CN109638248B - Preparation method of porous ternary material, porous ternary material and half cell - Google Patents
Preparation method of porous ternary material, porous ternary material and half cell Download PDFInfo
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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Abstract
The invention discloses a preparation method of a porous ternary material, the porous ternary material and a half battery, and relates to the technical field of lithium ion batteries. The method comprises the steps of mixing and stirring a template agent and a precursor in an aqueous solution, and drying to obtain primary particles; the primary particles are mixed with a lithium source and then sintered. According to the method, the template agent can be embedded into the precursor through mixing of the precursor and the template agent, the appearance of the precursor is changed to a certain extent, carbon in the template agent is converted into carbon dioxide gas to fly out after the template agent is mixed and sintered with a lithium source, the environment is not polluted, and meanwhile, the position occupied by the original carbon is vacated to form a porous shape. The porous ternary material enables the contact area of the anode material and the electrolyte to be enlarged and the contact to be more sufficient, shortens the diffusion path of lithium ions, and improves the electrochemical properties of the lithium ion battery, such as rate capability, cycle performance and the like.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, and particularly relates to a preparation method of a porous ternary material, the porous ternary material and a half battery.
Background
The anode material is an important component of the lithium ion battery, and the ternary material with the layered structure is considered to be one of the most promising anode materials of the lithium ion battery due to the advantages of low price, high capacity, good cycle performance, high safety performance and the like. However, the ternary material has some defects, which severely restrict the application development, and many scholars at home and abroad research and try to improve the performance of the ternary material through surface coating and doping. However, methods for preparing porous ternary materials have been rarely reported.
Disclosure of Invention
One of the purposes of the invention is to provide a preparation method of a porous ternary material, which is simple and convenient and can be used for quickly preparing the porous ternary material, so that the contact area of a positive electrode material of a lithium ion battery and an electrolyte is obviously improved, the diffusion path of lithium ions is shortened, and the electrochemical properties of the lithium ion battery, such as multiplying power performance, cycle performance and the like, are improved.
The invention also aims to provide a porous ternary material, which is prepared by the preparation method of the porous ternary material. The porous ternary material can obviously improve the contact area of the anode material of the lithium ion battery and the electrolyte, and simultaneously shorten the diffusion path of lithium ions, thereby improving the electrochemical properties of the lithium ion battery, such as rate capability, cycle performance and the like.
The invention also aims to provide a half cell which is prepared from the porous ternary material. Therefore, the contact area between the half cell and the electrolyte can be remarkably increased, so that the diffusion path of lithium ions can be shortened, and the electrochemical performance such as the rate performance and the cycle performance of the lithium ion battery can be improved.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a preparation method of a porous ternary material, which comprises the following steps:
mixing and stirring the template agent and the precursor in an aqueous solution, and then carrying out spray drying to obtain primary particles;
the primary particles are mixed with a lithium source and then sintered.
The invention provides a porous ternary material which is prepared by the preparation method of the porous ternary material.
The invention provides a half cell, which is prepared by the following method:
mixing the porous ternary material, the conductive agent and the binder to obtain a mixture;
and performing ball milling on the mixture, and sequentially coating and vacuum-drying slurry obtained by ball milling.
The preparation method of the porous ternary material, the porous ternary material and the half cell provided by the embodiment of the invention have the beneficial effects that:
the preparation method of the porous ternary material provided by the embodiment of the invention comprises the steps of mixing and stirring the template agent and the precursor in an aqueous solution, and then performing spray drying to obtain primary particles; the primary particles are mixed with a lithium source and then sintered. Through the mixing of the precursor and the template, the template can be embedded into the precursor, the appearance of the precursor is changed to a certain extent, and simultaneously, after the template is mixed with a lithium source and sintered, carbon in the template is converted into carbon dioxide gas and flies out, so that the environment is not polluted, and meanwhile, the position occupied by the original carbon is vacated to form a porous shape. The porous ternary material enables the contact area of the anode material and the electrolyte to be enlarged, the contact is more sufficient, meanwhile, the diffusion path of lithium ions is shortened, and the rate capability, the cycle performance and other electrochemical properties of the lithium ion battery are improved.
The porous ternary material provided by the embodiment of the invention is prepared by the preparation method of the porous ternary material. The porous ternary material can obviously improve the contact area of the anode material of the lithium ion battery and the electrolyte, and simultaneously shorten the diffusion path of lithium ions, thereby improving the electrochemical properties of the lithium ion battery, such as rate capability, cycle performance and the like.
The half cell provided by the embodiment of the invention is prepared from the porous ternary material. Therefore, the contact area between the half cell and the electrolyte can be remarkably increased, so that the diffusion path of lithium ions can be shortened, and the electrochemical performance such as the rate performance and the cycle performance of the lithium ion battery can be improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and those skilled in the art can also obtain other related drawings based on the drawings without inventive efforts.
Fig. 1 is an SEM image of a carbon nanoball provided by the present invention;
FIG. 2 is an SEM image of a porous ternary material provided by the present invention;
FIG. 3 is a graph of cycle number versus gram volume of the porous ternary material provided by the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
The preparation method of the porous ternary material, the porous ternary material and the half cell of the embodiment of the invention are specifically described below.
The embodiment of the invention provides a preparation method of a porous ternary material, which comprises the following steps:
mixing and stirring the template agent and the precursor in an aqueous solution, and then carrying out spray drying to obtain primary particles; the primary particles are mixed with a lithium source and then sintered.
In detail, the template agent can be embedded into the precursor through the mixing of the precursor and the template agent, the appearance of the precursor is changed to a certain extent, and simultaneously, after the template agent is mixed with a lithium source and sintered, carbon in the template agent is converted into carbon dioxide gas and flies out, so that the environment is not polluted, and meanwhile, the position occupied by the original carbon is vacated to form a porous shape. The porous ternary material enables the contact area of the anode material and the electrolyte to be enlarged and the contact to be more sufficient, shortens the diffusion path of lithium ions, and improves the electrochemical properties of the lithium ion battery, such as rate capability, cycle performance and the like.
Preferably, in this embodiment, the template is a carbon nanosphere. Through the pretreatment of the precursor, the precursor is uniformly mixed with a lithium source according to a certain proportion and then sintered at high temperature, the carbon nanospheres are converted into carbon dioxide and fly out, the positions occupied by the original carbon are vacated, and the porous ternary material is formed.
Specifically, the carbon nanoball is prepared by the following method: reacting the glucose solution in a hydrothermal reaction kettle; centrifugally separating a product after reaction, and washing with ethanol and water; and drying the washed product.
Wherein in the step of reacting the glucose solution in the hydrothermal reaction kettle, the concentration of the glucose solution is 0.5mol/L, and the reaction parameter is that the reaction is carried out for 3.5h at the temperature of 160 ℃; in the step of drying the washed product, the drying temperature is 80 ℃, and the particle size of the dried carbon nanoball is about 200nm. Fig. 1 is an SEM image of a carbon nanoball provided by the present invention. Referring to fig. 1, it can be seen that the prepared carbon nanoball has substantially no agglomeration phenomenon, good dispersibility, regular spherical shape and uniform size (mainly because the synthesized carbon nanoball has-OH and-CO groups on the surface), and has a diameter of about 200nm.
In detail, in an embodiment of the present invention, the precursor may be selected to be a type 622 precursor; and when the precursor is a 622-type precursor, the steps of mixing and stirring the template and the precursor in an aqueous solution, and then performing spray drying to obtain primary particles specifically comprise:
weighing 500 parts by weight of 622 type precursor, and dissolving in 2000-3500 parts by weight of deionized water; preferably, 3000 parts of deionized water can be selected;
and (3) after uniformly stirring, adding 35-80 parts of carbon nanospheres, preferably 50 parts of carbon nanospheres, and drying by using spray drying equipment to obtain a precursor doped with the carbon nanospheres, wherein the particle size of the precursor doped with the carbon nanospheres is 1-20 mu m.
Wherein, FIG. 2 is an SEM picture of the prepared porous ternary material. As can be seen from the figure, the prepared porous ternary material is composed of a plurality of hollow structures, a plurality of nano particles are attached to the edge of a hollow hemisphere, the nano particles are in an amorphous state, the shape and the size of the hollow structures are uniform, the diameter of the hollow structures is about 200nm, and the diameter of the hollow structures is about equal to the diameter of the carbon nanospheres, which indicates that the carbon nanospheres play the role of a template agent in the system.
Preferably, in the embodiment of the present invention, the lithium source is a lithium source obtained by preparing lithium hydroxide or lithium carbonate according to a predetermined lithium. The sintering step after mixing the primary particles with a lithium source specifically comprises:
weighing a lithium source according to the lithium proportion L/M =1.03 to 1.1, preferably, L/M =1.05, wherein the lithium source is lithium carbonate or lithium hydroxide;
and (3) uniformly mixing a lithium source and the precursor doped with the carbon nanosphere by a planetary ball mill, and then sintering.
In the preparation process, the precursor and the lithium source are mixed by a planetary ball mill in a dry method, a wet process is not added, lithium ions are not easy to form lithium dendrites on the surface of the negative electrode, and the prepared ternary material is ensured to have higher gram capacity.
Further preferably, in the embodiment of the invention, the sintering is carried out at a constant temperature of 10 ℃/min to 300 ℃ in the air or oxygen atmosphere, the temperature is kept constant for 2 to 3 hours, then the temperature is kept constant for 10 ℃/min to 500 ℃, the temperature is kept constant for 2 to 3 hours, finally the temperature is kept constant for 10 ℃/min to 900 ℃, and the temperature is kept constant for 10 to 12h, and then the mixture is naturally cooled. Of course, in other embodiments of the present invention, the sintering parameters may also be selected and adjusted according to requirements, and the embodiments of the present invention are not limited.
The porous ternary material provided by the embodiment of the invention is prepared by the preparation method of the porous ternary material. The porous ternary material can obviously improve the contact area of the anode material of the lithium ion battery and the electrolyte, and simultaneously shorten the diffusion path of lithium ions, thereby improving the electrochemical properties of the lithium ion battery, such as rate capability, cycle performance and the like.
The embodiment of the invention provides a half cell, which is prepared by the following method:
mixing the porous ternary material, the conductive agent and the binder to obtain a mixture;
and performing ball milling on the mixture, and sequentially coating and vacuum-drying slurry obtained by ball milling. The contact area between the half-cell and the electrolyte can be obviously improved, so that the diffusion path of lithium ions can be shortened, and the electrochemical properties such as the rate capability, the cycle performance and the like of the lithium ion battery can be improved.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a porous ternary material, which is prepared by the following method:
s1: weighing a certain amount of glucose, preparing a 0.5moL/L glucose solution, reacting in a hydrothermal reaction kettle at 160 ℃ for 3.5h, centrifugally separating, washing with a large amount of ethanol and water, and finally drying at 80 ℃ to obtain carbon nanospheres with the particle size of about 200 nm;
s2: weighing 622 type precursors 500g and dissolving in 3000g deionized water, adding 50g carbon nanospheres after stirring uniformly, pumping the suspension into spray drying equipment through a peristaltic pump for drying to obtain precursors doped with the carbon nanospheres, wherein the particle size range of the obtained products is 1-20 mu m.
S3: and weighing a lithium source (lithium carbonate or lithium hydroxide) according to the lithium proportion L/M =1.05, and uniformly mixing the lithium source and the precursor doped with the carbon nanospheres by a planetary ball mill to obtain a product to be burnt.
S4: and placing the obtained product to be burnt in an atmosphere muffle furnace, heating to 300 ℃ at a constant speed of 10 ℃/min under the air or oxygen atmosphere, keeping the temperature for 2 to 3h, heating to 500 ℃ at a constant speed of 10 ℃/min, keeping the temperature for 2 to 3h, heating to 900 ℃ at a constant speed of 10 ℃/min, keeping the temperature for 10 to 12h, and naturally cooling to obtain the porous lithium nickel cobalt manganese oxide ternary material.
The present embodiment also provides a half cell, which is prepared by the following method:
s1: mixing the prepared ternary material, the conductive agent and the binder according to a certain proportion;
s2: then ball milling is carried out for 2 hours by using a vacuum ball milling tank 600 rmp to prepare slurry which is evenly mixed and has moderate viscosity, coating is carried out, and vacuum drying is carried out to prepare the electrode slice.
The conductive agent adopts super 'P', the diaphragm is celgard 2300, the electrolyte adopts 1 mol/L LiPF6 conductive salt and DMC, DEC, EC (wt%) =1. The first effect and the cycle performance of the battery are tested under the conditions that the charge and discharge cut-off voltage is 2.3-4.75V and 0.1C, the result is shown in figure 3, the porous ternary material prepared according to figure 3 has high gram capacity and good cycle performance, the capacity retention rate is more than 94% after 30 cycles, and the first charge and discharge efficiency can reach 95%.
In summary, the preparation method of the porous ternary material provided by the embodiment of the invention is simple and convenient, and the porous ternary material can be quickly prepared, so that the contact area between the anode material and the electrolyte of the lithium ion battery is remarkably increased, the diffusion path of lithium ions is shortened, and the electrochemical properties such as the rate capability, the cycle performance and the like of the lithium ion battery are improved.
The porous ternary material provided by the embodiment of the invention is prepared by the preparation method of the porous ternary material. The porous ternary material can obviously improve the contact area of the anode material of the lithium ion battery and the electrolyte, and simultaneously shorten the diffusion path of lithium ions, thereby improving the electrochemical properties of the lithium ion battery, such as rate capability, cycle performance and the like.
The embodiment of the invention provides a half cell prepared from the porous ternary material. Therefore, the contact area between the half cell and the electrolyte can be remarkably increased, so that the diffusion path of lithium ions can be shortened, and the electrochemical performance such as the rate performance and the cycle performance of the lithium ion battery can be improved.
The embodiments described above are some, not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. 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.
Claims (8)
1. A preparation method of a porous ternary material is characterized by comprising the following steps:
mixing and stirring the template agent and the precursor in an aqueous solution, and then performing spray drying to obtain primary particles; wherein the template agent is a carbon nanosphere, and the precursor is a 622-type precursor; the step of mixing and stirring the template agent and the precursor in the aqueous solution and then drying to obtain the primary particles specifically comprises the following steps: weighing 500 parts by weight of 622 type precursor, and dissolving in 2000 to 3500 parts by weight of deionized water; adding 35-80 parts of carbon nanospheres after uniformly stirring, and drying by using spray drying equipment to obtain a precursor doped with the carbon nanospheres, wherein the particle size of the precursor doped with the carbon nanospheres is 1-20 mu m;
and mixing the primary particles with a lithium source and then sintering.
2. The method for preparing a porous ternary material according to claim 1, wherein:
the carbon nanosphere is prepared by the following method:
reacting the glucose solution in a hydrothermal reaction kettle;
centrifugally separating a product after reaction, and washing with ethanol and water;
and drying the washed product.
3. The method for preparing a porous ternary material according to claim 2, wherein:
in the step of reacting the glucose solution in the hydrothermal reaction kettle, the concentration of the glucose solution is 0.5mol/L, and the reaction parameter is that the glucose solution reacts for 3.5h at the temperature of 160 ℃;
in the step of drying the washed product, the drying temperature is 80 ℃.
4. The method for preparing a porous ternary material according to claim 1, wherein:
the lithium source is obtained by lithium hydroxide or lithium carbonate according to preset lithium.
5. The method for preparing a porous ternary material according to claim 4, wherein:
the sintering step after mixing the primary particles with a lithium source specifically comprises:
weighing the lithium source according to the lithium proportion L/M =1.03 to 1.1, wherein the lithium source is lithium carbonate or lithium hydroxide;
and uniformly mixing the lithium source and the precursor doped with the carbon nanospheres by a planetary ball mill, and sintering.
6. The method for preparing a porous ternary material according to claim 5, wherein:
and sintering, namely heating to 300 ℃ at a constant speed of 10 ℃/min in the air or oxygen atmosphere, keeping the temperature for 2 to 3 hours, heating to 500 ℃ at a constant speed of 10 ℃/min, keeping the temperature for 2 to 3 hours, heating to 900 ℃ at a constant speed of 10 ℃/min, keeping the temperature for 10 to 12h, and then naturally cooling.
7. A porous ternary material characterized by:
the porous ternary material is prepared by the preparation method of the porous ternary material as claimed in any one of claims 1 to 6.
8. A half-cell, characterized in that it is prepared by a process comprising:
mixing the porous ternary material of claim 7, a conductive agent and a binder to obtain a mixture;
and performing ball milling on the mixture, and sequentially coating and vacuum-drying slurry obtained by ball milling.
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