CN110395728B - Preparation method of porous carbon sphere negative electrode material for lithium battery - Google Patents
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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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- H—ELECTRICITY
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- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
The invention discloses a preparation method of a porous carbon sphere negative electrode material for a lithium battery. The method not only increases the surface defects of the carbon spheres and effectively shortens the diffusion and migration path of lithium ions, but also increases the surface functional groups and the specific surface area of the porous carbon sphere material, effectively relieves the film forming stability of the nano porous carbon spheres in the material, is favorable for large-current charge and discharge, and ensures the appropriate volume energy density and coulombic efficiency of the cathode material. The nano porous carbon sphere negative electrode material for the lithium ion battery prepared by the invention has small and uniform particle size and large specific surface area, has the first discharge specific capacity of nearly 1400 mAh/g under a large-current charge-discharge mechanism, can be stabilized to be more than 400 mAh/g after being circulated for 100 times, has high specific capacity, good rate capability and cycle capability, and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a porous carbon sphere negative electrode material for a lithium battery.
Background
The lithium ion battery has the advantages of high energy density, high open circuit voltage, good cycle performance, no memory effect, environmental protection, small self-discharge and the like, and is widely applied to the fields of mobile phones, game machines, notebook computers, electric automobiles, aerospace, new energy power grids and the like. Lithium ion batteries are also hot spots of research and development of global researchers, and a negative electrode material is one of key factors influencing the comprehensive electrochemical performance of the lithium ion batteries.
Carbon materials were the earliest commercialized negative electrode materials for lithium batteries. The carbon-based material has good conductivity and mechanical stability, the material has good cycling stability and rate performance in the charging and discharging processes of the battery, and the raw material is cheap and visible everywhere, the preparation process is simple and mature, and the de-intercalation mechanism and the reaction mechanism of lithium ions in the carbon material are well known by researchers. Carbon-based negative electrode materials can be divided into two categories: graphite and amorphous carbon. The theoretical specific capacity of the graphite is 372mAh/g, while the actual capacity of the commercial graphite cathode is close to the theoretical value, so that the improvement space is very limited, and the requirement of a high-energy-density battery is difficult to meet. The graphite itself has certain problems, such as relatively high requirements for the electrolyte. Although the demand of the amorphous carbon material on the electrolyte is not high as that of graphite, the reversible capacity of the battery is low in the first charge and discharge, and the amorphous carbon material contains more hydrogen atoms, so that the battery generates obvious voltage hysteresis phenomenon in the circulation. Therefore, the development of new anode materials with high capacity is one of the important directions in the field of lithium ion batteries.
Researchers have conducted a great deal of experimental research in response to the above problems. Mainly to carbon negative electrode material capacity low, energy density is low, and duration is not enough, requires high to the electrolyte, and phenomena such as voltage hysteresis lead to the unable problem such as play electrochemical performance of material, mainly starts from two aspects: firstly, modifying a traditional carbon negative electrode material; secondly, a novel carbon-based material is developed. Patent CN201410103033.9 discloses a Si/C composite as a negative electrode material for lithium ion batteries, the method comprising providing an active material comprising silicon, providing lignin, contacting said active material with a C precursor comprising lignin, converting the lignin to inorganic carbon at a temperature of at least 400 ℃ in an inert gas atmosphere. However, the carbon obtained by the method has low graphitization degree, and when the obtained Si/C composite is used on a lithium ion battery, the cycle performance and the capacity are not ideal, and the capacity is only about 800 mAh/g. The invention patent CN201310522221.0 discloses a porous carbon microsphere, a preparation method and a lithium ion battery cathode material, wherein the porous carbon microsphere prepared by using an emulsion polymerization method simultaneously has a micropore structure, a mesopore structure and a macropore structure, when the porous carbon microsphere is used for the lithium ion battery cathode material, the macropore structure provides a channel for rapid migration for electrolyte, the mesopore structure has the same size as ions in organic electrolyte, and is beneficial to rapid adsorption and desorption of ions, and the micropore structure is beneficial to insertion of lithium ions, so that the lithium ion secondary battery has higher specific capacity and better high-rate charge and discharge performance, but the lithium ion secondary battery has fewer active sites for storing the lithium ions and smaller capacity increasing space, and therefore, the problems of the lithium ion secondary battery are that the energy density is low and the cruising ability is insufficient.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a porous carbon sphere negative electrode material for a lithium battery, which solves the problems of large particle size, large irreversible capacity, low reversible capacity, low energy density, insufficient cruising ability, high requirement on electrolyte, poor wettability with an electrode, poor electrochemical performance and the like of the conventional negative electrode material.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a porous carbon sphere negative electrode material for a lithium battery comprises the following steps:
1) heating a tubular furnace to 450-580 ℃ at a heating rate of 5-10 ℃/min in an inert atmosphere, introducing a carbon source gas, and carrying out chemical vapor deposition reaction under the action of no catalyst to obtain nano carbon spheres;
thus, the carbon source gas is subjected to chemical cracking at a low temperature (450-580 ℃), and the gas does not reach the temperature of complete carbonization (cracking) and deposits, and more hydrogen-containing compounds exist in the interior and on the surface of the generated carbon spheres, so that the compounds are easy to remove in an acid environment to generate defects in the carbon material, the deposition speed is low under the condition of no catalyst and proper airflow, and the produced carbon material is the carbon spheres with small particle size and more defects.
2) Adding the nano carbon spheres obtained in the step 1) into an alkaline substance, fully mixing, then sintering under the protection of an inert atmosphere, carrying out activation treatment, cooling to room temperature, washing to be neutral, drying, then grinding, and then sieving by using a porous sieve of 300-400 meshes to obtain porous carbon spheres;
under the protective gas environment, when the environment temperature rises to the dissolving temperature of alkali, the alkaline substances on the nano carbon spheres can be decomposed into oxides and water, holes are formed on the surfaces of the nano carbon spheres, and the nano carbon spheres are activated for the first time. When the temperature is continuously raised to the decomposition temperature and the vaporization temperature of the oxide, the oxide and the carbon material generate partial oxidation-reduction reaction, and the specific surface area of the carbon material is properly increased, so that the defects of the material are increased, the lithium ion intercalation and deintercalation are accelerated, and the storage condition is increased.
3) And (3) placing the porous carbon spheres prepared in the step 2) into a strong acid solution for reaction, after the reaction is finished, carrying out suction filtration, washing to be neutral, and drying to obtain the porous carbon sphere negative electrode material for the lithium ion battery.
On one hand, in order to remove hydrogen-containing compounds existing inside and on the surface of the carbon spheres, hole defects are formed on the surface and inside of the material through strong acid acidification, which is beneficial to the rapid desorption and storage of lithium ions; on the other hand, functional groups on the surface of the carbon material are increased, the film forming stability of the nano-porous carbon spheres in the material is effectively relieved, large-current charge and discharge are facilitated, and the appropriate volume energy density and coulombic efficiency of the negative electrode material are ensured.
Preferably, the carbon source is natural gas or acetylene.
Preferably, the basic substance is potassium hydroxide, sodium hydroxide, lithium hydroxide, sodium carbonate, potassium carbonate, lithium carbonate or ammonium carbonate.
Preferably, the flow rate of the carbon source gas is 100 to 500 mL/min.
Cracking the carbon source gas at a lower temperature, and if the flow rate of the carbon source gas is too high, discharging the gas in an uncracked state or a cracking initial state to avoid generation of a deposition material; if the flow rate of the carbon source gas is too low, the deposition amount is too large, the particle size of the particles is too large, the defects on the surface of the particles are correspondingly reduced, the rapid transmission of lithium ions is not facilitated, and the storage amount is reduced.
Preferably, the mass ratio of the carbon nanospheres to the alkaline substance is 1: 1-8.
Preferably, the sintering temperature is 600-900 ℃, and the sintering time is 1-4 h.
Preferably, the concentration of the strong acid solution is 1-6 mol, and the strong acid is one or more of nitric acid and sulfuric acid which are mixed according to any proportion.
Preferably, the reaction temperature in the step 3) is 60-90 ℃, and the reaction time is 1-3 h.
Preferably, the inert atmosphere is nitrogen or argon, and the flow rate of the inert atmosphere is 100-300 mL/min.
The invention also provides the porous carbon sphere negative electrode material for the lithium battery, which is prepared by the method.
A lithium ion battery comprises the porous carbon sphere negative electrode material.
Compared with the prior art, the invention has the following beneficial effects:
1. in the preparation of the nano porous carbon sphere cathode material for the lithium ion battery, the uniform, stable and good-dispersibility nano carbon spheres are prepared by controlling the flow rate of a carbon source gas and setting the carbon source gas at a low temperature by adopting a chemical vapor deposition method, and the average diameter of the nano carbon spheres is 80-100 nm; secondly, the alkaline substance is used for activating the nano carbon spheres for the second time, so that the defects and the specific surface area of the nano carbon spheres are increased, and the pore diameters of the nano carbon spheres are more uniform; and finally, strong acid acidification treatment is adopted, so that hole defects are further formed on the surface and inside of the porous carbon sphere, and more oxygen-containing functional groups are formed on the surface of the nano carbon sphere. Therefore, the method not only increases the surface defects of the carbon spheres, effectively shortens the lithium ion diffusion and migration path, but also increases the surface functional groups and the specific surface area of the porous carbon sphere material, effectively relieves the film forming stability of the nano porous carbon spheres in the material, is beneficial to large-current charge and discharge, ensures the appropriate volume energy density and coulombic efficiency of the cathode material, and effectively solves the problems that the existing carbon material has low capacity, low energy density, insufficient cruising ability, high requirements on electrolyte, voltage hysteresis phenomenon and the like, so that the material cannot exert electrochemical performance and the like.
2. The nano porous carbon sphere negative electrode material for the lithium ion battery prepared by the invention has small and uniform particle size and large specific surface area, has the first discharge specific capacity of nearly 1400 mAh/g under a large-current charge-discharge mechanism, has the specific capacity of being stabilized above 400 mAh/g after being circulated for 100 times, and has high specific capacity, good rate capability and cycle performance. The preparation method disclosed by the invention is simple in process flow, low in cost, easy for large-scale production and good in application prospect.
Drawings
FIG. 1 is an XRD pattern of a porous carbon sphere negative electrode material prepared in example 1;
FIG. 2 is an SEM image of a porous carbon sphere negative electrode material prepared in example 1;
fig. 3 is a specific capacity versus cycle number cycle plot of button cell as negative electrode of the porous carbon sphere negative electrode material prepared in example 1 at 200 mA/g.
Detailed Description
The present invention will be described in further detail with reference to the following specific embodiments and the accompanying drawings. The experimental procedures are not specifically described in the following examples, and are carried out in a conventional manner using reagents which are generally commercially available.
Preparation method of porous carbon sphere negative electrode material for lithium battery
Example 1
1) Heating a tubular furnace to 450 ℃ at the heating rate of 5 ℃/min under the protection of argon atmosphere with the flow of 200mL/min, preserving heat for 30min, and then introducing acetylene gas with the flow of 200mL/min for cracking reaction for 1h to obtain nano carbon spheres;
2) adding an alkaline substance (the molar ratio of sodium hydroxide to sodium carbonate is 1: 3) into the nano carbon spheres obtained in the step 1), so that the mass ratio of the nano carbon spheres to the alkaline substance is 1:4, heating to 900 ℃ at a heating rate of 5 ℃/min under the protection of argon gas flow of 200mL/min, preserving heat for 30min, sintering for 4h for activation treatment, cooling to room temperature, washing to be neutral, grinding, and sieving by using a porous sieve of 300 meshes to obtain porous carbon spheres;
3) and (3) placing the porous carbon spheres prepared in the step 2) in a 2 mol/L nitric acid solution, stirring at a constant temperature of 60 ℃ for 3 hours, after the reaction is finished, performing suction filtration, washing to be neutral, and drying to obtain the porous carbon sphere cathode material for the lithium ion battery.
Example 2
1) Heating a tubular furnace to 550 ℃ at the heating rate of 5 ℃/min under the protection of argon gas with the flow of 100mL/min, preserving heat for 40min, and then introducing acetylene gas with the flow of 100mL/min for cracking reaction for 2h to obtain carbon nanospheres;
2) adding an alkaline substance (the molar ratio of potassium hydroxide to ammonium carbonate is 1: 1) into the nano carbon spheres obtained in the step 1), enabling the mass ratio of the nano carbon spheres to the alkaline substance to be 1:5, heating to 800 ℃ at a heating rate of 5 ℃/min under the protection of 100mL/min inert gas flow, preserving heat for 40min, sintering for 3h, carrying out activation treatment, cooling to room temperature, washing to be neutral, grinding, and sieving by using a porous sieve of 400 meshes to obtain porous carbon spheres;
3) and (3) placing the porous carbon spheres prepared in the step 2) in 6mol/L nitric acid solution, stirring at the constant temperature of 80 ℃ for 2h, after the reaction is finished, performing suction filtration, washing to be neutral, and drying to obtain the porous carbon sphere cathode material for the lithium ion battery.
Example 3
1) Heating a tubular furnace to 580 ℃ at the heating rate of 10 ℃/min under the protection of argon gas with the flow of 400mL/min, preserving heat for 30min, and then introducing acetylene gas with the flow of 400mL/min for cracking reaction for 2h to obtain carbon nanospheres;
2) adding sodium hydroxide into the nano carbon spheres obtained in the step 1) to enable the mass ratio of the nano carbon spheres to alkaline substances to be 1:8, heating to 900 ℃ at a heating rate of 10 ℃/min under the protection of 400mL/min inert gas flow, preserving heat for 30min, sintering for 1h for activation treatment, cooling to room temperature, washing to be neutral, grinding, and sieving by using a porous sieve of 300 meshes to obtain porous carbon spheres;
3) and (3) placing the porous carbon spheres prepared in the step 2) in a 5 mol/L nitric acid solution, stirring at a constant temperature of 90 ℃ for 2h, after the reaction is finished, performing suction filtration, washing to neutrality, and drying to obtain the porous carbon sphere cathode material for the lithium ion battery.
Second, performance verification
1. The structure of the nanoporous carbon sphere anode material obtained in example 1 was analyzed by an X-ray diffraction analyzer, as shown in fig. 1.
As can be seen from fig. 1, the nano-porous carbon sphere negative electrode material prepared in example 1 provided by the present invention has a sharp diffraction peak at 2 θ =26 °, corresponds to a (002) crystal face of carbon, has a secondary strong peak at 2 θ =43 °, and corresponds to (100) of carbon, which indicates that the preparation method provided by the present invention prepares a pure-phase nano-porous carbon sphere negative electrode material.
2. The morphology of the activated precursor porous carbon sphere material obtained in example 1 was observed by using a scanning electron microscope, as shown in fig. 2.
From fig. 2, it can be seen that the precursor nanoporous carbon spheres have uniform particle size, weaker particle agglomeration phenomenon, average diameter distribution of about 80-100nm, and a few cracks appear on the surface thereof, which indicates that the more serious the etching condition of the activation degree on the surface of the material is, the more channels and defects of the material are, and theoretically, the defects and the specific surface area of the channel-promoted material are favorable for storing lithium ions, and the lithium storage capacity of the material is increased.
3. The nano-porous carbon sphere negative electrode composite material prepared in the example 1, acetylene black and a water-based binder are mixed according to a mass ratio of 8:1:1, the mixture is placed in a mortar to be ground to prepare slurry with moderate viscosity, the slurry is uniformly coated on copper foil to prepare electrode plates, the electrode plates are assembled into a CR2032 button cell in a glove box, and the electrochemical performance of the CR2032 button cell is tested.
The assembled CR2032 button cell was tested for 100 cycles at a current density of 200mA/g, and the results are shown in fig. 3.
As can be seen from fig. 3, after 100 cycles, the nano-porous carbon sphere negative electrode composite material has more stable specific capacity of the rest cycles except for the serious first cycle attenuation, the initial capacity is maintained at about 1357mAh/g, and the initial capacity is maintained at about 480mAh/g after 100 cycles; the better cycle performance is attributed to the higher specific surface area and the sufficient functional group to relieve the film forming stability of the nano-porous carbon spheres in the material, and the electrochemical activity of the material is also greatly improved.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (4)
1. A preparation method of a porous carbon sphere negative electrode material for a lithium battery is characterized by comprising the following steps:
1) heating a tubular furnace to 450 ℃ at the heating rate of 5 ℃/min under the protection of argon atmosphere with the flow of 200mL/min, preserving heat for 30min, and then introducing acetylene gas with the flow of 200mL/min for cracking reaction for 1h to obtain nano carbon spheres;
2) adding an alkaline substance into the nano carbon spheres obtained in the step 1), wherein the alkaline substance is composed of sodium hydroxide and sodium carbonate according to a molar ratio of 1:3, the mass ratio of the nano carbon spheres to the alkaline substance is 1:4, heating to 900 ℃ at a heating rate of 5 ℃/min under the protection of argon gas flow of 200mL/min, preserving heat for 30min, sintering for 4h for activation treatment, cooling to room temperature, washing to be neutral, grinding, and sieving by a porous sieve of 300 meshes to obtain porous carbon spheres;
3) and (3) placing the porous carbon spheres prepared in the step 2) in a 2 mol/L nitric acid solution, stirring at a constant temperature of 60 ℃ for 3 hours, after the reaction is finished, performing suction filtration, washing to be neutral, and drying to obtain the porous carbon sphere cathode material for the lithium ion battery.
2. A preparation method of a porous carbon sphere negative electrode material for a lithium battery is characterized by comprising the following steps:
1) heating a tubular furnace to 550 ℃ at the heating rate of 5 ℃/min under the protection of argon gas with the flow of 100mL/min, preserving heat for 40min, and then introducing acetylene gas with the flow of 100mL/min for cracking reaction for 2h to obtain carbon nanospheres;
2) adding an alkaline substance into the nano carbon spheres obtained in the step 1), wherein the alkaline substance is prepared from potassium hydroxide and ammonium carbonate according to a molar ratio of 1:1, the mass ratio of the nano carbon spheres to the alkaline substance is 1:5, heating to 800 ℃ at a heating rate of 5 ℃/min under the protection of 100mL/min inert gas flow, preserving heat for 40min, sintering for 3h, activating, cooling to room temperature, washing to be neutral, grinding, and sieving with a porous sieve of 400 meshes to obtain porous carbon spheres;
3) and (3) placing the porous carbon spheres prepared in the step 2) in 6mol/L nitric acid solution, stirring at the constant temperature of 80 ℃ for 2h, after the reaction is finished, performing suction filtration, washing to be neutral, and drying to obtain the porous carbon sphere cathode material for the lithium ion battery.
3. The porous carbon sphere negative electrode material for the lithium battery prepared by the method of any one of claims 1 to 2.
4. A lithium ion battery comprising the porous carbon sphere anode material of claim 3.
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| CN1985340A (en) * | 2004-07-09 | 2007-06-20 | 大阪瓦斯株式会社 | Active carbon for electric double layer capacitor, active carbon electrode for electric double layer capacitor, and electric double layer capacitor therewith |
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