CN110429254B - Preparation method of lithium ion battery anode material - Google Patents
Preparation method of lithium ion battery anode material Download PDFInfo
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- CN110429254B CN110429254B CN201910696083.5A CN201910696083A CN110429254B CN 110429254 B CN110429254 B CN 110429254B CN 201910696083 A CN201910696083 A CN 201910696083A CN 110429254 B CN110429254 B CN 110429254B
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- 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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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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
- H01M4/48—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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- H—ELECTRICITY
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- 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
- H01M4/525—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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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a lithium ion battery anode material, which comprises the following steps: mixing DMF and water according to the volume ratio of 1: 34-34: 1 to obtain a solvent; adding 1.06-2.12 g of urotropin into every 35mL of solvent, and dissolving the urotropin into the solvent to obtain a solution A; adding nickel salt, cobalt salt and manganese salt into the solution A, and stirring to obtain a solution B; the total atom amount of nickel, cobalt and manganese in each 35mL of the solution A is 0.005 mol; transferring the solution B into a reaction kettle for hydrothermal reaction, and centrifuging the reaction solution after the hydrothermal reaction to obtain carbonate containing nickel, cobalt and manganese; sintering the carbonate at the high temperature of 450-500 ℃ to obtain nickel-cobalt-manganese oxide; mixing the oxide with lithium salt, and sintering at the high temperature of 750-800 ℃ to obtain the lithium-rich manganese-based positive electrode material Li1.2MnxNiyCozO2，x+y+z＝0.8。
Description
Technical Field
The invention relates to a preparation method of a lithium ion battery anode material.
Background
Lithium Ion Batteries (LIBs) are widely used as high-energy and high-power sources for Electric Vehicles (EVs) and as renewable energy storage in smart grids. Among the developed positive electrode materials, lithium-rich manganese-based positive electrode material (LMNCO) xLi2MnO3·(1-x)LiMO2(0<x<1, M ═ Ni, Mn, Co) is attracting attention due to its high capacity, low cost and environmental friendliness. However, the slow diffusion of electrons and lithium ions in LMNCO leads to rapid capacity fade and poor rate capability. Current research has demonstrated that electrochemical properties are closely related to material structure, and therefore rational design and control of the structure and morphology of LMNCO is considered to be an effective way to improve capacity retention and rate performance.
On this basis, the scientific community has been actively striving to develop nano-sized materials and has made great progress in the past few years, such as nanoparticles, nanowires, nanorods, nanoplates and the like, which have short Li due to size reduction+A diffusion path. However, side reactions between nanoscale electrodes/electrolytes are detrimental to structural stability. To address these challenges with nano-sized materials, graded micro/nanomaterials have recently been developed, and graded LMNCO with micro-material structural stability can extend cycle life by avoiding interfacial reactions with electrolytes. However, a single hierarchical structure design may not be sufficient to fully improve the performance of the lithium-rich manganese-based positive electrode material. Recent reports demonstrate that two-dimensional (2D) nanostructures have the advantages of shortening the electron solid-state transport path, increasing the surface area to volume ratio to relieve mechanical strain, and accommodating severe volume expansion, thereby imparting superior cycling stability to the electrode material. Furthermore, 2D structures (nanoplatelets) typically have large exposed surfaces and specifically oriented crystal planes. It has been widely reported that in lithium rich materials, if the nanoplatelet surface exposes the electrochemically active surface, then Li+The rate of intercalation/deintercalation will be significantly enhanced.
The above background disclosure is only for the purpose of assisting understanding of the inventive concept and technical solutions of the present invention, and does not necessarily belong to the prior art of the present patent application, and should not be used for evaluating the novelty and inventive step of the present application in the case that there is no clear evidence that the above content is disclosed before the filing date of the present patent application.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a lithium ion battery anode material, which prepares a lithium-rich manganese-based anode material or other nickel-cobalt-manganese-containing ternary anode materials with excellent performance by a simple synthesis process.
A preparation method of a lithium ion battery anode material comprises the following steps: s1, mixing DMF and water according to the volume ratio of 1: 34-34: 1 to obtain a mixed solution as a solvent; s2, adding the usage amount of 1.06-2.12 g of urotropine into each 35mL of solvent, and dissolving the urotropine into the solvent to obtain a mixed solution A; s3, adding nickel salt, cobalt salt and manganese salt into the mixed solution A, and stirring for at least 1 hour to obtain a mixed solution B; wherein, each 35mL of the mixed solution A contains original nickel, cobalt and manganeseThe total amount of the seed is 0.005 mol; s4, transferring the mixed solution B to a reaction kettle for hydrothermal reaction, and then centrifuging the reaction solution after the hydrothermal reaction to obtain carbonate containing nickel, cobalt and manganese; s5, sintering the carbonate at the high temperature of 450-500 ℃ to obtain nickel-cobalt-manganese oxide; s6, mixing the oxide with lithium salt, and then sintering at the high temperature of 750-800 ℃ to obtain the lithium-rich manganese-based positive electrode material Li1.2MnxNiyCozO2Wherein x + y + z is 0.8.
According to the technical scheme, the lithium-rich manganese-based anode material with the micron-nanometer grading morphology is synthesized by a simple hydrothermal method, the advantages of the micron structure and the nanometer structure are integrated, the lithium-rich manganese-based anode material with the good rate capability and the stability is obtained, and the lithium-rich manganese-based anode material has a more stable structure during circulation.
Preferably, when the DMF and the water are mixed according to the volume ratio of 4: 5-5: 4 in the step S1, the shape of the lithium-rich manganese-based positive electrode material obtained in the step S6 is a cube shape formed by nanosheets. In the preferred scheme, DMF and water are mixed according to the volume ratio of 4: 5-5: 4 to obtain a cubic lithium-rich manganese-based positive electrode material, the shape not only belongs to a micron-nanometer grading shape, but also is a cubic micron structure formed by nanosheets, and the material with the special shape has the advantages that:
the traditional single nanosheet is not stable enough and is easily eroded by electrolyte; although the structure of the single micro-sphere is stable, the electrolyte cannot be infiltrated, so that Li+Cannot be embedded/extracted. The micron structure formed by the nano sheets in the preferred scheme can combine the advantages of the nano structure and the micron structure to obtain a material with good rate capability and stability; compared with the conventional hierarchical micron structure (micron spheres consisting of nano particles), the cubic nano-micron hierarchical morphology in the preferred scheme has the advantages that lithium ions are easy to be inserted/extracted, and the specific electrochemical active surface can be exposed due to the specific crystal face orientation of the nanosheets, so that the multiplying power is further enhancedThe performance (the capability of lithium ions to be rapidly inserted/extracted) can realize the specific capacity of more than 120mAh/g when the lithium ion battery is charged and discharged at the super-high current of 20.0C.
Further, the nickel salt, the cobalt salt, and the manganese salt added in step S3 are respectively nickel acetate, cobalt acetate, and manganese acetate, or respectively nickel nitrate, cobalt nitrate, and manganese nitrate, or respectively nickel sulfate, cobalt sulfate, and manganese sulfate.
Furthermore, the temperature of the hydrothermal reaction in the step S4 is 155-165 ℃, and the reaction time is 12-24 hours. More preferably, the temperature of the hydrothermal reaction in step S4 is 160 ℃. The hydrothermal reaction temperature is preferably 160 ℃ because DMF may decompose at a temperature exceeding 160 ℃ and may affect the morphology to a certain extent, and therefore the hydrothermal reaction temperature is preferably kept at about 160 ℃.
Furthermore, the lower layer precipitate in the reaction solution after the hydrothermal reaction in step S4 is a carbonate precursor containing nickel, cobalt and manganese.
Further, the lithium salt lithium carbonate or lithium hydroxide used in step S6.
Further, the high-temperature sintering in steps S5 and S6 is performed in an oxygen or air atmosphere, and the sintering rate is 1-2 ℃/min.
Further, when the molar ratio of manganese atoms to nickel atoms to cobalt atoms in 35mL of the mixed solution A in the step S3 is 0.54:0.13:0.13, the lithium-rich manganese-based positive electrode material obtained in the step S6 is Li1.2Mn0.54Ni0.13Co0.13O2。
Drawings
FIG. 1 is a schematic diagram of a process for preparing a cubic lithium-rich manganese-based positive electrode material according to an embodiment of the present invention;
FIG. 2 is a morphology diagram of lithium-rich manganese-based cathode materials with different morphologies obtained by controlling the volume ratio of DMF to water;
FIG. 3 is a diagram of XRD characterization results of carbonates containing Ni, Co and Mn elements obtained in an embodiment of the present invention;
fig. 4 is a diagram of XRD characterization results of the lithium-rich manganese-based positive electrode material obtained in an embodiment of the present invention;
fig. 5 is a graph of electrochemical cycle performance of the lithium-rich manganese-based positive electrode material obtained in an embodiment of the present invention.
Detailed Description
The invention is further described with reference to the following figures and detailed description of embodiments.
The specific embodiment of the invention provides a preparation method of a lithium ion battery cathode material, which comprises the following steps of S1-S6:
step S1, mixing DMF and water according to the volume ratio of 1: 34-34: 1 to obtain a mixed solution as a solvent; DMF, i.e., N-dimethylformamide, and water is preferably deionized water.
Step S2, adding the usage amount of 1.06-2.12 g of urotropine into 35mL of solvent, and dissolving the urotropine into the solvent to obtain a mixed solution A; urotropin is referred to as "HMT".
Step S3, adding nickel salt, cobalt salt and manganese salt into the mixed solution A, and stirring for at least 1 hour to obtain a mixed solution B; wherein, the total atom amount of nickel, cobalt and manganese in each 35mL of the mixed solution A is 0.005 mol; the nickel salt, the cobalt salt and the manganese salt are respectively nickel acetate, cobalt acetate and manganese acetate, or are respectively nickel nitrate, cobalt nitrate and manganese nitrate, or are respectively nickel sulfate, cobalt sulfate and manganese sulfate.
And step S4, transferring the mixed solution B into a reaction kettle for hydrothermal reaction, wherein the lower-layer precipitate of the reaction solution is a carbonate precursor containing nickel, cobalt and manganese elements, and centrifuging the reaction solution after the hydrothermal reaction to obtain the carbonate containing the nickel, cobalt and manganese elements. The temperature range of the hydrothermal reaction in the step can be set to 155-165 ℃, the most preferable temperature is 160 ℃, and the reaction time is 12-24 hours.
S5, sintering the carbonate containing the nickel, cobalt and manganese elements obtained in the S4 at the high temperature of 450-500 ℃ to obtain an oxide containing the nickel, cobalt and manganese;
step S6, mixing the oxide with lithium salt, and then sintering at high temperature of 750-800 ℃ to obtain the lithium-rich manganese-based positive electrode material Li1.2MnxNiyCozO2Wherein x + y + z ═0.8. The lithium salt used in this step is lithium carbonate or lithium hydroxide.
The high-temperature sintering in the steps S5 and S6 is carried out in an oxygen or air atmosphere, preferably in an oxygen atmosphere, and the effect is good, and the sintering rate is 1-2 ℃/min.
In the preparation process, the components of the solvent in the step S1 play a crucial role in the morphology of the finally formed material, and when DMF and water are mixed according to the volume ratio of 4: 5-5: 4, the morphology of the lithium-rich manganese-based cathode material obtained in the step S6 is cubic and is formed by nanosheets. For example, fig. 2 exemplarily shows the morphology diagrams of the lithium-rich manganese-based cathode material obtained at three different proportions, where a), d), g) are the morphology diagrams of the lithium-rich manganese-based cathode material obtained at different magnifications when the DMF is water 1:2, b), e), h) are the morphology diagrams of the lithium-rich manganese-based cathode material obtained at different magnifications when the DMF is water 1:1, c), f), i) are the morphology diagrams of the lithium-rich manganese-based cathode material obtained at different magnifications when the DMF is water 2: 1. The appearance of the group of lithium-rich manganese-based positive electrode materials of b), e) and h) is a cube formed by the nanosheets.
The present invention will be described in detail below with reference to a specific example.
Referring to fig. 1, after DMF and deionized water are mixed according to a volume ratio of 1:1, 35mL of mixed solution is taken, 1.06g of urotropine, i.e. HMT, is dissolved in 35mL of the mixed solution, and is stirred for 30 minutes to obtain a uniform and transparent solution a; thereafter, 0.203g of C was added4H6CoO4·4H2O (99.0%, alatin), 0.202g of C4H6NiO4·4H2O (99.5%, alatin) and 0.836g of C4H6MnO4·4H2O (98.0%, alatin) was added to the solution A, and after stirring for 1 hour, a solution B was obtained and transferred to a 50mL stainless steel autoclave, which was kept at 160 ℃ for 24 hours without shaking or stirring, and then naturally cooled to room temperature. Centrifuging the precipitate, washing with distilled water to remove organic impurities, and drying in an oven at 80 deg.C for 24 hr to obtain carbonate Ni containing nickel, cobalt and manganese elements0.1625Co0.1625Mn0.675CO3(the XRD characterization result is shown in figure 3), the carbonate is firstly treated at 500 ℃ for 5 hours, the heating rate is 1 ℃/min, and after the carbonate is cooled to the room temperature, the black powder Ni which is the oxide of the nickel, the cobalt and the manganese is obtained0.1625Co0.1625Mn0.675O; then the oxide is mixed with lithium and calcined for 15h at 750 ℃ to obtain the final lithium-rich manganese-based cathode material Li1.2Mn0.54Ni0.13Co0.13O2The XDR characterization result of the positive electrode material is shown in figure 4, figure 5 is an electrochemical cycle performance diagram of the positive electrode material, the initial specific capacity of 133.4mAh/g is obtained under the condition of the super-large multiplying power of 20.0C, after 1200 cycles, the specific capacity can still be 100.1mAh/g, and the capacity retention rate is 75%. The positive electrode material prepared by the method has excellent rate performance.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several equivalent substitutions or obvious modifications can be made without departing from the spirit of the invention, and all the properties or uses are considered to be within the scope of the invention.
Claims (9)
1. A preparation method of a lithium ion battery anode material is characterized by comprising the following steps:
s1, mixing DMF and water according to the volume ratio of 1: 2-2: 1 to obtain a mixed solution as a solvent;
s2, adding the usage amount of 1.06-2.12 g of urotropine into each 35mL of solvent, and dissolving the urotropine into the solvent to obtain a mixed solution A;
s3, adding nickel salt, cobalt salt and manganese salt into the mixed solution A, and stirring for at least 1 hour to obtain a mixed solution B; wherein, the total atom amount of nickel, cobalt and manganese in each 35mL of the mixed solution B is 0.005 mol;
s4, transferring the mixed solution B to a reaction kettle for hydrothermal reaction, and then centrifuging the reaction solution after the hydrothermal reaction to obtain carbonate containing nickel, cobalt and manganese;
s5, sintering the carbonate at the high temperature of 450-500 ℃ to obtain nickel-cobalt-manganese oxide;
s6, mixing the oxide with lithium salt, and then sintering at the high temperature of 750-800 ℃ to obtain the lithium-rich manganese-based positive electrode material Li1.2MnxNiyCozO2Wherein x + y + z is 0.8.
2. The preparation method of the positive electrode material of the lithium ion battery as claimed in claim 1, wherein in the step S1, when the DMF and the water are mixed according to the volume ratio of 4: 5-5: 4, the shape of the lithium-rich manganese-based positive electrode material obtained in the step S6 is a cube shape formed by nanosheets.
3. The method for preparing the positive electrode material of the lithium ion battery according to claim 1, wherein the nickel salt, the cobalt salt and the manganese salt added in the step S3 are respectively nickel acetate, cobalt acetate and manganese acetate, or respectively nickel nitrate, cobalt nitrate and manganese nitrate, or respectively nickel sulfate, cobalt sulfate and manganese sulfate.
4. The method for preparing the positive electrode material of the lithium ion battery according to claim 1, wherein the hydrothermal reaction temperature in the step S4 is 155-165 ℃, and the reaction time is 12-24 hours.
5. The method for preparing a positive electrode material for a lithium ion battery according to claim 4, wherein the temperature of the hydrothermal reaction in step S4 is 160 ℃.
6. The method for preparing the positive electrode material of the lithium ion battery according to claim 1, wherein the lower layer precipitate in the reaction solution after the hydrothermal reaction in step S4 is a carbonate precursor containing nickel, cobalt and manganese.
7. The method for preparing a positive electrode material for a lithium ion battery according to claim 1, wherein the lithium salt used in step S6 is lithium carbonate or lithium hydroxide.
8. The method for preparing a positive electrode material for a lithium ion battery according to claim 1, wherein the high-temperature sintering in steps S5 and S6 is performed in an oxygen or air atmosphere, and the temperature rise rate during sintering is 1-2 ℃/min.
9. The method for preparing the positive electrode material of the lithium ion battery according to claim 1, wherein in the step S3, when the molar ratio of manganese atoms to nickel atoms to cobalt atoms in each 35mL of the mixed solution B is 0.54:0.13:0.13, the lithium-rich manganese-based positive electrode material obtained in the step S6 is Li1.2Mn0.54Ni0.13Co0.13O2。
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