CN111029565A - Lithium ion battery cathode material NiCo2O4Preparation method of porous nanosheet - Google Patents
Lithium ion battery cathode material NiCo2O4Preparation method of porous nanosheet Download PDFInfo
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- CN111029565A CN111029565A CN201911322454.XA CN201911322454A CN111029565A CN 111029565 A CN111029565 A CN 111029565A CN 201911322454 A CN201911322454 A CN 201911322454A CN 111029565 A CN111029565 A CN 111029565A
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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
- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- 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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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- 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 lithium ion battery cathode material NiCo2O4The preparation method of the porous nano-sheet is characterized in that cobalt nitrate hexahydrate and nickel nitrate hexahydrate are used as reaction raw materials, water, ethanol and a very small amount of ethanolamine are used as a solvent system, polyvinylpyrrolidone is used as a surfactant, and a lithium ion battery cathode material NiCo is prepared by a solvothermal method and thermal decomposition of a precursor2O4Porous nanoplatelets. The invention can obtain NiCo with high dispersibility and porous structure simply by regulating and controlling the solvent component and the surfactant and assisting simple and convenient heat treatment2O4The nano sheet has good product form and stable electrochemical performance, the reversible capacity reaches 695mAh/g after the nano sheet is cycled for 1000 times under the current density of 0.5A/g, and the reversible capacity is far higher than that of a commercial graphite negative electrode materialThe cooking theory has specific capacity (372 mAh/g), and the reaction system has low cost, does not generate pollutants, and is green and environment-friendly; the preparation process is simple, the yield and the purity are high, the repeatability is good, and the industrial production is easy to realize.
Description
Technical Field
The invention specifically relates to lithium ionsNiCo as negative electrode material of battery2O4A preparation method of porous nano-sheets belongs to the technical field of preparation of electrode materials of lithium ion batteries.
Background
The lithium ion battery is not only widely applied to small electronic products, but also can be used as a driving power supply of an electric automobile. However, the existing graphite negative electrode material is difficult to meet the market demand due to the lower theoretical specific capacity (372 mAh/g) and the poor rate performance, and the development of a high-performance negative electrode material is urgently needed. Bimetallic oxide NiCo2O4Due to higher theoretical specific capacity (890 mAh/g) and compared with widely researched Co3O4Has higher electrochemical activity and lower raw material cost, and is considered to be a lithium ion battery cathode material with great application and development prospects. Since the volume change of the metal oxide negative electrode material is huge in the charging and discharging process, the material is easy to pulverize and inactivate, and the cycle life is short, researchers mostly adopt the construction of a porous micro-nano hierarchical structure to buffer the huge volume change to solve the problems. In recent years, porous hierarchical structure NiCo of different micron sizes2O4Such as porous microspheres, hollow microspheres, porous cubes, flower-like microspheres, etc., have been prepared and used for lithium ion negative electrode materials. Because the bulk electronic conductivity of the metal oxide is not high, when the lithium ion battery negative plate is manufactured, the metal oxide, the conductive carbon nano particles and the binder are mixed according to a certain proportion to form paste, the paste is coated on two sides of a copper foil, and the paste is dried and rolled to form the lithium ion battery negative plate. Therefore, the surface of the micron-sized active material can be well contacted with the conductive carbon nanoparticles to improve the conductivity of the micron-sized active material, but the interior of the micron-sized active material cannot be contacted with the conductive carbon nanoparticles, so that the transmission of electrons is limited, and the exertion of the electrochemical activity of the micron-sized active material is influenced.
The porous nano-sheet structure can well avoid the problems, and the sheet structure can well contact with the conductive carbon nano-particles, so that the electronic conductivity of the material is improved; the porous structure can relieve the volume change of the material in the charging and discharging process, and is an ideal anode material microstructure. Currently, NiCo is prepared2O4For porous nanosheetsThe reports of the lithium ion battery cathode material are less, and the pure NiCo is prepared by adopting a solvothermal method in the document J Mater Chem A, 2014, 2, 4449-2O4Porous nano-sheets with a capacity of about 300 mAh/g after circulation for 70 times; the reference "ChemPlusChem 2015, 80, 1725-2O4The capacity of the porous nano-sheet is 626 mAh/g after circulation for 50 times; the cycle life of the nanosheet negative electrode material is short. The document J Alloy Compd, 2019, 772, 72-79 adopts a solvothermal method, ethanol and water are used as solvents, the pH of the solution is adjusted to 9, the solution reacts for 3 hours at 250 ℃ to obtain a precursor, and then the precursor is roasted for 3 hours at 500 ℃ to obtain NiCo2O4And the capacity of the porous nano sheet after circulation for 350 times is 674 mAh/g. Although the cycle number of the technology is improved, the technology still cannot meet the actual requirement, and the nanosheet synthesis reaction temperature exceeds 200 ℃, so that the equipment safety requirement is high; the pH of the solution needs to be controlled in the reaction system. Therefore, the existing synthesis processes have the problems of low cycle number and the like.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a lithium ion battery cathode material NiCo2O4The preparation method of the porous nano-sheet adopts the solvothermal synthesis technology to prepare NiCo2O4The porous nanosheet is used as the lithium ion battery cathode material, and the method has the advantages of low reaction temperature, easily controlled reaction conditions, low cost and easy mass preparation; the obtained nano-sheet has high reversible capacity and long cycle life.
In order to achieve the purpose, the invention adopts the technical means that:
lithium ion battery cathode material NiCo2O4The preparation method of the porous nano-sheet is characterized in that cobalt nitrate hexahydrate and nickel nitrate hexahydrate are used as reaction raw materials, water, ethanol and a very small amount of ethanolamine are used as a solvent system, polyvinylpyrrolidone is used as a surfactant, and a lithium ion battery cathode material NiCo is prepared by a solvothermal method and thermal decomposition of a precursor2O4Porous nanoplatelets.
The NiCo2O4Porous nanoparticlesThe preparation method of the tablet comprises the following specific steps:
accurately weighing nickel nitrate hexahydrate, cobalt nitrate hexahydrate and polyvinylpyrrolidone according to the amount, sequentially adding the nickel nitrate hexahydrate, the cobalt nitrate hexahydrate and the polyvinylpyrrolidone into a mixed solution of water, ethanol and ethanolamine, and stirring to obtain a uniform suspension;
secondly, transferring the suspension obtained in the first step into a hydrothermal reaction kettle, and reacting for a period of time at a constant temperature of 150-180 ℃;
thirdly, after the solution which is completely reacted is cooled and precipitated, filtering, washing and drying to obtain a pink precursor;
and fourthly, heating the precursor obtained in the third step to a set temperature in the air for thermal decomposition for a period of time to obtain a black product.
Further, in the first step, the volume ratio of water to ethanol is 1: 0.7-1.4, wherein the volume ratio of the total volume of water and ethanol to the volume of ethanolamine is 1: 60-170, the concentration of nickel nitrate hexahydrate is 0.02-0.08 mol/L, the concentration of cobalt nitrate hexahydrate is 0.08-0.16 mol/L, and the concentration of polyvinylpyrrolidone is 0.05-0.25 mol/L.
Further, in the second step, the reaction time is 5-10 h at constant temperature.
Further, in the third step, washing is to wash with deionized water and absolute ethyl alcohol for 3-5 times respectively, and the drying set temperature is 70-90 ℃.
Further, in the fourth step, the precursor is placed into a tube furnace, the heating rate is 2-5 ℃/min, the temperature is increased to 400-500 ℃, and the temperature is kept for 2-4 hours.
Compared with the prior art, the invention has the beneficial effects that:
(1) the uniform NiCo can be prepared by using low-cost water, ethanol and a small amount of ethanolamine as a reaction solvent system and simply regulating and controlling the solvent components and the dosage of a surfactant2O4The product of the porous nano sheet has regular appearance, high dispersity, rich pores, large specific surface area and many active sites;
(2) NiCo prepared by the method2O4The porous nanosheet used as the lithium ion battery cathode material has excellent electrochemical performance; can be used forThe reverse specific capacity is high, the cycle life is long, and the reverse capacity is as high as 695mAh/g after the battery is cycled for 1000 times under the current density of 0.5A/g;
(3) the material preparation process is simple, only the composition of the solution needs to be regulated and the pH value of the solution does not need to be regulated, the controllability is high, and the material is suitable for batch preparation; the solvent thermal reaction condition is mild and is lower than 200 ℃, and the requirement on equipment safety is low; no pollutant is generated, and the environment is protected; the product has strong consistency and good industrial application prospect.
Drawings
The invention is further elucidated with reference to the drawings and the embodiments.
FIG. 1 is a schematic representation of a NiCo product prepared in accordance with example 1 of the present invention2O4An X-ray diffraction pattern of the porous nanoplatelets;
FIG. 2 is a NiCo product of example 1 of the present invention2O4A scanning electron microscopy image of the porous nanoplatelets;
FIG. 3 is a NiCo product of example 1 of the present invention2O4Transmission electron microscopy of porous nanoplatelets;
FIG. 4 is a NiCo product of example 1 of the present invention2O4A rate performance graph of the porous nanosheets;
FIG. 5 is a NiCo product of example 1 of the present invention2O4A cycle performance profile of porous nanoplates;
FIG. 6 is a NiCo product of example 1 of the present invention2O4Scanning electron microscopy of forebody.
Detailed Description
Example 1
2mmol of nickel nitrate hexahydrate, 4mmol of cobalt nitrate hexahydrate and 0.5g of polyvinylpyrrolidone are sequentially added into a mixed solution of 18ml of water, 16ml of ethanol and 0.2ml of ethanolamine, and stirred into a uniform suspension. Then transferring the suspension into a reaction kettle with a polytetrafluoroethylene inner container, and reacting for 10 hours at a constant temperature of 170 ℃. And filtering and collecting precipitates after the reaction is completed, washing the precipitates for 3 times by using deionized water and absolute ethyl alcohol respectively, and drying the precipitates in an oven at 80 ℃ to obtain pink precursor solid powder. Putting the obtained precursor powder into a tube furnace, heating at the speed of 2 ℃/min, and thermally decomposing for 2h at 450 ℃ in the air to obtain a black product.
The button cell assembled by the lithium ion battery cathode material prepared by the invention has the following test method: mixing NiCo2O4Mixing the powder, the SuperP conductive carbon and the polyvinylidene fluoride binder according to a mass ratio of 70:20:10, adding a proper amount of N-methyl pyrrolidone solvent, uniformly stirring, coating on a copper foil, and performing vacuum drying at 80 ℃ to obtain the battery pole piece. The counter electrode is a lithium plate, the diaphragm is a Celgard2400 membrane, and the electrolyte is 1M LiPF6And the/EC + DMC (volume ratio of 1: 1) is assembled into the CR2016 coin cell. Constant-current charging and discharging tests are carried out on a battery CT2001A test system, and the voltage cut-off range is 0.01-3V.
FIG. 1 shows NiCo obtained in example 12O4XRD pattern of the product. As can be seen, the product produced had NiCo2O4Spinel phase structure and high crystallinity.
FIG. 2 shows NiCo obtained in example 12O4Scanning electron microscopy of the product. As can be seen, NiCo is prepared2O4The shape of the porous nanosheet is presented, the pores are rich, and the dispersity is high. The thickness of the nano-sheet is about 80nm, and the diameter is about 1-5 μm.
FIG. 3 shows NiCo obtained in example 12O4Transmission electron microscopy of the product. Further confirms NiCo2O4The porous structure of the nanosheet.
FIG. 4 shows NiCo obtained in example 12O4The product is used as a rate performance diagram of a lithium ion battery cathode material. As can be seen from the figure, the average discharge capacity under the current density of 0.2A/g is up to 1015mAh/g, and the average discharge capacity under the current density of 4A/g is still 400mAh/g, thus showing excellent high rate performance.
FIG. 5 shows NiCo obtained in example 12O4Cycle performance diagram of the negative electrode material. As can be seen, after the product is cycled for 1000 times under the current density of 0.5A/g, the discharge capacity of 695mAh/g still exists, which indicates that the product has excellent cycling stability.
FIG. 6 shows NiCo obtained in example 12O4Before the productScanning electron micrographs of the body. As can be seen from the figure, the precursor obtained by the solvothermal reaction is a regular nanosheet.
Example 2
2mmol of nickel nitrate hexahydrate, 4mmol of cobalt nitrate hexahydrate and 0.2g of polyvinylpyrrolidone are sequentially added into a mixed solution of 18ml of water, 16ml of ethanol and 0.5ml of ethanolamine, and stirred into a uniform suspension. Then transferring the suspension into a reaction kettle with a polytetrafluoroethylene inner container, and reacting for 10 hours at a constant temperature of 170 ℃. And filtering and collecting precipitates after the reaction is completed, washing the precipitates for 3 times by using deionized water and absolute ethyl alcohol respectively, and drying the precipitates in an oven at 80 ℃ to obtain pink precursor solid powder. Putting the obtained precursor powder into a tube furnace, heating at the speed of 2 ℃/min, and thermally decomposing for 2h at 450 ℃ in the air to obtain a black product.
Example 3
1.5mmol of nickel nitrate hexahydrate, 3mmol of cobalt nitrate hexahydrate and 0.1g of polyvinylpyrrolidone are sequentially added into a mixed solution of 16ml of water, 18ml of ethanol and 0.2ml of ethanolamine, and stirred into a uniform suspension. Then transferring the suspension into a reaction kettle with a polytetrafluoroethylene inner container, and reacting for 6 hours at a constant temperature of 180 ℃. And filtering and collecting precipitates after the reaction is completed, washing the precipitates for 3 times by using deionized water and absolute ethyl alcohol respectively, and drying the precipitates in an oven at 80 ℃ to obtain pink precursor solid powder. Putting the obtained precursor powder into a tube furnace, heating at the speed of 3 ℃/min, and thermally decomposing for 2h at the temperature of 500 ℃ in the air to obtain a black product.
Example 4
1mmol of nickel nitrate hexahydrate, 2mmol of cobalt nitrate hexahydrate and 1g of polyvinylpyrrolidone are sequentially added into a mixed solution of 20ml of water, 14ml of ethanol and 0.3ml of ethanolamine, and stirred into a uniform suspension. Then transferring the suspension into a reaction kettle with a polytetrafluoroethylene inner container, and reacting for 9 hours at a constant temperature of 160 ℃. And filtering and collecting precipitates after the reaction is completed, washing the precipitates for 3 times by using deionized water and absolute ethyl alcohol respectively, and drying the precipitates in an oven at 80 ℃ to obtain pink precursor solid powder. Putting the obtained precursor powder into a tube furnace, heating at the speed of 5 ℃/min, and thermally decomposing for 3h at the temperature of 420 ℃ in the air to obtain a black product.
Example 5
1mmol of nickel nitrate hexahydrate, 2mmol of cobalt nitrate hexahydrate and 0.2g of polyvinylpyrrolidone are sequentially added into a mixed solution of 14ml of water, 20ml of ethanol and 0.4ml of ethanolamine, and stirred into a uniform suspension. Then transferring the suspension into a reaction kettle with a polytetrafluoroethylene inner container, and reacting for 10 hours at a constant temperature of 150 ℃. And filtering and collecting precipitates after the reaction is completed, washing the precipitates for 3 times by using deionized water and absolute ethyl alcohol respectively, and drying the precipitates in an oven at 80 ℃ to obtain pink precursor solid powder. Putting the obtained precursor powder into a tube furnace, heating at the speed of 4 ℃/min, and thermally decomposing for 4h at the temperature of 470 ℃ in the air to obtain a black product.
By verifying the products obtained in the embodiments 2 to 5, the technical effects to be achieved by the present application can be achieved, which shows that the NiCo can be successfully prepared by using cobalt nitrate hexahydrate and nickel nitrate hexahydrate as reaction raw materials, polyvinylpyrrolidone as a surfactant in a solvent system of water, ethanol and a small amount of ethanolamine, and performing solvothermal reaction and thermal decomposition of a precursor2O4The porous nanosheet is used as a lithium ion battery negative electrode material, and shows high specific capacity and excellent cycling stability.
In summary, the lithium ion battery cathode material NiCo of the invention2O4The preparation method of the porous nanosheet has the advantages that the cost of the reaction solvent required by material preparation is low, and the reaction solvent is convenient and easy to obtain; the solvothermal reaction condition is mild, and the requirement on equipment is low; the process is simple and the controllability is strong; no pollutant is generated, and the environment is protected; the product has high consistency, long material cycle life and good industrial application prospect.
The examples disclosed herein are merely illustrative of the technical solutions of the present invention and should not be construed as limiting the content of the present invention, and variations of the present invention by those skilled in the art are still within the scope of the present invention.
Claims (6)
1. Lithium ion battery cathode material NiCo2O4The preparation method of the porous nanosheet is characterized by comprising the following steps: cobalt nitrate hexahydrate and nickel nitrate hexahydrate are used as reaction raw materials, water, ethanol and a very small amount of ethanolamine are used as solvent systems, and polyvinylpyrrolidone is usedIs used as a surfactant, and the NiCo serving as the negative electrode material of the lithium ion battery is prepared by a solvothermal method and thermal decomposition of a precursor2O4Porous nanoplatelets.
2. The lithium ion battery anode material NiCo of claim 12O4The preparation method of the porous nanosheet comprises the following specific steps:
accurately weighing nickel nitrate hexahydrate, cobalt nitrate hexahydrate and polyvinylpyrrolidone according to the amount, sequentially adding the nickel nitrate hexahydrate, the cobalt nitrate hexahydrate and the polyvinylpyrrolidone into a mixed solution of water, ethanol and ethanolamine, and stirring to obtain a uniform suspension;
secondly, transferring the suspension obtained in the first step into a hydrothermal reaction kettle, and reacting for a period of time at a constant temperature of 150-180 ℃;
thirdly, after the solution which is completely reacted is cooled and precipitated, filtering, washing and drying to obtain a pink precursor;
and fourthly, heating the precursor obtained in the third step to a set temperature in the air for thermal decomposition for a period of time to obtain a black product.
3. The lithium ion battery anode material NiCo of claim 22O4The preparation method of the porous nanosheet is characterized by comprising the following steps: in the first step, the volume ratio of water to ethanol is 1: 0.7-1.4, wherein the volume ratio of the total volume of water and ethanol to the volume of ethanolamine is 1: 60-170, the concentration of nickel nitrate hexahydrate is 0.02-0.08 mol/L, the concentration of cobalt nitrate hexahydrate is 0.08-0.16 mol/L, and the concentration of polyvinylpyrrolidone is 0.05-0.25 mol/L.
4. The lithium ion battery anode material NiCo of claim 22O4The preparation method of the porous nanosheet is characterized by comprising the following steps: in the second step, the reaction time is 5-10 h at constant temperature.
5. The lithium ion battery anode material NiCo of claim 22O4The preparation method of the porous nanosheet is characterized by comprising the following steps: in the third step, washing refers to deionized water and anhydrous waterWashing with ethanol for 3-5 times respectively, and drying at a set temperature of 70-90 ℃.
6. The lithium ion battery anode material NiCo of claim 22O4The preparation method of the porous nanosheet is characterized by comprising the following steps: in the fourth step, the precursor is put into a tube furnace, the heating rate is 2-5 ℃/min, the temperature is raised to 400-500 ℃, and the temperature is kept for 2-4 hours.
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| CN112758990A (en) * | 2020-11-09 | 2021-05-07 | 中国科学院合肥物质科学研究院 | Preparation method and application of transition metal nitride lithium ion battery cathode material |
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