CN114068914A - Lithium cobaltate positive electrode material and preparation method thereof - Google Patents
Lithium cobaltate positive electrode material and preparation method thereof Download PDFInfo
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Abstract
A lithium cobaltate positive electrode material has a chemical formula of LiCo1‑xMxO2Wherein x is more than or equal to 0 and less than or equal to 0.3, and M is one of Ni, Mn, Co and Mg. The method comprises the following steps: uniformly stirring cobalt salt, M salt, ammonium fluoride, urea and deionized water, pouring into a high-pressure hydrothermal kettle, cooling to room temperature, separating to obtain powder, and drying to obtain CoM LDHs powder; placing the obtained powder and a lithium source in a ball milling tank, uniformly mixing, then flatly distributing in a sagger, uniformly cutting into blocks, placing in a muffle furnace, sintering, continuously introducing air in the sintering process, cooling a sample to room temperature, crushing and sieving to obtain LiCo1‑xNixO2And (3) a positive electrode material. The method is simple, efficient, mild in condition and beneficial to industrial large-scale production.
Description
Technical Field
The invention relates to the field of lithium battery anode materials, in particular to a lithium cobaltate anode material and a preparation method thereof.
Background
Lithium cobaltate (LiCoO)2) The high-density carbon nano tube material has the advantages of high compaction density, high theoretical specific capacity (274mAh/g), simple synthesis conditions and the like, and occupies an important position in the high-end 3C electronic product market. Experiments have shown that Li at voltages above 4.2V+Is more than 0.5, resulting in LiCoO2The transition from hexagonal system with electrochemical properties to monoclinic system without electrochemical activity, so the cut-off voltage of the current commercial product is 4.2V. Meanwhile, the charge cut-off voltage is increased, and the material excessively removes Li+Then, LiCoO2The stability of the lattice structure is poor, the oxidability is enhanced, the decomposition of the electrolyte is serious, and the cycling stability of the battery is seriously influenced. To meet the high performance demands of the market, LiCoO is currently used2The research task for positive electrode materials has focused primarily on developing products with higher charge voltages, higher energy densities, longer cycle life, and acceptable safety levels at low cost.
Different methods of synthesis of LiCoO2The positive electrode materials have significant differences in structure and electrochemical properties. LiCoO2The micro-morphology and the particle size of the cathode material have great influence on the electrochemical performance of the lithium ion battery. The Layered Double Hydroxides (LDHs) have unique two-dimensional structures, large specific surface areas, controllable substance compositions and abundant production raw materials, so that the Layered Double Hydroxides (LDHs) can be used as potential raw materials, and simultaneously the synergistic effect between double metals is more favorable for improving the conductivity of the anode material. Meanwhile, the flaky structure reduces the diffusion path of Li < + > to increase the activity of the material, increases the contact area of the anode material and the electrolyte and promotes the ion transfer and diffusion, so that the charge and discharge rate of the battery can be improved, namely the rate capability is better.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a lithium cobaltate positive electrode material prepared by taking LDHs as a template and a method thereof.
The invention is realized by the following technical scheme.
A lithium cobaltate positive electrode material is characterized in that the chemical formula of the positive electrode material is LiCo1-xMxO2Wherein x is more than or equal to 0 and less than or equal to 0.3, and M is one of Ni, Mn, Co and Mg.
The preparation method of the lithium cobaltate positive electrode material is characterized by comprising the following steps of:
(1) preparation of CoM LDHs: uniformly stirring cobalt salt, M salt, ammonium fluoride, urea and deionized water, pouring into a high-pressure hydrothermal kettle, setting the temperature to be 120-160 ℃, preserving the heat for 4-8 h, cooling to room temperature, separating to obtain powder, and drying to obtain CoM LDHs (layered Co and M hydroxide) powder;
(2) preparation of LiCo1-xNixO2A positive electrode material: placing the powder obtained in the step (1) and a lithium source in a ball milling tank, uniformly mixing, then flatly distributing in a sagger, uniformly cutting into blocks, placing in a muffle furnace, heating to 1000-1050 ℃ at a heating rate of 5-10 ℃/min, keeping the temperature for 8-10 h, continuously introducing air in the sintering process, cooling a sample to room temperature, crushing and sieving to obtain LiCo1-xNixO2And (3) a positive electrode material.
Further, in the step (1), the cobalt salt is cobalt nitrate, and the M salt is nitric acid M.
Further, in the step (1), the molar ratio of the cobalt salt, the M salt, the ammonium fluoride and the urea is 0.7-1.0: 0-0.3: 4: 10.
Further, in the step (1), the deionized water is 2/3 of the volume of the hydrothermal kettle.
Further, in the step (1), stirring is carried out for 20-30 min at room temperature.
Further, in the step (1), a centrifugal machine is adopted for separation, the rotating speed of the centrifugal machine is set to be 5000-8000 rad/min, and the time is 5-8 min.
Further, in the step (1), the centrifugally collected powder is washed 3-5 times with deionized water and absolute ethyl alcohol respectively and then dried.
Further, in the step (1), a vacuum drying oven is adopted for drying, the temperature is set to be 60-80 ℃, and the drying time is 8-10 hours.
Further, in the step (2), the lithium source is lithium carbonate, and the powder and the lithium source are mixed according to the ratio of lithium to cobalt metal of 1.03-1.07.
Further, in the step (2), the rotating speed of the ball milling tank is 300rad/min, and ball milling is carried out for 1-1.5 h; the powder, lithium source were cut evenly into 4 x 4 grids in a sagger; the crushing process comprises the steps of firstly adopting a mortar for coarse crushing, then pouring the crushed materials into a universal crusher for crushing, wherein the rotating speed is 25000r/min, and the crushing time is 15-30 s; the crushed sample is poured into a 325-mesh screen for sieving treatment.
The invention has the beneficial technical effects that:
(1) the lithium cobaltate prepared by the method has high purity, no impurity phase and no great damage to a lattice structure;
(2) the hydrothermal method provided by the invention for preparing the flaky cobalt salt raw material is more beneficial to the bulk phase doping of elements, the preparation conditions are mild, and the effect is obvious;
(3) the LiCoO with the sheet structure provided by the invention2The preparation method of the cathode material effectively reduces Li+The diffusion path increases the contact area of the anode material and the electrolyte, is beneficial to ion transfer and diffusion, and improves the multiplying power performance;
(4) the invention provides a method for preparing a lithium cobaltate positive electrode material by taking LDHs as a template, which is simple, efficient, mild in condition and beneficial to industrial large-scale production.
Drawings
Fig. 1 is an XRD pattern of the prepared cathode material.
Fig. 2 is a charge-discharge polarization curve diagram of the prepared anode material at normal temperature.
FIG. 3 is a charge-discharge polarization curve diagram of the prepared anode material at high temperature.
Fig. 4 is a cycle curve diagram of the prepared cathode material at high temperature.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention utilizes a hydrothermal method to prepare a layered bimetal raw material, provides cobalt salt, introduces M metal element, improves the conductivity of an electrode material, stabilizes a lithium cobaltate lattice structure, and adopts a sheet structurePreparation of sheet LiCoO for template by high temperature calcination method2Effectively reduce Li+The diffusion path increases the activity of the material, increases the contact area between the anode material and the electrolyte, and promotes the ion transfer and diffusion, thereby improving the charge and discharge rate of the battery, namely improving the rate capability, and being more beneficial to LiCoO under high voltage2And the electrochemical performance is improved.
Example 1
A lithium cobaltate cathode material with chemical formula of LiCo0.7Ni0.3O2M is a Ni element.
Preparing a NiCo LDHs positive electrode material:
weighing 0.7mmol of cobalt nitrate, 0.3mmol of nickel nitrate, 4mmol of ammonium fluoride and 10mmol of urea, adding 30mL of deionized water (2/3 of the volume of a hydrothermal kettle), stirring for 30min at room temperature, pouring into a high-pressure hydrothermal kettle, placing the high-pressure hydrothermal kettle in an oven, setting the temperature of the oven at 130 ℃, keeping the temperature for 6h, cooling the high-pressure reaction kettle to room temperature, separating powder by using a centrifugal machine, setting the rotating speed of the centrifugal machine at 5000rad/min for 8min, washing for 3 times by using the deionized water and absolute ethyl alcohol respectively, placing in a vacuum drying oven at 60 ℃, and drying for 10h to obtain NiCo LDHs;
LiCo8.5Ni1.5O2preparing a positive electrode material:
100.00g of NiCo LDHs powder and 47.14g of lithium carbonate (the ratio of lithium to cobalt is 1.03) are placed in a ball milling tank to be mixed, the rotating speed is set to 300rad/min, the ball milling time is 1h, the blending powder is uniformly and flatly distributed in a sagger, the uniform blocks (cut into 4 x 4 grids) are placed in a muffle furnace after being uniformly cut into blocks, the temperature is raised to 1030 ℃ at the heating rate of 7 ℃/min and is kept for 8h, an oxygen source is continuously introduced during the sintering process, after a sample is cooled to room temperature, the sample is coarsely crushed by the mortar and is poured into a universal crusher at the rotating speed of 25000r/min, the crushed sample is poured into a 325-mesh screen for sieving after being crushed for 15s, and the sieved sample is collected and named as LCN.
Example 2
A lithium cobaltate cathode material with chemical formula of LiCo0.85Mn0.15O2And M is Mn element.
Preparing a CoMnLDHs anode material:
weighing 0.85mmol of cobalt nitrate, 0.15mmol of manganese nitrate, 4mmol of ammonium fluoride and 10mmol of urea, adding 30mL of deionized water, stirring at room temperature for 20min, pouring into a high-pressure hydrothermal kettle, placing the high-pressure hydrothermal kettle in an oven, setting the temperature of the oven to be 120 ℃, keeping the temperature for 8h, cooling the high-pressure reaction kettle to room temperature, separating powder by using a centrifugal machine, setting the rotating speed of the centrifugal machine to be 7000rad/min, setting the time to be 7min, cleaning by using deionized water and absolute ethyl alcohol for 3 times respectively, placing in a vacuum drying oven to be 80 ℃, and drying for 8h to obtain CoMn LDHs;
LiCo8.5Mn1.5O2preparing a positive electrode material:
100.00g of CoMnLDHs powder and 52.64g of lithium carbonate (the ratio of lithium to cobalt is 1.05) are placed in a ball milling tank to be mixed, the rotating speed is set to 300rad/min, the ball milling time is 1h, the blending powder is uniformly and flatly distributed in a sagger, the uniform blocks are placed in a muffle furnace after being cut into blocks, the temperature is increased to 1000 ℃ at the heating rate of 5 ℃/min, the temperature is kept for 9h, air is continuously introduced in the sintering process to provide an oxygen source, after the sample is cooled to the room temperature, the sample is coarsely ground by a mortar and then poured into a universal grinder, the rotating speed is 25000r/min, after being ground for 30s, the sample is poured into a 325-mesh screen to be screened, the screened sample is collected and named as LCM.
Example 3
A lithium cobaltate cathode material with chemical formula of LiCoO2。
Preparation of CoCoCoLDHs cathode material:
weighing 1.0mmol of cobalt nitrate, 4mmol of ammonium fluoride and 10mmol of urea, adding 30mL of deionized water, stirring at room temperature for 25min, pouring into a high-pressure hydrothermal kettle, placing the high-pressure hydrothermal kettle in an oven, setting the temperature of the oven to 160 ℃, keeping the temperature for 4h, cooling the high-pressure reaction kettle to room temperature, separating powder by using a centrifuge, setting the rotation speed of the centrifuge to 8000rad/min and the time to 5min, washing with deionized water and absolute ethyl alcohol for 3 times respectively, placing in a vacuum drying oven, drying for 8h, and obtaining CoCo LDHs;
LiCoO2preparing a positive electrode material:
100.00g of CoCo LDHs powder and 54.36g of lithium carbonate (the ratio of lithium to cobalt is 1.07) are placed in a ball milling tank to be mixed, the rotating speed is set to 300rad/min, the ball milling time is 1.5h, the blending powder is uniformly and flatly distributed in a sagger, the uniform blocks are placed in a muffle furnace after being cut into blocks, the temperature is increased to 1050 ℃ at the heating rate of 10 ℃/min and is kept for 10h, air is continuously introduced to provide an oxygen source in the sintering process, after the sample is cooled to the room temperature, the sample is coarsely crushed by a mortar and then poured into a universal crusher, the rotating speed is 25000r/min, the sample is crushed for 15s and then poured into a 325-mesh screen to be sieved, the sieved sample is collected and named as LCO.
Experimental example 1 XRD test
XRD tests are carried out on the LCN, LCM and LCO cathode materials prepared in the examples, and the results are shown in figure 1.
Experimental example 1 electrochemical Performance test
The results of normal temperature (25 ℃) charge and discharge test, high temperature (45 ℃) charge and discharge test, and high temperature (45 ℃) cycle test were carried out on the LCN, LCM, and LCO positive electrode materials prepared in the examples, and are shown in fig. 2, 3, and 4.
TABLE 1 discharge capacity under different multiplying power conditions (3.0-4.55V)
As can be seen from table 1, the specific discharge capacity of 0.2C of the LCN cathode material prepared in embodiment 1 reaches 189.0mAh/g, the first efficiency is 90.54%, the ratio of 0.5C/0.2C, 1.0C/0.2C, 2.0C/0.2C is 97.5%, 95.1% and 92.7%, respectively; the specific discharge capacity of 0.2C of the LCM anode material prepared in the embodiment 2 reaches 184.5mAh/g, the ratios of 0.5C/0.2C, 1.0C/0.2C and 2.0C/0.2C are 97.1%, 94.7% and 92.1% respectively; the 0.2C specific discharge capacity of the LCO anode material prepared in the embodiment 3 reaches 187.8mAh/g, the ratios of 0.5C/0.2C, 1.0C/0.2C and 2.0C/0.2C are 97.1%, 94.4% and 91.5% respectively; as can be seen from the test data, the rate performance at 4.55V is excellent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.
Claims (11)
1. A lithium cobaltate positive electrode material is characterized in that the chemical formula of the positive electrode material is LiCo1-xMxO2Wherein x is more than or equal to 0 and less than or equal to 0.3, and M is one of Ni, Mn, Co and Mg.
2. A method for preparing the lithium cobaltate positive electrode material according to claim 1, wherein the method comprises:
(1) preparation of CoM LDHs: uniformly stirring cobalt salt, M salt, ammonium fluoride, urea and deionized water, pouring into a high-pressure hydrothermal kettle, setting the temperature to be 120-160 ℃, preserving the heat for 4-8 hours, cooling to room temperature, separating to obtain powder, and drying to obtain CoM LDHs powder;
(2) preparation of LiCo1-xNixO2A positive electrode material: placing the powder obtained in the step (1) and a lithium source in a ball milling tank, uniformly mixing, then flatly distributing in a sagger, uniformly cutting into blocks, placing in a muffle furnace, heating to 1000-1050 ℃ at a heating rate of 5-10 ℃/min, keeping the temperature for 8-10 h, continuously introducing air in the sintering process, cooling a sample to room temperature, crushing and sieving to obtain LiCo1-xNixO2And (3) a positive electrode material.
3. The method according to claim 2, wherein in the step (1), the cobalt salt is cobalt nitrate and the M salt is M nitrate.
4. The method according to claim 2, wherein in the step (1), the molar ratio of the cobalt salt, the M salt, the ammonium fluoride and the urea is 0.7-1.0: 0-0.3: 4: 10.
5. The method according to claim 2, wherein the deionized water is 2/3 based on the volume of the hydrothermal kettle in the step (1).
6. The preparation method according to claim 2, wherein in the step (1), the stirring condition is stirring at room temperature for 20-30 min.
7. The method according to claim 2, wherein in the step (1), the separation is performed by using a centrifuge, and the rotation speed of the centrifuge is set to 5000-8000 rad/min for 5-8 min.
8. The method according to claim 7, wherein in the step (1), the centrifugally collected powder is washed 3 to 5 times with deionized water and absolute ethanol, respectively, and then dried.
9. The preparation method according to claim 2, wherein in the step (1), the drying is carried out by adopting a vacuum drying oven, the temperature is set to be 60-80 ℃, and the drying time is 8-10 h.
10. The method according to claim 2, wherein in the step (2), the lithium source is lithium carbonate, and the powder is mixed with the lithium source at a lithium to cobalt metal ratio of 1.03 to 1.07.
11. The preparation method according to claim 2, wherein in the step (2), the rotation speed of the ball milling pot is 300rad/min, and the ball milling is carried out for 1-1.5 h; the powder, lithium source were cut evenly into 4 x 4 grids in a sagger; the crushing process comprises the steps of firstly adopting a mortar for coarse crushing, then pouring the crushed materials into a universal crusher for crushing, wherein the rotating speed is 25000r/min, and the crushing time is 15-30 s; the crushed sample is poured into a 325-mesh screen for sieving treatment.
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| CN114702080A (en) * | 2022-03-17 | 2022-07-05 | 宜昌邦普时代新能源有限公司 | Preparation method and application of sea urchin-shaped lithium cobalt oxide |
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