CN107369825B - Nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material and preparation method and application thereof - Google Patents
Nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material, and a preparation method and application thereof. Mixing prepared spherical manganese oxide nanoparticles with dopamine hydrochloride, filtering, washing and drying to obtain a compound of manganese oxide and polydopamine; then converting the polymerized layer into a nitrogen-doped carbon layer through high-temperature carbonization; the nitrogen-doped carbon-coated manganese oxide (MnO @ NC) lithium ion battery composite negative electrode material prepared by the invention has a stable structure and good conductivity, and has excellent rate capability and cycle stability as a lithium ion battery negative electrode material; the polymerization of dopamine is only completed under the conditions of room temperature and alkalescence, so that the cost is low, the energy consumption is low, the control is convenient, the environment is friendly, the lithium ion battery is suitable for practical application, and the industrial scale production can be realized.
Description
Technical Field
The invention belongs to the field of electrochemistry, and particularly relates to a nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material, and a preparation method and application thereof.
Background
The three main subjects of scientific and technical development of the twenty-first century are energy, environment and information, wherein the problems of energy shortage and serious environmental pollution become two major problems to be solved urgently. In order to solve the above two problems, people are engaged in developing new green clean energy sources such as solar energy, wind energy and tidal energy, so as to gradually replace non-renewable fossil fuels causing environmental pollution. However, most of the clean energy sources that have been utilized are uncontrolled and intermittent, which increases the cost of energy storage and management, thereby prompting a great deal of research on energy storage materials.
The traditional energy storage equipment comprises a lead-acid battery and a chromium-nickel battery, wherein the lead-acid battery and the chromium-nickel battery have low energy density and can cause environmental pollution, and the requirements of people cannot be met. Lithium ion batteries have the advantages of high voltage, long service time, large capacity, small volume, no memory effect, good safety performance and the like, and are gradually replacing lead-acid batteries and chromium-nickel batteries, which become the focus of attention of people. With the rapid popularization of portable electronic devices and the rapid development of electric automobiles, the commercial natural graphite negative electrode material cannot meet the requirements of electric devices on energy density and power density, and thus a high-performance lithium ion negative electrode material is urgently needed. Therefore, the development of a new generation of lithium ion battery cathode material is imminent.
Transition metal oxides have been extensively studied in the field of lithium ion batteries because of their high specific capacity. Among numerous transition metal oxides, manganese oxide has the advantages of high initial specific capacity, environmental friendliness, low cost and the like, so that the manganese oxide becomes a potential next-generation lithium ion battery negative electrode material. However, most metal oxides have poor electronic and ionic conductivity, resulting in poor rate performance. Meanwhile, the large volume change of the metal oxide may reduce the cycle stability of the material during repeated charge and discharge processes. Therefore, how to improve the electron conductivity and the cycle stability of the metal oxide is a great challenge for researchers. At present, reducing the particle size, coating or doping with conductive substances is the main means for improving the electrochemical performance of materials.
According to the invention, the nitrogen-doped carbon-coated manganese oxide (MnO @ NC) composite material is prepared by compounding manganese oxide and dopamine hydrochloride by using a natural polymerization method, and until now, no report related to compounding spherical manganese oxide and polydopamine exists.
Disclosure of Invention
Aiming at the defects of poor conductivity, poor cycle stability and the like of the traditional transition metal oxide lithium ion battery cathode material, the invention provides a nitrogen-doped carbon-coated manganese oxide (MnO @ NC) lithium ion battery cathode material, a preparation method and application thereof. In addition, the preparation method of the nitrogen-doped carbon-coated manganese oxide (MnO @ NC) provided by the invention is simple, low in cost and environment-friendly, can promote the development of a large-scale lithium ion battery cathode material, and is expected to be applied in large-scale industrialization.
The purpose of the invention is realized by the following technical scheme.
A preparation method of a nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material comprises the following steps:
1) dissolving a manganese source and ammonium bicarbonate in a solvent, then transferring the solution into a polytetrafluoroethylene lining autoclave for hydrothermal treatment, then centrifugally washing and drying to obtain manganese carbonate nanospheres;
2) dissolving manganese carbonate nanospheres and dopamine hydrochloride in a buffer solution for reaction, then carrying out solid-liquid separation on a reaction product, washing the solid, and drying to obtain a manganese carbonate/polydopamine composite material;
3) calcining the manganese carbonate/polydopamine composite material obtained in the step 2) in a nitrogen atmosphere to obtain the nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material.
Preferably, the manganese source in the step 1) is one or more of manganese acetate, manganese nitrate, manganese sulfate and manganese chloride.
Preferably, the solvent in the step 1) is one or more of ethylene glycol, water and absolute ethyl alcohol.
Preferably, the hydrothermal treatment of step 1) is carried out in a forced air drying oven.
Preferably, the temperature of the hydrothermal treatment in the step 1) is 150-200 ℃, and the time is 10-15 h.
Preferably, the washing in step 1) is 3 to 5 times with water and absolute ethanol, respectively.
Preferably, the drying in step 1) is drying in a vacuum oven at 80 ℃.
Preferably, the particle size of the manganese carbonate/polydopamine nanosphere in the manganese carbonate/polydopamine composite material in the step 2) is 400 ~ 600 nm.
Preferably, the adding mass ratio of the manganese oxide nanospheres and the dopamine hydrochloride in the step 2) is controlled to be 1 (1 ~ 1.5).
Preferably, the reaction of step 2) is carried out at room temperature.
Preferably, the reaction time of the step 2) is 10-48 h.
Preferably, the washing in step 3) is 3 to 5 times with water and absolute ethanol, respectively.
Preferably, the drying in step 3) is drying in a vacuum drying oven at 80 ℃.
Preferably, the calcination treatment in step 4) is to calcine at 600 ~ 800 ℃ for 3-8h, and then reduce the temperature to 300-500 ℃ for 1-3 h.
The composite cathode material of the nitrogen-doped carbon-coated manganese oxide lithium ion battery prepared by the method is formed by uniformly coating nano manganese oxide particles on a layered carbon layer, wherein the particle size of the carbon-coated manganese oxide is 400 ~ 600nm, and the carbon-coated manganese oxide is formed by polymerizing dopamine hydrochloride on the surface of manganese oxide.
The composite cathode material of the nitrogen-doped carbon-coated manganese oxide lithium ion battery is applied to the preparation of the lithium ion battery.
Compared with the prior art, the invention has the following advantages:
1) the coated carbon layer has good conductivity, so that the conductivity of the material can be increased, and the nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material has better rate performance in the charge-discharge process; meanwhile, the carbon layer can also be used as a buffer layer, so that the volume change of the material in the charge and discharge process can be effectively relieved, and the material has better stability.
2) The composite material is doped with nitrogen elements, and the carbon material doped with nitrogen can also improve the cycle performance and rate capability of the material.
3) The polymerization method of dopamine is very simple, and only needs to be carried out at room temperature and under alkalescent conditions, so that the synthesis cost is low, the energy consumption is low, the environment is friendly, the method is suitable for the practical application of lithium ion batteries, and the industrial scale production can be realized.
Drawings
Fig. 1 is an XRD chart of the composite negative electrode material of the nitrogen-doped carbon-coated manganese oxide lithium ion battery obtained in example 1 of the present invention.
Fig. 2 is a raman spectrum of the composite negative electrode material of the nitrogen-doped carbon-coated manganese oxide lithium ion battery obtained in example 1 of the present invention.
Fig. 3 is an SEM image of the composite negative electrode material of the nitrogen-doped carbon-coated manganese oxide lithium ion battery obtained in example 1 of the present invention.
Fig. 4 is a TEM image of the composite negative electrode material of the nitrogen-doped carbon-coated manganese oxide lithium ion battery obtained in example 1 of the present invention.
Fig. 5 is a constant current charge and discharge performance graph of the composite negative electrode material of the nitrogen-doped carbon-coated manganese oxide lithium ion battery obtained in example 1 of the present invention as a negative electrode material of a lithium ion battery.
Fig. 6 is a constant current charge and discharge performance graph of the nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material obtained in example 1 of the present invention after 50 cycles as a lithium ion battery negative electrode material.
Fig. 7 is a graph of rate capability of the composite negative electrode material of the nitrogen-doped carbon-coated manganese oxide lithium ion battery obtained in example 1 of the present invention as a negative electrode material of a lithium ion battery.
Detailed Description
The present invention will be further described with reference to the following examples and drawings, but the embodiments of the present invention are not limited thereto.
Example 1
(1) Weighing 1mmol of manganese acetate and 10mmol of ammonium bicarbonate, dissolving the manganese acetate and the ammonium bicarbonate in 30mL of ethylene glycol, and stirring the mixture at room temperature for 30min to obtain a uniformly mixed solution; transferring the obtained solution into a 50mL reaction kettle, and carrying out hydrothermal reaction for 12h at 180 ℃; carrying out centrifugal separation on the hydrothermal reaction product, washing the hydrothermal reaction product for 4 times by using water and absolute ethyl alcohol, and drying the hydrothermal reaction product in a vacuum drying oven at the temperature of 80 ℃ to obtain precursor nanosphere manganese carbonate particles; subsequently, dopamine coating was performed as follows: respectively weighing 100mg of nanosphere manganese carbonate and 100mg of dopamine hydrochloride, and dissolving in 50mL of Tris buffer (pH = 8.5), stirring at room temperature for 24h, washing with absolute ethanol by centrifugation 4 times, and drying to obtain manganese carbonate @ polydopamine complex. And finally, putting the obtained manganese carbonate @ polydopamine compound into a porcelain boat, placing the porcelain boat in a tubular furnace, reacting for 5 hours at 700 ℃ under the protection of nitrogen atmosphere, then cooling to 500 ℃, continuously reacting for 2 hours, and finally cooling to room temperature to obtain nitrogen-doped carbon-coated manganese oxide particles, namely the nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material. X-ray powder diffraction (XRD) analysis showed the resulting product to be pure manganese oxide with no impurity phase found, indicating a higher purity (as shown in figure 1). As can be seen from the Raman spectrum, the G peak appears at 1350cm-1About, the D peak appears at 1600cm-1On the left and right, the carbon contained in the product obtained by the present invention is mainly amorphous carbon (as shown in FIG. 2). It can be seen from the Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) images that the carbon layer uniformly covers the surface of the spherical manganese oxide particles, and the particle size is 400-600nm (as shown in fig. 3 and 4).
(2) Taking the nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material obtained in the step (1) as an active material, taking acetylene black as a conductive agent, taking polyvinylidene fluoride as a binder, and mixing the active material: conductive agent: binder = 7: 2: 1, then 0.5 mL of azomethylpyrrolidone is dripped into a penicillin bottle with the mass ratio of 1, the mixture is stirred for 4 hours to form slurry, the slurry is uniformly coated on a copper foil, then the slurry is dried for 12 hours in a constant-temperature drying box with the temperature of 80 ℃, a small wafer with the thickness of 12mm is punched by a punching machine after the slurry is dried to constant weight, the small wafer is taken as a working electrode, the small wafer is placed into a glove box filled with argon under the condition of ensuring no water, the purchased lithium wafer is taken as a counter electrode and a reference electrode, the used Celgard 2400 type diaphragm is provided, and the electrolyte is 1 mol L-1LiPF of6Mixed with Ethylene Carbonate (EC), dimethyl carbonate (DMC) (EC: DMC = 1: 2, v/v) and finally assembled into a button cell type CR2025 in a glove box, which must be kept at an oxygen and water vapour content of less than 1 ppm throughout the process. When constant current charge and discharge test is carried out at the temperature of 25 ℃ and the current density of 100 mA/g, the first discharge capacity is 2312 mAh/gThe charging capacity reaches 1444 mAh/g (as shown in FIG. 5). When a constant current charge/discharge test was performed at a current density of 100 mA/g at a temperature of 25 ℃, the reversible capacity was 1126 mAh/g after 50 weeks of circulation (as shown in FIG. 6). The rate performance at different current densities at the temperature of 25 ℃ is shown in figure 6, and the reversible capacity of about 330 mAh/g still has good rate performance (shown in figure 7) at the large current density of 5000 mA/g.
Example 2
(1) Weighing 1mmol of manganese nitrate and 5mmol of ammonium bicarbonate, dissolving the manganese nitrate and the ammonium bicarbonate in 30mL of absolute ethanol, and stirring the mixture at room temperature for 30min to obtain a uniformly mixed solution; transferring the obtained solution into a 50mL reaction kettle, and carrying out hydrothermal reaction for 10h at 150 ℃; carrying out centrifugal separation on the hydrothermal reaction product, washing the hydrothermal reaction product for 4 times by using water and absolute ethyl alcohol, and drying the hydrothermal reaction product in a vacuum drying oven at the temperature of 80 ℃ to obtain precursor nanosphere manganese carbonate particles; subsequently, dopamine coating was performed as follows: 100mg of nanosphere manganese carbonate and 150mg of dopamine hydrochloride are respectively weighed and dissolved in 50mL of Tris buffer solution (pH = 8.5), the solution is stirred for 24 hours at room temperature, and the product manganese carbonate @ polydopamine composite is obtained after centrifugal washing for 4 times by absolute ethyl alcohol and drying. And finally, putting the obtained manganese carbonate @ polydopamine compound into a porcelain boat, placing the porcelain boat in a tubular furnace, reacting for 3h at 800 ℃ under the protection of nitrogen atmosphere, then cooling to 500 ℃, continuously reacting for 2h, and finally cooling to room temperature to obtain nitrogen-doped carbon-coated manganese oxide particles, namely the nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material.
(2) The nitrogen-doped carbon-coated manganese oxide prepared in this example and a lithium sheet were assembled into a button type half cell in the same manner as in example 1. When constant-current charge and discharge tests are carried out at the temperature of 25 ℃ and the current density of 100 mA/g, the first discharge capacity is 2002 mAh/g, and the first charge capacity reaches 1204 mAh/g. When constant current charge and discharge tests are carried out at the temperature of 25 ℃ and the current density of 100 mA/g, the reversible capacity is 1008 mAh/g after circulation for 50 weeks. At the temperature of 25 ℃, the reversible capacity of about 300 mAh/g still has under the heavy current density of 5000mA/g, and has better rate performance.
Example 3
(1) Weighing 1mmol of manganese sulfate and 15mmol of ammonium bicarbonate, dissolving in 30mL of deionized water, and stirring at room temperature for 30min to obtain a uniformly mixed solution; transferring the obtained solution into a 50mL reaction kettle, and carrying out hydrothermal reaction for 15h at 200 ℃; carrying out centrifugal separation on the hydrothermal reaction product, washing the hydrothermal reaction product for 4 times by using deionized water and absolute ethyl alcohol respectively, and drying the hydrothermal reaction product in a vacuum drying oven at the temperature of 80 ℃ to obtain precursor nanosphere manganese carbonate particles; subsequently, dopamine coating was performed as follows: 100mg of nanosphere manganese carbonate and 125mg of dopamine hydrochloride are respectively weighed and dissolved in 50mL of Tris buffer solution (pH = 8.5), the solution is stirred for 24 hours at room temperature, and the product manganese carbonate @ polydopamine composite is obtained after centrifugal washing for 4 times by absolute ethyl alcohol and drying. And finally, putting the obtained manganese carbonate @ polydopamine compound into a porcelain boat, placing the porcelain boat in a tubular furnace, reacting for 8 hours at the temperature of 600 ℃ under the protection of nitrogen atmosphere, then cooling to 500 ℃, continuously reacting for 2 hours, and finally cooling to room temperature to obtain nitrogen-doped carbon-coated manganese oxide particles, namely the nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material.
(2) The nitrogen-doped carbon-coated manganese oxide prepared in this example and a lithium sheet were assembled into a button type half cell in the same manner as in example 1. When constant-current charge and discharge tests are carried out at the temperature of 25 ℃ and the current density of 100 mA/g, the first discharge capacity is 1908 mAh/g, and the first charge capacity reaches 1054 mAh/g. When a constant-current charge and discharge test is carried out at the temperature of 25 ℃ and the current density of 100 mA/g, the reversible capacity is 1038 mAh/g after circulation for 50 weeks. At the temperature of 25 ℃, the reversible capacity of about 310 mAh/g still has under the heavy current density of 5000mA/g, and has better rate performance.
Claims (5)
1. A preparation method of a nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material is characterized by comprising the following steps of:
1) dissolving a manganese source and ammonium bicarbonate in a solvent, then transferring the solution into a polytetrafluoroethylene lining autoclave for hydrothermal treatment, then centrifugally washing and drying to obtain manganese carbonate nanospheres;
2) dissolving manganese carbonate nanospheres and dopamine hydrochloride in a buffer solution for reaction, then carrying out solid-liquid separation on a reaction product, washing the solid, and drying to obtain a manganese carbonate/polydopamine composite material;
3) calcining the manganese carbonate/polydopamine composite material obtained in the step 2) in a nitrogen atmosphere to obtain a nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material;
the manganese source in the step 1) is one or more of manganese acetate, manganese nitrate, manganese sulfate and manganese chloride; the molar ratio of the manganese source to the ammonium bicarbonate is 1: (5-15);
the temperature of the hydrothermal treatment in the step 1) is 150-200 ℃, and the time of the hydrothermal treatment is 10-15 h;
step 2), the adding mass ratio of the manganese carbonate nanospheres to the dopamine hydrochloride is controlled to be 1 (1 ~ 1.5.5);
the reaction time of the step 2) is 10-48 h;
the calcining treatment in the step 3) is to calcine for 3 to 8 hours at the temperature of 600 ~ 800 ℃ and then to calcine for 1 to 3 hours at the temperature of 300 ℃ and 500 ℃.
2. The preparation method according to claim 1, wherein the solvent in step 1) is one or more selected from ethylene glycol, water and absolute ethyl alcohol.
3. The preparation method of claim 1, wherein the manganese carbonate/polydopamine nanosphere in the manganese carbonate/polydopamine composite material of step 2) has a particle size of 400 ~ 600 nm.
4. A nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material prepared by the method of any one of claims 1-3.
5. The application of the nitrogen-doped carbon-coated manganese oxide lithium ion battery composite negative electrode material in the preparation of a lithium ion battery, according to claim 4.
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