CN111916729A - Ternary lithium nickel cobalt manganese oxide material and preparation method and application thereof - Google Patents
Ternary lithium nickel cobalt manganese oxide material and preparation method and application thereof Download PDFInfo
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- CN111916729A CN111916729A CN202010783113.9A CN202010783113A CN111916729A CN 111916729 A CN111916729 A CN 111916729A CN 202010783113 A CN202010783113 A CN 202010783113A CN 111916729 A CN111916729 A CN 111916729A
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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
- H01M4/48—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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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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- 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
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
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- 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
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Abstract
The invention discloses a ternary nickel cobalt lithium manganate material and a preparation method thereof, wherein cobalt manganese oxide is used as a template and a cobalt source and a manganese source, nickel acetate hexahydrate and lithium carbonate are used as a nickel source and a lithium source, deionized water is used as a solvent, cobalt manganese oxalate is synthesized by a hydrothermal method, then a cobalt manganese oxide precursor is obtained after calcination in air, finally, the nickel source and the lithium source are added and uniformly mixed through ball milling, and then oxygen is introduced to sinter in a tubular furnace to obtain the ternary nickel cobalt lithium manganate material. The ternary nickel cobalt lithium manganate material has larger specific surface area, is beneficial to full contact and ion transmission of electrolyte and active substances, increases the active sites of reaction, overcomes the defect of poor high-current discharge capacity of the ternary nickel cobalt lithium manganate material, greatly improves the electrochemical performance and enhances the cycle stability and the rate capability when being used as the anode material of a lithium ion battery.
Description
Technical Field
The invention relates to the field of lithium ion battery anode materials, in particular to a ternary nickel cobalt lithium manganate material and a preparation method and application thereof.
Background
With the rapid development of economy, people have increasingly demanded energy. Due to the non-renewable nature of fossil energy and environmental pollution, there is an urgent need for new green energy sources. Lithium ion batteries have attracted much attention as the main power source of portable electronic products (such as notebook computers, mobile phones, communication devices, cameras, etc.). At present, the anode materials of lithium ion batteries mainly comprise lithium nickelate, olivine lithium iron phosphate, spinel lithium manganate and lithium cobaltate, but the traditional anode materials of lithium ion batteries are gradually eliminated due to a series of defects of difficult synthesis conditions, poor thermal stability, high price and the like, so that the search for novel anode materials with high capacity, high multiplying power and long cycle life becomes a research hotspot in recent years. The lithium nickel cobalt manganese oxide of the ternary transition metal oxide composite material combines the advantages of lithium cobaltate, lithium manganese oxide and lithium nickelate due to synergistic effect, and the capacity and the cycling stability of the lithium nickel cobalt manganese oxide composite material are superior to those of a single component, so that the lithium nickel cobalt manganese oxide composite material becomes an optimal substitute material. However, the ternary lithium nickel cobalt manganese oxide material also has the defects of poor thermal stability, cation mixed discharge, poor high-current discharge capacity and the like caused by the increase of the nickel content. The ternary nickel cobalt lithium manganate material prepared by the oxalic acid coprecipitation method and the high-temperature solid phase method has a large specific surface area, is beneficial to full contact of an electrode material and an electrolyte, and reduces diffusion resistance of charges or ions between the electrolyte and the electrode material, so that the electrochemical energy storage performance of the electrode material is improved.
Disclosure of Invention
The invention aims to provide a ternary nickel cobalt lithium manganate material, a preparation method and application thereof, and mainly solves the technical problems of poor cycle stability and poor large-current discharge capacity of the conventional ternary nickel cobalt lithium manganate material in the application of a lithium battery anode material.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a ternary nickel cobalt lithium manganate material comprises the following steps:
(1) placing oxalic acid in deionized water for magnetic stirring to obtain an oxalic acid solution, and then placing the oxalic acid solution in an ultrasonic device for ultrasonic dispersion;
(2) adding cobalt acetate and manganese acetate into deionized water to obtain a cobalt acetate solution and a manganese acetate solution, and respectively stirring the two solutions until the two solutions are clear;
(3) fixing the oxalic acid solution treated in the step (1) in an oil bath pan, and respectively dropwise adding the two solutions obtained in the step (2) into the oxalic acid solution to carry out hydrothermal reaction;
(4) putting the product obtained in the step (3) into a drying oven for drying, putting the dried product into a rapid heating and cooling furnace for annealing, and cooling to obtain a cobalt-manganese oxide precursor;
(5) placing the product obtained in the step (4), nickel acetate and lithium carbonate in a ball milling tank for high-speed ball milling to mix materials;
(6) and (5) placing the product obtained in the step (5) into a rapid temperature rising and falling furnace for annealing, then introducing oxygen into the rapid temperature rising and falling furnace as reaction gas, and heating at high temperature to obtain the ternary nickel cobalt lithium manganate material.
Preferably, in the step (1), the magnetic stirring time is 20-30min, the stirring speed is 200-300r/min, and the oxalic acid solution is placed in an ultrasonic device for ultrasonic dispersion for 10 min.
Preferably, in the step (2), cobalt acetate and manganese acetate are added into deionized water in a molar ratio of 1:1, and the mixture is stirred until the mixture is clear, so that the total concentration of transition metal cobalt ions and manganese ions in the obtained acetate solution is 0.1 mol/L.
Preferably, in the step (3), the oil bath time is 1-2 h, and the oil bath temperature is 60-80 ℃.
Preferably, in the step (4), the specific drying conditions in the drying oven are as follows, the drying temperature is 60-80 ℃, and the drying time is 10-12 hours, so as to obtain the cobalt manganese oxalate.
Preferably, in the step (4), the calcination temperature in the rapid heating and cooling furnace is 450-550 ℃, the heating rate is 3-5 ℃/min, the heat preservation time is 6-8 h, and the calcination is carried out in the air.
Preferably, in the step (5), the molar ratio of nickel acetate to lithium carbonate is (1-1.05): (0.83-0.88), the rotation speed of ball milling is 300-500 r/min, and the ball milling time is 2-3 h.
Preferably, in the step (6), the calcination temperature during high-temperature heating is 800-850 ℃, the heating rate is 3-5 ℃/min, the heat preservation time is 10-12 h, and the oxygen flow is 30-50 cc.
Preferably, the ternary lithium nickel cobalt manganese oxide material is prepared according to the method.
Preferably, the ternary nickel cobalt lithium manganate material is used for preparing the lithium ion battery cathode material.
Compared with the prior art, the invention has the beneficial effects that:
1. when the cobalt manganese oxalate is prepared by the hydrothermal method, nickel, cobalt and manganese are not precipitated together, but a nickel source is added during the subsequent ball milling, so that the problem of uneven precipitation of nickel, cobalt and manganese in the oxalic acid is successfully solved.
2. The invention adopts the ball-milling mixed material to improve the dispersity of the material and reduce the granularity, thereby improving the formability and the sinterability of the ternary nickel cobalt lithium manganate, and the ball-milling mixed material can ensure that all components are mixed more uniformly, and because the granularity of the material is thinned, impurities in powder particles are exposed, thereby being beneficial to subsequent purification.
3. The invention adopts acetate as raw material and oxalic acid as precipitant, so the cost is low.
4. The method adopts a hydrothermal method and a high-temperature solid-phase method for synthesis, controls the morphology by regulating and controlling the concentration of oxalic acid, the reaction temperature, the reaction time and the calcination temperature, and has simple operation and controllable process.
5. The product synthesized by the method has larger specific surface area, is beneficial to full contact of electrolyte and active substances, increases the active sites of reaction, overcomes the defect of poor high-current discharge capability of the ternary nickel cobalt lithium manganate material, greatly improves the electrochemical performance of the lithium ion battery when used as the anode material of the lithium ion battery, greatly enhances the cycle stability of the lithium ion battery, and is beneficial to realizing commercial application.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 shows ternary lithium nickel cobalt manganese oxide (LiNi) in example0.6Co0.2Mn0.2O2) XRD pattern of (a);
FIG. 2 shows ternary lithium nickel cobalt manganese oxide (LiNi) in example0.6Co0.2Mn0.2O2) Scanning electron microscope pictures under low power;
FIG. 3 shows ternary lithium nickel cobalt manganese oxide (LiNi) in example0.6Co0.2Mn0.2O2) A transmission electron microscope image;
FIG. 4 shows ternary lithium nickel cobalt manganese oxide (LiNi) in example0.6Co0.2Mn0.2O2) At 34mA g-1A picture of the cyclic capacity at current density;
FIG. 5 shows ternary lithium nickel cobalt manganese oxide (LiNi) in example0.6Co0.2Mn0.2O2) A graph of rate performance at different current densities;
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
A preparation method of a ternary nickel cobalt lithium manganate material comprises the following steps:
(1) in a stoichiometric ratio n (Co) n (Mn) n (oxalic acid) 1: 1: 2, respectively dissolving 1.5mmol of cobalt acetate, 1.5mmol of manganese acetate and 3mmol of oxalic acid in 15ml of deionized water, 15ml of deionized water and 30ml of deionized water, placing the oxalic acid in the deionized water, carrying out magnetic stirring to obtain an oxalic acid solution, wherein the magnetic stirring time is 30min, and the stirring speed is 250r/min, and then placing the oxalic acid solution in an ultrasonic device for ultrasonic dispersion for 10 min;
(2) respectively dissolving cobalt acetate and manganese acetate in deionized water to obtain a cobalt acetate solution and a manganese acetate solution, and respectively stirring the two solutions until the two solutions are clear, wherein the total concentration of transition metal cobalt ions and manganese ions in the obtained acetate solution is 0.1 mol/L;
(3) fixing the oxalic acid solution treated in the step (1) in an oil bath pan, heating the oil bath pan to 80 ℃, stirring for half an hour, wherein the oil bath time is 2 hours, firstly dropwise adding 8ml of cobalt acetate solution into the oxalic acid solution, stirring for one hour to react to generate rod-shaped cobalt oxalate, and then dropwise adding the remaining 7ml of cobalt acetate and 15ml of manganese acetate solution into the oxalic acid and cobalt oxalate solution to react for 2 hours under magnetic stirring;
(4) putting the pink solution obtained in the step (3) into a drying oven to be dried for 12 hours at the temperature of 80 ℃ to obtain cobalt manganese oxalate, manually grinding the dried pink powder for 1 hour, then putting the pink powder into a rapid heating and cooling furnace to be annealed for 6 hours at the temperature of 450 ℃ in the air, wherein the heating rate is 3 ℃/min, and cooling to obtain a cobalt manganese oxide precursor;
(5) then carrying out high-speed ball milling and mixing on 0.211g of cobalt manganese oxide precursor, 1.058g of nickel acetate and 0.262g of lithium carbonate for 2 hours, wherein the rotating speed of the ball milling is 400r/min, and the time of the ball milling is 2 hours;
(6) and (3) sintering the powder obtained in the step (5) in a rapid heating and cooling furnace at 450 ℃ for 6h, cooling to room temperature, taking out, grinding for 1h, sintering in the rapid heating and cooling furnace at 700 ℃ for 3h, and sintering at 850 ℃ for 12h, wherein the heating rate is 3 ℃/min, and the oxygen flow is 40cc, so as to obtain the ternary lithium nickel cobalt manganese oxide material.
The obtained sample was analyzed by X-ray diffraction analyzer model D/max-2500 of Pasacaceae, Netherlands, and the obtained results are shown in FIG. 1. Using SU of Hitachi Ltd8020A sample observed by scanning electron microscope, ternary lithium nickel cobalt manganese oxide (LiNi)0.6Co0.2Mn0.2O2) The material morphology is shown in fig. 2. The size of the particles is mainly around 300-500nm, as shown in FIG. 3. Mixing ternary nickel cobalt lithium manganate (LiNi)0.6Co0.2Mn0.2O2) The materials are assembled into button cells for electrochemical performance test. The voltage range of the cycle performance test is 2.7-4.3V, and the current density is 34mA g-1The first discharge specific capacity can reach 170mAh g-1Above, after circulating for 100 times, the specific capacity can reach 150mAh g-1The cycle performance results are shown in FIG. 4. FIG. 5 shows ternary lithium nickel cobalt manganese oxide (LiNi)0.6Co0.2Mn0.2O2) Graph of rate performance at different current densities.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the present invention as defined in the accompanying claims.
Claims (10)
1. The preparation method of the ternary nickel cobalt lithium manganate material is characterized by comprising the following steps of:
(1) placing oxalic acid in deionized water for magnetic stirring to obtain an oxalic acid solution, and then placing the oxalic acid solution in an ultrasonic device for ultrasonic dispersion;
(2) respectively adding cobalt acetate and manganese acetate into deionized water to obtain a cobalt acetate solution and a manganese acetate solution, and respectively stirring the two solutions until the two solutions are clear;
(3) fixing the oxalic acid solution treated in the step (1) in an oil bath pan, and respectively dropwise adding the two solutions obtained in the step (2) into the oxalic acid solution to carry out hydrothermal reaction;
(4) putting the product obtained in the step (3) into a drying oven for drying, putting the dried product into a rapid heating and cooling furnace for annealing, and cooling to obtain a cobalt-manganese oxide precursor;
(5) placing the product obtained in the step (4), nickel acetate and lithium carbonate in a ball milling tank for high-speed ball milling to mix materials;
(6) and (5) placing the product obtained in the step (5) into a rapid temperature rising and falling furnace for annealing, then introducing oxygen into the rapid temperature rising and falling furnace as reaction gas, and heating at high temperature to obtain the ternary nickel cobalt lithium manganate material.
2. The method for preparing the ternary lithium nickel cobalt manganese oxide material according to claim 1, wherein the method comprises the following steps: in the step (1), the magnetic stirring time is 20-30min, the stirring speed is 200-300r/min, and the oxalic acid solution is placed in an ultrasonic device for ultrasonic dispersion for 10 min.
3. The method for preparing the ternary lithium nickel cobalt manganese oxide material according to claim 1, wherein the method comprises the following steps: in the step (2), cobalt acetate and manganese acetate are added into deionized water according to the molar ratio of 1:1, and the mixture is stirred until the mixture is clear, so that the total concentration of transition metal cobalt and manganese ions in the obtained acetate solution is 0.1 mol/L.
4. The method for preparing the ternary lithium nickel cobalt manganese oxide material according to claim 1, wherein the method comprises the following steps: in the step (3), the oil bath time is 1-2 h, and the oil bath temperature is 60-80 ℃.
5. The method for preparing the ternary lithium nickel cobalt manganese oxide material according to claim 1, wherein the method comprises the following steps: in the step (4), the specific drying conditions in the drying oven are as follows, the drying temperature is 60-80 ℃, and the drying time is 10-12 h, so that the cobalt manganese oxalate is obtained.
6. The method for preparing the ternary lithium nickel cobalt manganese oxide material according to claim 1, wherein the method comprises the following steps: in the step (4), the calcination temperature in the rapid heating and cooling furnace is 450-550 ℃, the heating rate is 3-5 ℃/min, the heat preservation time is 6-8 h, and the calcination is carried out in the air.
7. The method for preparing the ternary lithium nickel cobalt manganese oxide material according to claim 1, wherein the method comprises the following steps: in the step (5), the molar ratio of the nickel acetate to the lithium carbonate is (1-1.05): (0.83-0.88), the rotation speed of ball milling is 300-500 r/min, and the ball milling time is 2-3 h.
8. The method for preparing the ternary lithium nickel cobalt manganese oxide material according to claim 1, wherein the method comprises the following steps: in the step (6), the calcination temperature during high-temperature heating is 800-850 ℃, the heating rate is 3-5 ℃/min, the heat preservation time is 10-12 h, and the oxygen flow is 30-50 cc.
9. The ternary lithium nickel cobalt manganese oxide material is characterized by being prepared by the preparation method according to any one of claims 1 to 8.
10. The ternary lithium nickel cobalt manganese oxide material of claim 9 is used for preparing a positive electrode material of a lithium ion battery.
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