturally cooling. In this example, the mass ratio of cotton to zinc chloride was 1: 2-4; adding the raw materials into a hydrothermal reaction kettle for hydrothermal treatment; the temperature of the hydrothermal treatment is 140-160 ℃, and the time of the hydrothermal treatment is 12-24 h.
Secondly, washing filter residues obtained by suction filtration with dilute acid and pure water respectively until the filter residues are neutral, and drying.
And then, mixing the dried filter residue with molten salt, and performing thermal cracking in an inert atmosphere, wherein the molten salt is a mixed salt of sodium sulfate and sodium hydroxide or a mixed salt of potassium sulfate and potassium hydroxide, and the molar ratio of the sodium sulfate to the sodium hydroxide is 1: 7-10, wherein the molar ratio of potassium sulfate to potassium hydroxide is 1: 15-16; putting the reaction raw materials into a vacuum tube furnace protected by inert atmosphere for thermal cracking; the thermal cracking temperature is 400-900 ℃, and the thermal cracking time is 1-3 h.
And then, cleaning and drying the thermal cracking product to obtain the cotton-based carbon fiber.
(b) Preparing a cotton-based carbon fiber/MnO/C material:
firstly, dissolving potassium permanganate in ethanol to form an ethanol solution of potassium permanganate, weighing the required cotton-based carbon fiber, adding the cotton-based carbon fiber into the ethanol solution of potassium permanganate, and soaking, wherein in the embodiment, the molar ratio of the cotton-based carbon fiber to the potassium permanganate is 8: 1-3; the soaking time is 1.5-4 h.
Secondly, slowly dropwise adding an ethanol solution of pyrrole, uniformly stirring, and then carrying out solvothermal reaction, wherein in the embodiment, the dosage ratio of the pyrrole to the potassium permanganate is 1-3 ml: 10-20 mmol; transferring the reaction raw materials into a reaction kettle to carry out solvothermal reaction; the temperature of the solvent thermal reaction is 120-180 ℃, and the time of the solvent thermal reaction is 6-8 h.
And then, cleaning and drying the thermal reaction product, and calcining in an inert protective atmosphere at the temperature of 700-900 ℃ for 0.5-1.5h to obtain the cotton-based carbon fiber/MnO/C material.
The embodiment of the invention provides a cotton-based carbon fiber/MnO/C material, which is prepared by adopting the preparation method of the cotton-based carbon fiber/MnO/C material.
According to the embodiment of the invention, the good morphology and excellent ion and electron conductivity of the carbon material are utilized, and the small-particle MnO active material is loaded on the surface or inside, so that the volume change caused by the separation and the intercalation of lithium ions can be relieved, the agglomeration of the small particles in the circulation process can be prevented, and the rate capability and the circulation performance of the composite electrode material can be improved.
The embodiment of the invention provides application of a cotton-based carbon fiber/MnO/C material, wherein the cotton-based carbon fiber/MnO/C material is used as a lithium ion battery cathode material.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a cotton-based carbon fiber/MnO/C material, which is prepared by the following preparation method:
firstly, the cotton is crushed, 5g of crushed cotton is weighed and added into 75ml of 1mol/LZnCl2(the mass ratio of the cotton to the zinc chloride is 1: 2.04), stirring uniformly, transferring into a 100ml reaction kettle, placing in a drying oven at 140 ℃ for heat preservation for 24 hours, and filtering after natural cooling. And secondly, washing filter residues obtained by suction filtration with acid and water until the filter residues are washed and dried. Mixing the dried residue with mixed salt (composed of sodium hydroxide and sodium sulfate at molar ratio of 9: 1), and placing in inert atmosphere (Ar or N)2) The obtained product was thermally cracked in a tube furnace at 450 ℃ for 3 hours under protection to obtain 1.3417g of cotton-based carbon fiber.
Firstly weighing 4mmol of cotton-based carbon fiber, adding the cotton-based carbon fiber into 40ml of ethanol dissolved with 1.5mmol of potassium permanganate, soaking for 2 hours, and uniformly oscillating by ultrasonic. And then 0.1ml of pyrrole is transferred and dissolved in 20ml of ethanol, the ethanol solution of the pyrrole is slowly dripped into the ethanol solution of the potassium permanganate added with the cotton-based carbon fiber, the ultrasonic oscillation is continued to be uniform, the mixed solution is transferred into a 100ml reaction kettle, the reaction kettle is placed in a 120 ℃ oven for heat preservation for 8 hours, and the mixture is naturally cooled. Washing the thermal reaction product with ethanol and water for 3 times, oven drying, and placing in inert atmosphere (Ar or N)2) Calcining for 1.5h in a 700 ℃ tubular furnace under protection to obtain the cotton-based carbon fiber/MnO/C material.
Example 2
The embodiment provides a cotton-based carbon fiber/MnO/C material, which is prepared by the following preparation method:
firstly, the cotton is crushed, 5g of crushed cotton is weighed and added into 70ml of 2mol/LZnCl2(the mass ratio of the cotton to the zinc chloride is 1: 3.82), stirring uniformly, transferring the mixture into a 100ml reaction kettle, placing the reaction kettle in a 160 ℃ oven for heat preservation for 12 hours, and filtering after naturally cooling. And secondly, washing filter residues obtained by suction filtration with acid and water until the filter residues are washed and dried. Mixing the dried residue with mixed salt (composed of potassium hydroxide and potassium sulfate at a molar ratio of potassium hydroxide to potassium sulfate of 15.67: 1), and placing in inert atmosphere (Ar or N)2) Thermally cracking for 1h in a 850 ℃ tubular furnace under protection. Then cleaning and drying the thermal cracking product1.1384g of cotton-based carbon fiber was obtained.
Firstly weighing 4mmol of cotton-based carbon fiber, adding the cotton-based carbon fiber into 40ml of ethanol dissolved with 0.5mmol of potassium permanganate (the molar ratio of the cotton-based carbon fiber to the potassium permanganate is 8: 1), soaking for 2h, and uniformly oscillating by ultrasonic. And then 0.12ml of pyrrole is transferred and dissolved in 20ml of ethanol, the ethanol solution of the pyrrole is slowly dripped into the ethanol solution of the potassium permanganate added with the cotton-based carbon fiber, the ultrasonic oscillation is continued to be uniform, the mixed solution is transferred into a 100ml reaction kettle, the reaction kettle is placed in an oven at the temperature of 170 ℃ for heat preservation for 6 hours, and the mixture is naturally cooled. Washing the thermal reaction product with ethanol and water for 3 times, oven drying, and placing in inert atmosphere (Ar or N)2) Calcining for 0.5h in a 900 ℃ tubular furnace under protection to obtain the cotton-based carbon fiber/MnO/C material.
Example 3
The embodiment provides a cotton-based carbon fiber/MnO/C material, which is prepared by the following preparation method:
firstly, the cotton is crushed, 5g of the crushed cotton is weighed and added into 75ml of 1.5mol/LZnCl2(the mass ratio of the cotton to the zinc chloride is 1: 3.07), stirring uniformly, transferring the mixture into a 100ml reaction kettle, placing the reaction kettle in a 150 ℃ oven, preserving heat for 16 hours, and naturally cooling and filtering the mixture. And secondly, washing filter residues obtained by suction filtration with acid and water until the filter residues are washed and dried. Mixing the dried residue with mixed salt (composed of sodium hydroxide and sodium sulfate at molar ratio of 9: 1), and placing in inert atmosphere (Ar or N)2) Thermal cracking in a 650 ℃ tubular furnace for 2h under protection. 1.2763g of cotton-based carbon fiber was obtained.
Firstly weighing 4mmol of cotton-based carbon fiber, adding the cotton-based carbon fiber into 40ml of ethanol dissolved with 1mmol of potassium permanganate, soaking for 2 hours, and uniformly oscillating with ultrasound. And secondly, transferring 0.3ml of pyrrole to be dissolved in 20ml of ethanol, slowly dripping ethanol solution of the pyrrole into the ethanol solution of the potassium permanganate added with the cotton-based carbon fiber, continuing to perform ultrasonic oscillation uniformly, transferring the mixed solution into a 100ml reaction kettle, placing the reaction kettle in a 150 ℃ oven for heat preservation for 8 hours, and naturally cooling the reaction kettle. Washing the thermal reaction product with ethanol and water for 3 times, oven drying, and placing in inert atmosphere (Ar or N)2) Under the protection ofCalcining for 1h in a 800 ℃ tubular furnace to obtain the cotton-based carbon fiber/MnO/C material.
Example 4
In this example, the cotton-based carbon fiber/MnO/C materials of examples 1-3 were assembled into lithium ion batteries, respectively, as follows:
each of the samples of examples 1 to 3 was dissolved in N-methylpyrrolidone with acetylene black and polyvinylidene fluoride in a mass ratio of 8:1:1, respectively, and then coated on a copper foil. The copper foil was dried at 80 ℃ for 10 hours under vacuum, rolled, and cut into a wafer with a diameter of 14 mm to prepare an electrode. Using metallic lithium plate as counter electrode, LiPF6A CR2016 cell was assembled in a glove box as an electrolyte.
Under room temperature, in the voltage range of 0.01-3.0V, the current density is 100mA g-1Charging and discharging with specific discharge capacity of 850, 870 and 905mA h g-1. Increase in current density from 100 to 2000mA g-1The specific discharge capacity of the material is 410 mA h g, 407 mA h g and 420mA h g respectively-1. At 500mA g-1After 500 weeks of charging and discharging at the current density, the capacity retention rates were 75%, and 78%, respectively.
In conclusion, the preparation method of the cotton-based carbon fiber/MnO/C material provided by the embodiment of the invention has the advantages of rich raw materials, low cost and easiness in industrial production; the cotton-based carbon fiber/MnO/C material is low in cost and has excellent rate capability and cycling stability; the cotton-based carbon fiber/MnO/C material can be used as a lithium ion battery cathode to improve the performance of the lithium ion battery.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of a cotton-based carbon fiber/MnO/C material is characterized by comprising the following steps:
carrying out hydrothermal treatment on the crushed cotton and an aqueous solution of zinc chloride, cooling and then carrying out suction filtration; washing the filter residue obtained by suction filtration with dilute acid and pure water respectively until the filter residue is neutral, and drying; mixing the dried filter residue with molten salt, and carrying out thermal cracking in an inert atmosphere; cleaning and drying the thermal cracking product to obtain a cotton-based carbon fiber material;
weighing the cotton-based carbon fibers, adding the cotton-based carbon fibers into an ethanol solution of potassium permanganate for soaking, then dropwise adding an ethanol solution of pyrrole, and carrying out solvothermal reaction; and cleaning and drying the thermal reaction product, and calcining under an inert protective atmosphere.
2. The method of claim 1, wherein the mass ratio of cotton to zinc chloride is 1: 2-4.
3. The method for preparing cotton-based carbon fiber/MnO/C material according to claim 1, wherein the temperature of the hydrothermal treatment is 140-160 ℃, and the time of the hydrothermal treatment is 12-24 h.
4. The method for preparing cotton-based carbon fiber/MnO/C material according to claim 1, wherein said molten salt is a mixed salt of sodium sulfate and sodium hydroxide or a mixed salt of potassium sulfate and potassium hydroxide, and the molar ratio of sodium sulfate to sodium hydroxide is 1: 7-10, wherein the molar ratio of potassium sulfate to potassium hydroxide is 1: 15-16.
5. The method for preparing cotton-based carbon fiber/MnO/C material according to claim 1, wherein the temperature of said thermal cracking is 400-900 ℃ and the time of said thermal cracking is 1-3 h.
6. The method of claim 1, wherein the molar ratio of the cotton-based carbon fibers to the potassium permanganate is 8: 1-3, wherein the dosage ratio of the pyrrole to the potassium permanganate in the ethanol solution of the pyrrole is 1-3 ml: 10-20 mmol.
7. The method for preparing cotton-based carbon fiber/MnO/C material as defined in claim 1, wherein the temperature of the solvothermal reaction is 120-180 ℃ and the time of the solvothermal reaction is 6-8 h.
8. The method for preparing cotton-based carbon fiber/MnO/C material according to claim 1, wherein the calcination temperature is 700-900 ℃ and the calcination time is 0.5-1.5 h.
9. A cotton-based carbon fiber/MnO/C material, characterized in that it is obtained by the method of preparation of a cotton-based carbon fiber/MnO/C material according to any one of claims 1 to 8.
10. Use of the cotton-based carbon fiber/MnO/C material of claim 9 as a negative electrode material for lithium ion batteries.
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| CN109192960A (en) * | 2018-09-18 | 2019-01-11 | 龙岩学院 | A kind of MnO/ cellulose base porous carbon and preparation method thereof and the application in lithium ion battery negative material |
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