CN112062168B - Lithium ion battery anode material LiNi0.8Co0.1Mn0.1O2And high-pressure solid phase preparation method and application - Google Patents
Lithium ion battery anode material LiNi0.8Co0.1Mn0.1O2And high-pressure solid phase preparation method and application Download PDFInfo
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- 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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- 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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Abstract
The invention belongs to the technical field of lithium ion battery anode materials, and discloses a lithium ion battery anode material LiNi0.8Co0.1Mn0.1O2And a high-pressure solid-phase preparation method and application. The method comprises the following steps: mixing a ternary precursor and a lithium salt according to the stoichiometric ratio of nickel, cobalt, manganese and lithium of 1: uniformly mixing the raw materials in a ratio of 1.05-1.15, and performing ball milling for 2-4 h to obtain a mixed precursor; treating the obtained precursor in an oxygen atmosphere at 350-450 ℃ for 2-4 h, naturally cooling, and grinding to obtain a powder material; and ball-milling the powdery material for 2-4 h again, then treating the powdery material for 6-15 h at 600-750 ℃ in a high-pressure oxygen atmosphere with 1-12 MPa, and naturally cooling to obtain the lithium ion battery anode material. The method has simple process, can shorten the reaction time, reduce the reaction temperature and reduce the production cost by adopting high-pressure atmosphere, and the obtained product has high actual capacity and excellent cycle performance.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery anode materials, and relates to a lithium ion battery anode material LiNi0.8Co0.1Mn0.1O2And a high-pressure solid-phase preparation method and application.
Background
The lithium ion battery has the unique advantages of high working voltage, large specific energy, wide application temperature range, low self-discharge rate, long storage and working life, environmental friendliness and the like, is widely applied to portable electronic products such as mobile phones, notebook computers, digital cameras, video cameras and the like, and is already applied to the fields of electric tools, vehicles (such as electric automobiles and hybrid electric automobiles), aerospace, military, medicine, power storage and the like. However, the lithium ion battery still faces a series of problems of low energy density, time consuming charging, poor safety performance and the like. The positive electrode material is one of the important bottlenecks that limit the performance improvement, especially the energy density, of the lithium ion battery.
Currently, common lithium ion battery positive electrode materials include layered lithium cobaltate, olivine-structured lithium iron phosphate, spinel-structured lithium manganate, a new nickel-cobalt-manganese ternary positive electrode material and the like. Wherein: lithium cobaltate is commercialized at the earliest because of the advantages of excellent cycle performance, high voltage platform and the like, but the price of cobalt is higher, and resources are deficient, so that the development of lithium cobaltate is limited; the lithium iron phosphate has the advantages of stable structure, low price and excellent safety performance, but has the defects of low charge-discharge voltage, low energy density and the like. The nickel-cobalt-manganese ternary material has the characteristics of 3 materials of lithium cobaltate, lithium manganate and lithium nickelate, weakens respective defects to a certain extent, and has the advantages of low cost, small environmental pollution, low toxicity, high energy density, high voltage platform and the like, so that the ternary material quickly becomes an important direction for the development of lithium ion battery materials.
The ternary positive electrode material mainly comprises the following materials: LiNi0.333Co0.333Mn0.333O2(111)、LiNi0.5Co0.2Mn0.3O2(523)、LiNi0.6Co0.2Mn0.2O2(622)、LiNi0.8Co0.1Mn0.1O2(811). As a composite material, the Ni-Co-Mn composite material integrates the advantages of the Ni-Co-Mn composite material and the Ni-Co-Mn composite material through the synergistic effect of the Ni-Co-Mn composite material: LiCoO2Of LiNiO, LiNiO2High specific capacity and LiMnO2The nickel-cobalt-manganese ternary transition metal composite oxide has high safety and low cost, and is widely concerned by researchers. The discharge specific capacity of the anode material is obviously increased along with the increase of the nickel content in the ternary material,but the cycling stability of the material is also greatly reduced and thus the battery life is shortened. In consideration of safety and stability, the current new energy electric vehicles mainly use low-nickel ternary materials such as 111 and 523. However, as the electric automobile requires higher driving range, the capacity requirement of the battery material is higher and higher, and in order to meet the requirement of the market on the energy density of the anode material, the ternary anode material is high in nickel (Ni) in the positive direction>0.6) high specific capacity high nickel material LiNi0.8Co0.1Mn0.1O2(811) More and more attention is being paid to ternary materials. Although high nickel ternary materials have many advantages, they also have disadvantages. Due to high nickel ternary material LiNi0.8Co0.1Mn0.1O2Contains relatively more nickel elements, and the ion radiuses of monovalent lithium ions and divalent nickel ions are approximately the same, so that a cation mixing and discharging phenomenon exists, and free movement of the lithium ions is limited to a certain extent. These also necessarily affect the electrochemical performance of the cell, reducing its cyclability and thermal stability. Meanwhile, high-temperature long-time calcination has huge energy consumption and higher preparation cost of the material.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-pressure solid-phase synthesis LiNi suitable for industrial production0.8Co0.1Mn0.1O2Method for synthesizing LiNi by solid-phase sintering in high-pressure atmosphere0.8Co0.1Mn0.1O2The material can reduce the reaction temperature, shorten the reaction time, inhibit the growth of product particles, and the obtained product has fine particle size, uniform particle size distribution and high electrochemical performance. Meanwhile, the lower calcination temperature and the shorter calcination time can greatly reduce the energy consumption in the preparation process and the preparation cost.
The invention relates to LiNi0.8Co0.1Mn0.1O2The high-pressure solid-phase synthesis method and application of the anode material comprise the following steps:
(1) mixing precursors: mixing a ternary precursor and a lithium salt according to the stoichiometric ratio of nickel, cobalt, manganese and lithium of 1: 1.05-1.15, and performing ball milling to obtain a mixed precursor;
(2) pretreatment: treating the precursor obtained in the step (1) at 350-450 ℃ in an oxygen atmosphere, naturally cooling, and grinding to obtain a powder material;
(3) sintering reaction: ball-milling the powdery material obtained in the step (2), sintering in a high-pressure oxygen atmosphere of 1-12 MPa, and naturally cooling to obtain the LiNi of the lithium ion battery0.8Co0.1Mn0.1O2And (3) a positive electrode material.
The ternary precursor in the step (1) is Ni0.8Co0.1Mn0.1(OH)2(ii) a The lithium salt is lithium carbonate, lithium acetate or lithium hydroxide monohydrate, and the ball milling time is 2-4 hours.
And (3) the pretreatment time in the step (2) is 2-4 h.
In the step (3), the ball milling time is 2-4 hours, the sintering temperature is 600-750 ℃, and the sintering time is 6-15 hours.
The invention also provides LiNi prepared by the preparation method0.8Co0.1Mn0.1O2Positive electrode material
The invention also provides the LiNi0.8Co0.1Mn0.1O2The application of the anode material in a lithium ion battery. Compared with the prior art, the invention has the following advantages:
(1) by using the high-pressure solid-phase synthesis method, the reaction temperature is reduced, the reaction time is shortened, and the production cost is reduced.
(2) LiNi obtained by high pressure solid phase synthesis0.8Co0.1Mn0.1O2The positive electrode material has a single structure and does not contain any impurity phase.
(3) LiNi obtained by high pressure solid phase synthesis0.8Co0.1Mn0.1O2The positive electrode material has the advantages of good crystallization, small crystal grain size, high actual capacity, excellent cycle performance and high reversible capacity. LiNi synthesized by the invention0.8Co0.1Mn0.1O2The test cell is composed of the anode material and the metal lithium sheet, and the rate is 0.1CAnd (4) charging and discharging, wherein when the charging voltage is 3.0-4.3V, the capacity reaches 191mAh/g, and after 50 weeks of circulation, the capacity retention rate still reaches 94.2%.
Drawings
FIG. 1 is an x-ray diffraction pattern of examples 1-4, wherein: (a) is the x-ray diffraction pattern of example 1; (b) the x-ray diffraction pattern of example 2; (c) the x-ray diffraction pattern of example 3; (d) the x-ray diffraction pattern of example 4;
FIG. 2 is an SEM photograph of example 1;
FIG. 3 is a cycle performance curve of example 1; wherein: the charge-discharge multiplying power is 0.1C, and the charge-discharge voltage is 3.0-4.3V;
FIG. 4 is an SEM photograph of example 2;
FIG. 5 is an SEM photograph of example 3;
fig. 6 is a first charge and discharge curve of example 3, wherein: the charge-discharge multiplying power is 0.1C, and the charge-discharge voltage is 3.0-4.4V;
fig. 7 is a first charge-discharge curve of example 4, wherein: the charge and discharge multiplying power is 0.1C, and the charge and discharge voltage is 2.8-4.3V.
Detailed Description
The present invention is further described below with reference to examples, but the embodiments and the scope of the present invention are not limited thereto.
Example 1
The ternary precursor Ni0.8Co0.1Mn0.1(OH)2And LiOH. H2Weighing 40g of O according to the stoichiometric ratio of 1:1.05, uniformly mixing, and carrying out ball milling on a planetary ball mill for 2 hours; then pretreating for 3h at 350 ℃ in an oxygen atmosphere, naturally cooling, and grinding to obtain a powdery product; the powdery product was again ball milled in a planetary ball mill for 4h, in O2Sintering for 6 hours at 600 ℃ under the pressure of 12 MPa in the atmosphere to obtain LiNi0.8Co0.1Mn0.1O2And (3) a positive electrode material.
The XRD spectrum of the sample is shown in a curve (a) in figure 1, and as can be seen, by utilizing the solid phase sintering method, the layered LiNi with a single phase is synthesized0.8Co0.1Mn0.1O2And (3) a positive electrode material. No impurity peak exists in the spectrogram, and the product purity is high. The appearance of the sample is shown in figure 2, the sample is spherical, and the particle size is 3-5 microns. The LiNi0.8Co0.1Mn0.1O2The cycle performance of the anode material is shown in figure 3, and as can be seen from figure 3, when the charge-discharge voltage is 3.0-4.3V and the charge-discharge rate is 0.1C, the discharge capacity of the battery reaches 191mAh/g, and after 50 weeks of cycle, the capacity retention rate still reaches 94.2%, so that the anode material has better cycle performance.
Example 2
The ternary precursor Ni0.8Co0.1Mn0.1(OH)2And Li2CO3Weighing 50g of the raw materials according to the stoichiometric ratio of 1:0.55, uniformly mixing, and carrying out ball milling on a planetary ball mill for 4 hours; then pretreating for 3h at 400 ℃ in an oxygen atmosphere, naturally cooling and grinding to obtain a powdery product; the powdery product was again ball milled in a planetary ball mill for 3h, in O2Sintering for 8 hours at 650 ℃ under the pressure of 10 MPa in the atmosphere to obtain LiNi0.8Co0.1Mn0.1O2And (3) a positive electrode material.
The XRD pattern of the sample is shown in the (b) curve in FIG. 1, and it can be seen from the graph that the sample is free of impurities and is a single-phase layered LiNi0.8Co0.1Mn0.1O2And (3) a positive electrode material. The morphology of the sample is shown in FIG. 4, and the LiNi is0.8Co0.1Mn0.1O2The positive electrode material has a spherical particle morphology, and the sample particle size is about 5 microns.
Example 3
The ternary precursor Ni0.8Co0.1Mn0.1(OH)2And LiCH3COO is weighed to be 40g according to the stoichiometric ratio of 1:1.15, uniformly mixed and ball-milled for 3 hours on a planetary ball mill; then pretreating for 4 hours at 350 ℃ in an oxygen atmosphere, naturally cooling, and grinding to obtain a powdery product; the powdery product was again ball milled in a planetary ball mill for 4h, in O2Sintering at 700 ℃ for 12h under the pressure of 8 MPa in the atmosphere to obtain LiNi0.8Co0.1Mn0.1O2And (3) a positive electrode material.
The XRD pattern of the sample is shown in the (c) curve in FIG. 1, and it can be seen from the graph that the sample is free of impurities and is a single-phase layered LiNi0.8Co0.1Mn0.1O2And (3) a positive electrode material. The morphology of the sample is shown in FIG. 5, which shows a spherical particle morphology with a particle size of up to about 10 microns. The LiNi0.8Co0.1Mn0.1O2The first charge-discharge curve of the positive electrode material at 0.1 multiplying power and 3-4.4V charge-discharge voltage is shown in figure 6, and the initial charge-discharge capacities are respectively as follows: 225.8mAh/g and 215.9 mAh/g.
Example 4
The ternary precursor Ni0.8Co0.1Mn0.1(OH)2And LiOH. H2Weighing 45g of O according to the stoichiometric ratio of 1:1.15, uniformly mixing, and carrying out ball milling on a planetary ball mill for 2 hours; then pretreating for 3h at 450 ℃ in an oxygen atmosphere, naturally cooling, and grinding to obtain a powdery product; the powdery product was again ball milled in a planetary ball mill for 2h, in O2Sintering for 15h at 750 ℃ under the pressure of 1 MPa in the atmosphere to obtain LiNi0.8Co0.1Mn0.1O2And (3) a positive electrode material.
The XRD pattern of the sample is shown in the (d) curve in FIG. 1, and it can be seen that the sample is free of impurities and is single-phase LiNi0.8Co0.1Mn0.1O2And (3) a positive electrode material. The LiNi0.8Co0.1Mn0.1O2The first charge-discharge curve of the positive electrode material under the multiplying power of 0.1 and the charge-discharge voltage of 2.8-4.3V is shown in figure 7, and the initial charge-discharge capacities are respectively as follows: 195.1mAh/g and 191.3 mAh/g.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. Lithium ion battery anode material LiNi0.8Co0.1Mn0.1O2The high-pressure solid phase preparation method is characterized by comprising the following steps:
(1) mixing precursors: mixing the ternary precursor with any one of lithium carbonate, lithium acetate or lithium hydroxide monohydrate according to the stoichiometric ratio of nickel, cobalt, manganese and lithium of 1: 1.05-1.15, and performing ball milling to obtain a mixed precursor;
(2) pretreatment: pretreating the mixed precursor in the step (1) at 350-450 ℃ in an oxygen atmosphere, naturally cooling, and grinding to obtain a powder material;
(3) sintering reaction: ball-milling the powder material obtained in the step (2), sintering in a high-pressure oxygen atmosphere of 8-12 MPa, and naturally cooling to obtain the LiNi anode material of the lithium ion battery0.8Co0.1Mn0.1O2；
In the step (3), the sintering temperature is 600-700 ℃, and the sintering time is 6-12 h.
2. The high pressure solid phase preparation method according to claim 1, wherein the ternary precursor in step (1) is Ni0.8Co0.1Mn0.1(OH)2。
3. The high-pressure solid phase preparation method according to claim 1, wherein the ball milling time in step (1) is 2-4 h.
4. The high pressure solid phase preparation method according to claim 1, wherein the pretreatment time in step (2) is 2 to 4 hours.
5. The high-pressure solid phase preparation method according to claim 1, wherein the ball milling time in the step (3) is 2-4 h.
6. LiNi which is a positive electrode material of a lithium ion battery prepared by the high-pressure solid-phase preparation method of any one of claims 1 to 50.8Co0.1Mn0.1O2。
7. The positive electrode material LiNi for lithium ion battery of claim 60.8Co0.1Mn0.1O2Application in lithium ion batteries.
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