CN110723759A - Preparation method and application of lithium-rich manganese-based solid solution cathode material - Google Patents
Preparation method and application of lithium-rich manganese-based solid solution cathode material Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a lithium-rich manganese-based solid solution cathode material, wherein the preparation method comprises the steps of dissolving soluble metal salts containing Li, Mn, Co and Ni in secondary deionized water according to a molar ratio, and mixing to obtain a solution with a certain concentration; dissolving a polymer in absolute ethyl alcohol to prepare a polymer solution with a certain concentration; uniformly mixing the polymer solution and the metal salt solution, transferring the mixture into an injector, and preparing a precursor by using an electrostatic spinning device; and roasting the obtained precursor in an oxygen environment to obtain the lithium-rich manganese-based solid solution cathode material. The above scheme provided by the present application, due to the Li1.2Mn0.54Co0.13Ni0.13O2Positive electrodeThe concentration of the precursor of the material is 30mmol, so that the sample has a complete fiber structure, and the high specific capacity can be exerted; meanwhile, the catalyst is formed by roasting at 800 ℃ for 10h, so that the catalyst not only has high cation order degree and good structural stability, but also has proper morphology and crystallinity, and supports the material to carry out large-current charge and discharge.
Description
Technical Field
The invention relates to the technical field of lithium ion battery anode materials, in particular to a preparation method and application of a lithium-rich manganese-based solid solution anode material.
Background
In recent years, with the development of economy, environmental issues have been receiving more and more attention. The problems of haze, greenhouse effect and the like are increasingly prominent. The cause of these problems is derived largely from the emission of automobile exhaust gas. In order to reduce the emission of automobile exhaust, people gradually turn attention to new energy automobiles, and the power of the new energy automobiles is mainly a lithium ion battery. The lithium ion battery has the advantages of high specific energy, good cycle performance, wide working temperature range, low self-discharge rate, environmental friendliness and the like. However, the conventional lithium ion battery cathode material cannot meet the requirements of high specific energy and high specific capacity of the new energy automobile battery.
At present, the lithium-rich manganese-based material has the characteristics of high specific capacity, high working voltage and the like, and has great prospect of realizing 300Wh kg-1One of the positive electrode material systems of the high-specific energy lithium ion battery, however, the application of the high-specific energy lithium ion battery is severely restricted by the problems of low coulombic efficiency, poor rate capability, poor cycle performance and the like in the first week.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a lithium-rich manganese-based solid solution cathode material.
The invention provides a preparation method of a lithium-rich manganese-based solid solution cathode material, which comprises the following steps of:
dissolving soluble metal salts containing Li, Mn, Co and Ni in secondary deionized water according to a molar ratio, and mixing to obtain a solution with a certain concentration;
dissolving a polymer in absolute ethyl alcohol to prepare a polymer solution with a certain concentration;
uniformly mixing the polymer solution and the metal salt solution, transferring the mixture into an injector, and preparing a precursor by using an electrostatic spinning device;
and roasting the obtained precursor in an oxygen environment to obtain the lithium-rich manganese-based solid solution cathode material.
Further, the soluble metal salt is one or two of acetate and nitrate.
Further, the polymer is polyethylene pyrrole 21773and the mass fraction of the polyethylene pyrrole 21773and the ketone in absolute ethyl alcohol is 8 wt%.
Further, the concentration of the precursor is 30 mmol-50 mmol.
Further, the concentration of the precursor was 30 mmol.
Further, the roasting temperature is 500-900 ℃, and the roasting time is 5-10 h.
Further, the roasting temperature is 800 ℃, and the roasting time is 10 hours.
Further, the lithium-rich manganese-based solid solution cathode material is Li1.2Mn0.54Co0.13Ni0.13O2。
The invention also provides application of the lithium-rich manganese-based solid solution cathode material prepared by the method of any claim described in the embodiment of the application, the cathode material is used for a lithium ion battery system, and the lithium ion battery comprises the lithium-rich manganese-based solid solution (Li)1.2Mn0.54Co0.13Ni0.13O2) The lithium ion battery comprises a positive electrode material, a polypropylene (PP) diaphragm, a lithium metal negative electrode and electrolyte.
The method for preparing the lithium-rich manganese-based solid solution cathode material according to the above embodiment, since the Li1.2Mn0.54Co0.13Ni0.13O2The concentration of the precursor of the anode material is 30mmol, so that the sample has a complete fiber structure, and the high specific capacity can be exerted; meanwhile, the cationic modified starch is formed by roasting at 800 ℃ for 10 hours, so that the cationic modified starch has high cationic degree of order and good cationic degreeThe structure is stable, and the material has proper morphology and crystallinity, and supports the material to carry out heavy current charge and discharge.
Drawings
FIG. 1 is an SEM image of a lithium-rich manganese-based solid solution sample synthesized under different precursor concentrations provided by an embodiment of the invention;
FIG. 2 is a first charge-discharge diagram of a lithium-rich manganese-based solid solution sample synthesized under different precursor concentrations according to an embodiment of the present invention;
FIG. 3 is a graph of the cycle performance of samples of lithium-rich manganese-based solid solution synthesized at different precursor concentrations according to the embodiment of the present invention at 0.1C (a) and 1C (b);
FIG. 4 is an SEM image of samples of lithium-rich manganese-based solid solution synthesized at different calcination temperatures provided by an embodiment of the invention;
FIG. 5 is a graph showing the first charge and discharge of lithium-rich manganese-based solid solution samples synthesized at different calcination temperatures according to the example of the present invention;
FIG. 6 is a graph of the cycle performance at 0.1C (a) and 1C (b) for lithium-rich manganese-based solid solution samples synthesized at different calcination temperatures according to the examples of the present invention;
FIG. 7 shows lithium-rich manganese-based solid solution samples synthesized at different calcination times according to examples of the present invention;
FIG. 8 is a graph showing the first charge and discharge of lithium-rich manganese-based solid solution samples synthesized at different calcination times according to the example of the present invention;
fig. 9 is a graph of cycle performance of lithium-rich manganese-based solid solution samples synthesized at different calcination times according to the embodiment of the present invention at 0.1c (a) and 1c (b).
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings. Wherein like elements in different embodiments are numbered with like associated elements. In the following description, numerous details are set forth in order to provide a better understanding of the present application. However, those skilled in the art will readily recognize that some of the features may be omitted or replaced with other elements, materials, methods in different instances. In some instances, certain operations related to the present application have not been shown or described in detail in order to avoid obscuring the core of the present application from excessive description, and it is not necessary for those skilled in the art to describe these operations in detail, so that they may be fully understood from the description in the specification and the general knowledge in the art.
Furthermore, the features, operations, or characteristics described in the specification may be combined in any suitable manner to form various embodiments. Also, the various steps or actions in the method descriptions may be transposed or transposed in order, as will be apparent to one of ordinary skill in the art. Thus, the various sequences in the specification and drawings are for the purpose of describing certain embodiments only and are not intended to imply a required sequence unless otherwise indicated where such sequence must be followed.
The numbering of the components as such, e.g., "first", "second", etc., is used herein only to distinguish the objects as described, and does not have any sequential or technical meaning. The term "connected" and "coupled" when used in this application, unless otherwise indicated, includes both direct and indirect connections (couplings).
Example (b): a preparation method of a lithium-rich manganese-based solid solution cathode material comprises the following steps:
(1)1.5096g of lithium acetate, 1.5652g of manganese acetate, 0.3838g of nickel acetate, 0.3841g of cobalt acetate and 0.1651g of diammonium phosphate were dissolved in 18ml of secondary deionized water to obtain a mixed solution.
(2) 0.3g of PVP-600 was dissolved in 15ml of absolute ethanol to prepare a polymer solution.
(3) And (3) uniformly mixing the polymer solution obtained in the step (2) with the mixed solution obtained in the step (1), transferring the mixture into an injector, and preparing a precursor by using an electrostatic spinning device.
(4) Uniformly mixing the precursor obtained in the step (3) with 0.0324g of lithium fluoride, and roasting at 800 ℃ for 10h in an oxygen environment to obtain the lithium-rich manganese-based solid solution cathode material Li1.2Mn0.54Co0.13Ni0.13O2。
As shown in FIG. 1, the precursor concentration of both graphs a and b in FIG. 1 is 10 mmol; the precursor concentration of the c graph and the d graph is 20 mmol; the precursor concentration of the two graphs of e and f is 30 mmol; the precursor concentration of h and g is 40 mmol; the precursor concentration of the i graph and the j graph is 50 mmol; as can be seen from fig. 1, the change of the precursor concentration has a great influence on the morphology of the product, although all samples are stacked by nanoparticles at the microscopic level, and the overall morphology of the sample is a band shape about 2 μm wide when the precursor concentration is 10 mmol; the strip-shaped structure tends to be closed along with the increase of the concentration, and when the concentration is 30mmol, the sample basically forms a hollow tube shape with the diameter less than 2 mu m and is mutually staggered; when the concentration was increased to 50mmol, the sample was no longer tubular and formed an overlapping wrinkle. In addition, as the concentration increases, the primary particle size of the sample gradually increases, and from 100nm at 10mmol to 200nm at 50mmol, the particle-to-particle connection becomes increasingly tight, which is not favorable for the permeation of the electrolyte.
As can be seen from fig. 2: has maximum specific charge capacity of 347.5mAhg at 30mmol-1. The discharge process is basically not obviously different, the five samples are increased according to the concentration, and the discharge specific capacity of each sample is 219.3mAhg-1、221.5mAhg-1、274.5mAhg-1、252.8mAhg-1、259.2mAhg-1. The first coulombic efficiencies of the respective samples were 82.5%, 82.3%, 79.0%, 82.3%, and 77.4% in this order, and the tendency of the total decrease was shown to be illustrative of Li2MnO3Is irreversible.
From fig. 3, it is known that: the capacity of each sample is reduced in different degrees after being cycled for 30 times under the multiplying power of 0.1C, the capacity retention rate of each sample is 63.3%, 72.0%, 85.5%, 75.1% and 69.8% in sequence according to the increase of the precursor concentration, and the sample synthesized by the precursor concentration of 30mmol has the highest specific discharge capacity and capacity retention rate; when the current was increased to 1C, its capacity was reduced to 221.0mAhg-1Still have higher specific discharge capacity relative to other samples.
Selecting a precursor solution with the concentration of 30mmol, performing electrostatic spinning, keeping the temperature at 500 ℃ for 5h, then respectively heating to 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, keeping the temperature for 10h, and naturally cooling to room temperature to obtain the final product. Performing morphology analysis and electrochemical analysis on different products as shown in FIG. 4, wherein a and b in FIG. 4 are samples obtained by roasting at 700 ℃; the two diagrams of c and d are samples formed by roasting at 750 ℃; e and f are samples calcined at 800 ℃; g and h are samples calcined at 850 ℃; i and j are samples calcined at 900 ℃;
as can be seen from fig. 4, as the temperature of calcination is gradually increased, the overall morphology of the fiber and the nanoparticles on the fiber are significantly changed. The diameter of the product fiber at 700 ℃ is smaller, and the product fiber is in a closed tubular shape; when the temperature is raised to 800 ℃, the tubular structure of the fibers is split, but still continuous; when the temperature is continuously increased to 900 ℃, the fiber tubular structure is completely cracked, and the irregular flaky shape formed by the agglomeration of a plurality of nano-particles is changed. On the other hand, the size of the nanoparticles in the sample gradually increases, the diffusion path of lithium ions is prolonged, the surface of the particles becomes smoother, and even fusion of the particles occurs at high temperature, which is not favorable for the diffusion of the electrolyte, and these characteristics will deteriorate the rate capability and capacity of the material.
As can be seen from fig. 5: the provided capacity of the charging platform below 4.5V is greatly different, and the specific capacity of the platform is about 130mAhg for samples synthesized at 700 ℃, 750 ℃ and 900 ℃-1Whereas samples synthesized at 800 ℃ and 850 ℃ provided approximately 180mAh g-1The specific capacity of (A). With the increase of the temperature, the specific discharge capacity of each sample is 243.2mAh g-1、226.2mAhg-1、274.5mAhg-1、260.3mAhg-1、240.1mAhg-1The first coulombic efficiencies were 73.1%, 79.5%, 79.0%, 71.3%, 78.0%
As can be seen from fig. 6: and (3) a cycle performance diagram of the LMCNO sample synthesized at different calcination temperatures at 0.1C and 1C, wherein the voltage interval is 2.0-4.8V. The capacity of each sample is reduced in different degrees after being cycled for 30 times under the multiplying power of 0.1C, the capacity retention rate of each sample is respectively 58.2%, 80.1%, 82.5%, 82.6% and 85.9% according to the temperature rise, the capacity retention rate is gradually increased, and the stability is higher. When the multiplying power is increased to 1C, the capacity of the sample at 800 ℃ is obviously higher than that of other samples, but the stability is slightly insufficient, and the specific discharge capacity of the sample at 750 ℃ is basically kept unchanged after the sample is subjected to the first few times of activation, which probably means that the synthesized sample at the calcining temperature of 750 ℃ exists more in a layered structure with higher cationic order.
Further, at high temperature, metal elements in the material are easily lost, especially Li elements, which causes defects in the crystal structure of the material, and in turn, affects the electrochemical properties of the material. The calcination time of the electrostatic spinning precursor at 800 ℃ is explored. Heating to 800 deg.C, keeping the temperature for 8h, 10h, 12h, and 15h, respectively, and naturally cooling to room temperature to obtain the final product, as shown in FIG. 7. In FIG. 7, a and b are samples calcined for 8 h; the graph c and the graph d are samples calcined for 10 hours; e and f are samples calcined for 12 h; g and h are samples calcined for 15 h; as can be seen in fig. 7, the overall morphology remained as a continuous fiber tubular morphology as the calcination time was extended. When the calcination time is 8 hours, the particle size is small and uneven; when the calcination time is 10 hours, the particles become larger and are aggregated into continuous fibers with more gaps, which is beneficial to the electrolyte to enter the fibers; when the calcination time is 15 hours, the particles become dispersed, even the structure is collapsed on the local part of the fiber, the particle size of the nano particles on the fiber becomes larger and uniform, but the fusion between the particles obviously occurs, which is not beneficial to the permeation of the electrolyte, and the specific discharge capacity is reduced because the active substances can not be fully utilized.
As can be seen from FIG. 8, the first discharge specific capacities of the samples synthesized at different calcination times were 249.33mAhg-1、274.5mAh g-1、231.4mAh g-1、228.2mAh g-1The first coulombic efficiencies were 72.8%, 79.0%, 70.0%, 75.4%, respectively. Taken together, these materials have the charge and discharge characteristics typical of lithium rich manganese based materials, with two charge plateaus at 4.0V and 4.5V. The sample with the calcination time of 10h shows high specific discharge capacity and coulombic efficiency.
As can be seen from FIG. 9, each sampleThe capacity is reduced to different degrees after 30 cycles under the multiplying power of 0.1C, and the capacity retention rate of each sample is 63.5%, 82.5%, 79.7% and 84.5% respectively according to the extension of the calcining time. When the multiplying power is increased to 1C, in the previous cycles, the discharge specific capacities are all improved due to the existence of the activation process, and the maximum discharge specific capacity is 206.8mAh g in sequence-1、221.0mAh g-1、190.9mAh g-1、188.6mAh g-1The capacity retention rates after 50 cycles were 54.5%, 86.6%, 86.4%, 88.7%. The capacity retention rate under the condition of large current is higher than that under the condition of small current in the data, which is mainly caused by the fact that the capacity of the LMCNO sample is increased in the activation process, the capacity fading becomes smaller relative to the first time, and the reaction is fully performed under the condition of small current, and Li2MnO3The first time of activation shows high first discharge specific capacity. The capacity and the stability of the sample are poor when the calcination time is 8h, the crystal structure tends to be complete along with the extension of the calcination time, and the structural stability of the material is improved.
Synthesizing the fibrous LMCNO anode material with the nano/micron structure by an electrostatic spinning method, and respectively performing physical structure characterization and electrochemical performance test on the synthesized sample from the three aspects of precursor concentration, calcination temperature and calcination time. The optimal conditions for synthesis were found to be: the concentration of the precursor is 30mm0l, the calcining temperature is 800 ℃, and the calcining time is 10 h. The material synthesized under the conditions has the electrochemical advantages of high specific capacity, high capacity retention rate, good rate capability and the like, and the material is suitable for the application of high-power lithium batteries.
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. For a person skilled in the art to which the invention pertains, several simple deductions, modifications or substitutions may be made according to the idea of the invention.
Claims (9)
1. The preparation method of the lithium-rich manganese-based solid solution cathode material is characterized by comprising the following steps of:
dissolving soluble metal salts containing Li, Mn, Co and Ni in secondary deionized water according to a molar ratio, and mixing to obtain a solution with a certain concentration;
dissolving a polymer in absolute ethyl alcohol to prepare a polymer solution with a certain concentration;
uniformly mixing the polymer solution and the metal salt solution, transferring the mixture into an injector, and preparing a precursor by using an electrostatic spinning device;
and roasting the obtained precursor in an oxygen environment to obtain the lithium-rich manganese-based solid solution cathode material.
2. The method for preparing the lithium-rich manganese-based solid solution cathode material according to claim 1, wherein the soluble metal salt is one or both of acetate and nitrate.
3. The method for preparing the lithium-rich manganese-based solid solution cathode material according to claim 1, wherein the polymer is polyethylene pyrrole 21773and the mass fraction of the polyethylene pyrrole 21773and the ketone in the absolute ethanol is 8 wt%.
4. The method for preparing the lithium-rich manganese-based solid solution cathode material according to claim 1, wherein the concentration of the precursor is 30mmol to 50 mmol.
5. The method for preparing the lithium-rich manganese-based solid solution cathode material according to claim 4, wherein the concentration of the precursor is 30 mmol.
6. The preparation method of the lithium-rich manganese-based solid solution cathode material as claimed in claim 1, wherein the baking temperature is 500-900 ℃ and the baking time is 5-10 h.
7. The method for preparing the lithium-rich manganese-based solid solution cathode material according to claim 6, wherein the baking temperature is 800 ℃ and the baking time is 10 hours.
8. Rich in as claimed in claim 1The preparation method of the lithium-manganese-based solid solution cathode material is characterized in that the lithium-manganese-rich solid solution cathode material is Li1.2Mn0.54Co0.13Ni0.13O2。
9. Use of a lithium-rich manganese-based solid solution cathode material prepared by the method according to any one of claims 1 to 8, wherein the cathode material is used in a lithium ion battery system comprising the lithium-rich manganese-based solid solution (Li)1.2Mn0.54Co0.13Ni0.13O2) The lithium ion battery comprises a positive electrode material, a polypropylene (PP) diaphragm, a lithium metal negative electrode and electrolyte.
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