CN112952064B - Lithium ion battery ternary nanosheet and preparation method and application thereof - Google Patents
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Abstract
The invention provides a ternary nanosheet of a lithium ion battery and a preparation method and application thereof, wherein potassium nickel cyanide is dissolved in deionized water to obtain a solution A; dissolving soluble cobalt salt, soluble ferric salt and sodium citrate tribasic into deionized water to obtain a solution B; slowly adding the solution A into the solution B, stirring for 30 minutes, and standing at room temperature; filtering and collecting a product, and washing the product with deionized water and ethanol; drying for 5 hours in a vacuum drying oven at the temperature of 60-80 ℃; calcining the powder in a nitrogen-filled tube furnace; and then putting the powder into a muffle furnace for calcining to obtain a final product. The preparation method provided by the invention has the advantages of rich raw material resources, low price, simple and convenient operation and easy industrial production. The prepared ternary metal oxide has a nanosheet structure, so that volume expansion caused in the charging and discharging process is effectively relieved, the transmission distance of lithium ions is shortened, and the electrochemical performance of the lithium battery is greatly improved.
Description
Technical Field
The invention relates to the technical field of lithium battery materials, in particular to a lithium ion battery ternary nanosheet and a preparation method and application thereof.
Background
The increasing global environmental pollution and energy crisis are receiving wide attention from various countries, and thus a new green energy storage or conversion device, such as a secondary battery, a super capacitor and water separation, is urgently developed. In particular, the high energy density and excellent cycle performance of Lithium Ion Batteries (LIBs) are widely applied to the application fields of portable electronic devices such as mobile phones, notebook computers and cameras, and are rapidly developed into one of the most important energy storage devices. Meanwhile, the lithium ion battery also has the advantages of small environmental pollution, high voltage and the like, and is considered as an energy storage device for solving the energy crisis with the greatest potential. The lithium battery consists of the following five parts: positive electrode, negative electrode, organic electrolyte, diaphragm and battery shell. In recent years, researchers have conducted a great deal of research to improve the performance of lithium ion batteries, such as rate and cycle. The binary metal oxide generally has excellent electrochemical performance, the electrochemical performance is further improved by continuously increasing elements to expand the binary metal oxide into the ternary metal oxide, namely, a binary system is converted into a ternary system, and the electrochemical performance of the ternary system material becomes a research hotspot with the increase of the requirement of a high-performance ratio battery.
In one of the prior art, patent CN109659537A "preparation method of citrate assisted fluorine-doped ternary nanosheet/polypyrrole and product and application" firstly adds lithium salt, nickel salt, cobalt salt, manganese salt and lithium fluoride into 40mL of deionized water according to a molar weight ratio of 1-x-y: x: y: z, and magnetically stirs until the solution is uniformly dispersed to obtain solution a; then, mixing hexamethylene tetramine and citrate according to a molar ratio of 10:1, adding the mixture into the solution A, continuously stirring the mixture until the mixture is completely dissolved to obtain solution B, and then carrying out magnetic stirring reflux on the solution B for 6 to 10 hours under the condition of oil bath at the temperature of between 90 and 110 ℃ to obtain a reactant; cooling the reactant, washing the obtained black precipitate with deionized water and ethanol for 2-3 times, and then putting the black precipitate into a vacuum oven to be dried overnight at 60-80 ℃ to obtain a dried substance; then placing the dried material in a muffle furnace, and calcining for 5-8 h at 500-700 ℃ to obtain a fluorine-doped ternary nanosheet material; dissolving fluorine-doped ternary nanosheets into absolute ethyl alcohol, adding 0.05mL of pyrrole monomer, and carrying out polymerization reaction for 5-7 h under a dark condition to obtain a sample; the sample is washed for 2-3 times by ethanol and deionized water, and is subjected to vacuum drying at 60-80 ℃ overnight to obtain the target product, namely the citrate auxiliary fluorine-doped ternary nanosheet/polypyrrole. According to the method, the growth of the ternary nanosheet is assisted by the citrate, the steps for preparing the fluorine-doped NCM nanosheet by the heat treatment low-temperature solution method are complex, byproducts are easy to generate, the yield of reactants is low, and the industrialization is not easy to realize.
Two High-performance machinery oxides for lithium storage. Https:// doi. Org/10.1016/j. Ceramine.2020.08.059 of the prior art, 13.25g of Na will be first mixed under stirring 2 CO 3 And 3.95g of NH 4 HCO 3 Dissolved in 500ml of distilled water to form solution A. 0.12mol of NiSO 4 ·6H 2 O,CoSO 4 ·7H 2 O and MnSO 4 (molar ratios of 2, 1. Then, solution B was added rapidly to solution a while continuing to stir vigorously for 6 hours. Washing, drying the precursor obtained and drying it in air at 500 ℃ for min -1 Is heated at 500 c for 2 hours to convert the mesoporous oxide. The ammonium bicarbonate material has great harm to human body, can cause blindness, pulmonary edema and other symptoms, releases irritant ammonia when being affected with damp, is harmful to water, cannot be directly discharged into a sewer, is difficult to treat and has great harm to environment.
Disclosure of Invention
The invention aims to provide a lithium ion battery ternary nanosheet and a preparation method and application thereof, which greatly simplify synthesis steps, reduce the generation of byproducts, have simple synthesis and easy industrialization, and reduce the risk of experimental operation by replacing an ammonium bicarbonate material with a tetracyanopotassium hydrate material. The cycle life and the rate capability of the battery are improved, and the electrochemical performance of the battery is greatly improved.
The specific technical scheme is as follows:
the preparation method of the ternary nanosheet of the lithium ion battery comprises the following steps:
(1) Dissolving potassium nickel cyanide into deionized water, and magnetically stirring until the solution A is completely dissolved;
dissolving soluble cobalt salt, soluble ferric salt and sodium citrate into deionized water, and magnetically stirring until the solution B is completely dissolved;
(2) Slowly adding the solution A into the solution B, stirring for 30 minutes, and standing at room temperature;
(3) Filtering and collecting a product, and washing the product with deionized water and ethanol;
(4) Drying the mixture for 5 hours in a vacuum drying oven at the temperature of between 60 and 80 ℃ to obtain dry powder;
(5) Calcining the powder in a nitrogen-filled tube furnace;
(6) And then putting the powder into a muffle furnace for calcining to obtain a final product.
In the step (1), the material ratio is configured according to the following proportion:
solution A,8mmol potassium nickel cyanide, 400ml deionized water;
solution B,4mmol of soluble cobalt salt, 4mmol of soluble iron salt, 3mmol of sodium citrate tribasic and 400ml of deionized water.
The soluble cobalt salt is cobalt acetate tetrahydrate, cobalt chloride and cobalt sulfate; the soluble ferric salt is tetrahydrate ferric acetate, ferric chloride and ferric sulfate.
Further, the standing time of the step (2) is 24-48 hours.
The temperature rise rate of the step (5) is 1 to 3 ℃ for min -1 The temperature range is 400-450 ℃.
The temperature rise rate of the step (6) is 1 to 3 ℃ min -1 The temperature range is 300-350 ℃.
The ternary nanosheet of the lithium ion battery obtained by the preparation method is applied as an electrode material in the lithium ion battery.
The preparation method provided by the invention has the advantages of rich raw material resources, low price, simple and convenient operation and easy industrial production. The prepared ternary metal oxide has a nanosheet structure, the prepared nanosheet structure can effectively relieve volume expansion caused in the charging and discharging process, the transmission distance of lithium ions is shortened, the electrochemical performance of the lithium battery is greatly improved, and the lithium battery has a good market prospect.
Drawings
FIG. 1 is an XRD diffraction pattern of the product of example 1;
FIG. 2 is the ternary metal oxide Fe of the product of example 1 2 O 3 /Co 3 O 4 A scanning electron microscope image of/NiO/NC;
FIG. 3 is the rate capability of the product of example 1;
FIG. 4 shows the cycle performance of the product of example 1.
Detailed Description
The embodiments of the present invention will be described with reference to the accompanying examples.
Example 1
Firstly, dissolving 8mmol of potassium nickel cyanide in 400ml of deionized water, magnetically stirring until the solution A is completely dissolved, then dissolving 4mmol of cobalt acetate tetrahydrate, 4mmol of ferric acetate tetrahydrate and 3mmol of sodium citrate in 400ml of deionized water, magnetically stirring until the solution B is completely dissolved, then slowly adding the solution A into the solution B, stirring for 30 minutes, then standing the sample for 24 hours at room temperature, carrying out suction filtration, collecting the sample, washing the sample with deionized water and ethanol for several times, and finally drying the sample for 5 hours at 60 ℃ in a vacuum drying oven to obtain dry powder. And heating the powder in a nitrogen-filled tube furnace at 1 ℃/min, keeping the temperature for 1 hour when the temperature is raised to 450 ℃, calcining the powder in a muffle furnace at 1 ℃/min, keeping the temperature for 0.5 hour when the temperature is raised to 350 ℃, and calcining the powder to obtain a final sample.
Fig. 1 is an X-ray diffraction pattern of the oversized ternary nanosheet prepared in this example, and the material is subjected to phase analysis. FIG. 2 is a scanning electron microscope image of an oversized ternary nanosheet, and as can be seen from the image, the prepared material is flaky in shape, about 7 μm in length, large in size and good in dispersibility.
After the material obtained in the embodiment is assembled into a battery, the oversized ternary nanosheet has excellent rate capability and cycle performance, as shown in fig. 3 and 4.
Example 2
Firstly, dissolving 8mmol of potassium nickel cyanide in 400ml of deionized water, magnetically stirring until the solution A is completely dissolved, then dissolving 4mmol of cobalt chloride, 4mmol of ferric chloride and 3mmol of sodium citrate in 400ml of deionized water, magnetically stirring until the solution B is completely dissolved, then slowly adding the solution A into the solution B, stirring for 30 minutes, then standing the sample for 24 hours at room temperature, carrying out suction filtration, collecting the sample, washing the sample with deionized water and ethanol for several times, and finally drying the sample in a vacuum drying oven at 60 ℃ for 5 hours to obtain dry powder. And heating the powder in a nitrogen-filled tube furnace at the speed of 2 ℃/min, keeping the temperature for 1 hour when the temperature is raised to 450 ℃, calcining the powder in a muffle furnace at the speed of 3 ℃/min, keeping the temperature for 0.5 hour when the temperature is raised to 300 ℃, and calcining the powder to obtain the final sample.
Example 3
Firstly, dissolving 8mmol of potassium nickel cyanide in 400ml of deionized water, magnetically stirring until the solution A is completely dissolved, then dissolving 4mmol of cobalt sulfate, 4mmol of ferric sulfate and 3mmol of sodium citrate in 400ml of deionized water, magnetically stirring until the solution B is completely dissolved, then slowly adding the solution A into the solution B, stirring for 30 minutes, then standing the sample for 48 hours at room temperature, carrying out suction filtration, collecting the sample, washing the sample with deionized water and ethanol for several times, and finally drying the sample in a vacuum drying oven at 60 ℃ for 5 hours to obtain dry powder. And heating the powder in a nitrogen-filled tube furnace at the speed of 2 ℃/min, keeping the temperature for 1 hour when the temperature is raised to 400 ℃, calcining the powder in a muffle furnace at the speed of 2 ℃/min, keeping the temperature for 0.5 hour when the temperature is raised to 350 ℃, and calcining the powder to obtain the final sample.
Example 4
Firstly, dissolving 8mmol of potassium nickel cyanide in 400ml of deionized water, magnetically stirring until the solution A is completely dissolved, then dissolving 4mmol of cobalt acetate tetrahydrate, 4mmol of ferric chloride and 3mmol of sodium citrate in 400ml of deionized water, magnetically stirring until the solution B is completely dissolved, then slowly adding the solution A into the solution B, stirring for 30 minutes, then standing the sample for 48 hours at room temperature, carrying out suction filtration, collecting the sample, washing the sample with deionized water and ethanol for several times, and finally drying the sample in a vacuum drying oven at 60 ℃ for 5 hours to obtain dry powder. And heating the powder in a nitrogen-filled tube furnace at 1 ℃/min, keeping the temperature for 1 hour when the temperature is raised to 400 ℃, calcining, then putting the powder in a muffle furnace at 3 ℃/min, heating to 300 ℃, keeping the temperature for 1 hour, calcining and obtaining the final sample.
Claims (6)
1. The preparation method of the ternary nanosheet of the lithium ion battery is characterized by comprising the following steps of:
(1) Dissolving potassium nickel cyanide into deionized water, and magnetically stirring until the solution A is completely dissolved;
dissolving soluble cobalt salt, soluble ferric salt and sodium citrate into deionized water, and magnetically stirring until the solution B is completely dissolved;
(2) Slowly adding the solution A into the solution B, stirring for 30 minutes, and standing at room temperature;
(3) Performing suction filtration to collect a product, and washing the product with deionized water and ethanol;
(4) Drying the mixture for 5 hours in a vacuum drying oven at the temperature of 60-80 ℃ to obtain dry powder;
(5) Calcining the powder in a nitrogen-filled tube furnace; the heating rate of the step (5) is 1 to 3 ℃ min -1 The temperature range is 400 to 450 ℃;
(6) Then, putting the powder into a muffle furnace for calcining to obtain a final product; the temperature rise rate of the step (6) is 1 to 3 ℃ min -1 The temperature range is 300 to 350 ℃.
2. The preparation method of ternary nanosheets of lithium ion batteries according to claim 1, wherein in step (1), the material ratio is configured according to the following ratio:
solution A,8mmol potassium nickel cyanide, 400ml deionized water;
solution B,4mmol of soluble cobalt salt, 4mmol of soluble iron salt, 3mmol of sodium citrate tribasic and 400ml of deionized water.
3. The preparation method of ternary nanosheets for lithium ion batteries according to claim 1, wherein the soluble cobalt salt is cobalt acetate tetrahydrate, cobalt chloride, cobalt sulfate; the soluble ferric salt is tetrahydrate ferric acetate, ferric chloride and ferric sulfate.
4. The preparation method of ternary nanosheets for lithium ion batteries according to claim 1, wherein the standing time of step (2) is 24-48 hours.
5. Ternary nanoplatelets for lithium ion batteries, characterized in that they are prepared according to the process of any of claims 1-4.
6. The lithium ion battery ternary nanoplate of claim 5, for use as an electrode material in a lithium ion battery.
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