CN110098394B - Nitrogen and boron codoped carbon quantum dot coated nickel-cobalt lithium aluminate positive electrode material and preparation method thereof - Google Patents
Nitrogen and boron codoped carbon quantum dot coated nickel-cobalt lithium aluminate positive electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention is suitable for the technical field of lithium batteries, and provides a nitrogen and boron codoped carbon quantum dot coated nickel-cobalt aluminum acid lithium battery anode material and a preparation method thereof, wherein in the preparation process, nitrogen and boron codoped carbon quantum dots are coated on the lithium battery anode material, and the existence of N-containing groups on the carbon quantum dots can strengthen the interaction with Li, thereby playing a good coating protection effect and inhibiting the interaction between the anode material and electrolyte; the presence of boron can reduce irreversible capacity loss. Meanwhile, the nano-scale pore channel structure formed after coating can reduce the volume change degree of the material in the charge and discharge process and improve the stability of the material structure. And the carbon quantum dots have certain conductivity, the bulk phase lithium ion transmission rate can be improved, and in addition, the untreated carbon quantum dots have certain acidity, so that part of surface residual alkali can be neutralized, and the surface residual alkali can be directly coated without being subjected to coating treatment after a water washing process, and finally, the lithium ion battery has excellent rate performance and cycle performance and also has good safety performance.
Description
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to a nitrogen and boron codoped carbon quantum dot coated nickel-cobalt lithium aluminate battery positive electrode material and a preparation method thereof.
Background
The nickel-cobalt-manganese or nickel-cobalt-aluminum ternary lithium ion battery anode material is widely applied to the fields of IT products and new energy automobiles due to high energy density and relatively simple preparation process. However, pure nickel cobalt lithium manganate (LNCM) or nickel cobalt lithium aluminate (LNCA) has poor structural stability, and is easily subjected to collapse of the material structure due to the de-intercalation of Li ions and the change of the valence states of Ni, Co and Mn/Al ions in the charging and discharging processes, thereby causing great harm to the cycle life and safety of the material. The surface coating is an effective method for improving the electrical property of the ternary material, and the effective surface coating can reduce the side reaction of the battery material and the electrolyte and prevent the electrolyte from corroding the surface of the electrode material. The conventional coating material is TiO2Oxide of an isometal、AlF3And fluoride and phosphate, however, these coating materials are easily detached from the surface of the battery material due to weak acting force with the battery material, and most of the materials have poor conductivity, so that the transfer of lithium ions is inhibited, and the improvement of the rate capability of the lithium ion battery is limited, which is disadvantageous for the development of high-performance lithium battery materials. Therefore, the stability of the material needs to be ensured while the cycle rate performance of the lithium ion battery is improved.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a positive electrode material of a nickel-cobalt lithium aluminate battery coated with nitrogen and boron co-doped carbon quantum dots and a preparation method thereof, and aims to solve the technical problem that the existing positive electrode material of a lithium ion battery cannot have good rate capability and structural stability at the same time.
On one hand, the preparation method of the positive electrode material of the nickel cobalt aluminum acid lithium battery coated with the nitrogen and boron co-doped carbon quantum dots comprises the following steps:
s1, weighing citric acid monohydrate in a beaker, adding ultrapure water to completely dissolve the citric acid monohydrate in the beaker to obtain a citric acid solution, then adding a boron source and a nitrogen-containing compound into the citric acid solution, and performing ultrasonic dispersion to obtain a uniformly mixed aqueous solution;
step S2, reacting the aqueous solution in an oven for a period of time, taking out the aqueous solution, naturally cooling the aqueous solution to room temperature to obtain a nitrogen and boron co-doped carbon quantum dot material, dissolving the nitrogen and boron co-doped carbon quantum dot material in water, and performing ultrasonic dispersion to obtain a nitrogen and boron co-doped carbon quantum dot solution;
step S3, uniformly mixing a lithium source and a nickel-cobalt-aluminum precursor in a high-speed mixer according to a certain molar ratio, then sintering in an oxygen atmosphere furnace, naturally cooling to room temperature after the reaction is finished, and obtaining a nickel-cobalt lithium aluminate single crystal primary sintering semi-finished product cathode material after crushing, sieving and iron removal;
and S4, mixing the nitrogen and boron co-doped carbon quantum dot solution with the nickel-cobalt lithium aluminate monocrystal calcined semi-finished product cathode material, uniformly mixing, drying in a vacuum drying oven, and cooling to obtain the nitrogen and boron co-doped carbon quantum dot coated nickel-cobalt lithium aluminate cathode material.
Specifically, in step S1, the concentration of the citric acid solution is 0.5-2g/mL, the addition amount of the boron element in the boron source and the nitrogen element in the nitrogen-containing compound is 0.5-3% of the molar amount of citric acid, and the nitrogen-containing compound is one or more of urea, ammonia water, and ethylenediamine.
Specifically, in step S2, the temperature rise rate of the oven is 10 ℃/min, the temperature is kept constant after rising to 200 ℃, and then the reaction is continued for 2.5 h.
Specifically, in step S3, the ratio of the molar amount of the lithium element in the lithium source to the molar sum of the metal elements in the nickel-cobalt-aluminum precursor is 1.01:1, the temperature of the oxygen atmosphere furnace is 770-800 ℃, and the sintering time is 12 hours.
Specifically, in the step S4, the addition amount of the nitrogen and boron co-doped carbon quantum dots is 0.05-0.5% of the mass of the nickel-cobalt lithium aluminate single crystal primary sintered semi-finished positive electrode material, and the vacuum drying time is 2-8 hours.
On the other hand, the positive electrode material of the nitrogen and boron codoped carbon quantum dot coated nickel-cobalt lithium aluminate battery is prepared by the preparation method of the positive electrode material of the nitrogen and boron codoped carbon quantum dot coated nickel-cobalt lithium aluminate battery.
According to the nitrogen and boron co-doped carbon quantum dot coated nickel-cobalt aluminum acid lithium battery positive electrode material and the preparation method, the nitrogen and boron co-doped carbon quantum dot is coated on the lithium ion battery positive electrode material in the preparation process, and the existence of the N-containing element group on the carbon quantum dot can enhance the interaction with Li, so that a good coating protection effect is achieved, and the interaction between the positive electrode material and electrolyte can be inhibited; the presence of boron can reduce irreversible capacity. Meanwhile, the nano-scale pore channel structure formed after coating can reduce the volume change degree of the material in the charge and discharge process and improve the stability of the material structure. And the carbon quantum dots have certain conductivity, the bulk phase lithium ion transmission rate can be improved, and in addition, the untreated carbon quantum dots have certain acidity, so that part of surface residual alkali can be neutralized, and the surface residual alkali can be directly coated without being subjected to coating treatment after a water washing process, and finally, the lithium ion battery has excellent rate performance and cycle performance and also has good safety performance.
Drawings
FIG. 1 is a graph comparing rate performance curves for example one of the present invention and comparative example one;
FIG. 2 is a graph comparing the cycle life curves of the first example of the present invention and the first comparative example.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In this embodiment, the preparation method of the positive electrode material of the lithium nickel cobalt aluminate battery coated with nitrogen and boron codoped carbon quantum dots comprises the following steps:
step S1, weighing citric acid monohydrate in a beaker, adding ultrapure water to completely dissolve the citric acid monohydrate to obtain a citric acid solution, then adding a boron source and a nitrogen-containing compound into the citric acid solution, and performing ultrasonic dispersion to obtain a uniformly mixed aqueous solution.
In the step, the concentration of the citric acid solution is 0.5-2g/mL, the adding amount of boron in the boron source and the adding amount of nitrogen in the nitrogen-containing compound are both 0.5-3% of the molar amount of the citric acid, the nitrogen-containing compound is one or more of urea, ammonia water and ethylenediamine, and the boron source can be boric acid.
And S2, reacting the aqueous solution in an oven for a period of time, taking out the aqueous solution, naturally cooling the aqueous solution to room temperature to obtain a nitrogen and boron co-doped carbon quantum dot material, dissolving the nitrogen and boron co-doped carbon quantum dot material in water, and performing ultrasonic dispersion to obtain the nitrogen and boron co-doped carbon quantum dot solution.
In the step, the heating rate of the oven is 10 ℃/min, the temperature is kept constant after being raised to 200 ℃, and then the reaction is continued for 2.5 h. In the embodiment, the carbon quantum dots are prepared by citric acid, a nitrogen-containing compound (such as ethylenediamine) and a boron source (such as boric acid), and in the specific process, citric acid, ethylenediamine, boric acid and the like are firstly subjected to polycondensation to form large-size carbon dots similar to polymers, and then are carbonized to form the carbon quantum dots.
And step S3, uniformly mixing the lithium source and the nickel-cobalt-aluminum precursor in a high-speed mixer according to a certain molar ratio, then sintering in an oxygen atmosphere furnace, naturally cooling to room temperature after the reaction is finished, and obtaining the nickel-cobalt lithium aluminate single crystal primary sintering semi-finished anode material after crushing, sieving and iron removal.
In this step, the lithium source may be lithium hydroxide or lithium carbonate. The ratio of the molar weight of the lithium element in the lithium source to the molar sum of the metal elements in the nickel-cobalt-aluminum precursor is 1.01:1, the temperature of the oxygen atmosphere furnace is 770-800 ℃, and the sintering time is 12 h.
And S4, mixing the nitrogen and boron co-doped carbon quantum dot solution with the nickel-cobalt lithium aluminate monocrystal calcined semi-finished product cathode material, uniformly mixing, drying in a vacuum drying oven, and cooling to obtain the nitrogen and boron co-doped carbon quantum dot coated nickel-cobalt lithium aluminate cathode material.
In the step, the addition amount of the nitrogen and boron co-doped carbon quantum dots is 0.05-0.5% of the mass of the nickel-cobalt lithium aluminate single crystal one-firing semi-finished product anode material, and the vacuum drying time is 2-8 h.
In order to explain the technical means of the present invention, the following description will be given by way of specific examples.
The first embodiment is as follows:
1) accurately weighing 50g of citric acid monohydrate in a beaker, adding 50mL of ultrapure water to completely dissolve the citric acid monohydrate, enabling the concentration of the final citric acid solution to be 1g/mL, then adding 2.9g of boric acid and 1.43g of ethylenediamine, carrying out ultrasonic treatment for 30min to fully and uniformly disperse the materials, then placing the materials in an oven, setting the heating speed of 10 ℃/min to carry out thermal cracking reaction at 200 ℃ for 2.5h, after the reaction is finished, naturally cooling to room temperature to obtain a nitrogen and boron co-doped carbon quantum dot solution, weighing 1g of the product, and dissolving the product in 20mL of water by means of the ultrapure water with the help of ultrasonic treatment to form the nitrogen and boron co-doped carbon quantum dot solution;
2) uniformly mixing lithium hydroxide and a nickel cobalt aluminum hydroxide precursor in a high-speed mixer according to the lithium/metal molar ratio of 1.01, placing the mixture in an atmosphere furnace, sintering the mixture for 12 hours at 790 ℃ in the oxygen atmosphere, naturally cooling the mixture to room temperature after the reaction is finished, and then performing air flow crushing, sieving and iron removal on the mixture to obtain a nickel cobalt lithium aluminate monocrystal anode material primary sintering semi-finished product;
3) uniformly mixing the nitrogen and boron co-doped carbon quantum dot solution obtained in the step 1) with 1kg of nickel-cobalt lithium aluminate single crystal ternary material, wherein the addition amount of the nitrogen and boron co-doped carbon quantum dots is 0.1%, uniformly mixing, drying in a vacuum drying oven for 3h, and cooling to obtain the nickel-cobalt lithium aluminate ternary cathode material coated with the nitrogen and boron co-doped carbon quantum dots;
4) and (4) forming the positive electrode material obtained in the step (3) into a button battery through size mixing, coating and drying, and carrying out battery charge and discharge tests.
Comparative example one:
1) the uncoated nickel-cobalt-aluminum ternary material was assembled into a button cell in the same manner as in example one, and then a charge and discharge test was performed.
2) And (3) forming the electrode material into the button battery through size mixing, coating and drying, and carrying out battery charge and discharge tests.
The rate performance and cycle life curves of the button battery prepared by the preparation method of the first embodiment and the first comparative example are respectively shown in fig. 1 and fig. 2, and the graphs of the rate performance and the cycle life of the button battery prepared by the preparation method of the first embodiment are combined with the graphs of the first comparative example, so that the rate retention of the capacity of the battery prepared by the first embodiment from 0.5C to 2C is larger than that of the battery prepared by the first comparative example, the capacity retention of the lithium battery prepared by the first embodiment still reaches 98.0% after 50 cycles, and the capacity retention of the lithium battery prepared by the first comparative example is only 94.0%. Therefore, after the cathode material of the first embodiment is coated with the nitrogen and boron co-doped carbon quantum dots, the rate performance and the cycle performance are both remarkably improved, and the performance of the material is improved to the maximum extent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (4)
1. The preparation method of the positive electrode material of the nickel-cobalt-aluminum acid lithium battery coated with nitrogen and boron codoped carbon quantum dots is characterized by comprising the following steps of:
s1, weighing citric acid monohydrate in a beaker, adding ultrapure water to completely dissolve the citric acid monohydrate in the beaker to obtain a citric acid solution, then adding a boron source and a nitrogen-containing compound into the citric acid solution, and performing ultrasonic dispersion to obtain a uniformly mixed aqueous solution;
step S2, reacting the aqueous solution in an oven for a period of time, taking out the aqueous solution, naturally cooling the aqueous solution to room temperature to obtain a nitrogen and boron co-doped carbon quantum dot material, dissolving the nitrogen and boron co-doped carbon quantum dot material in water, and performing ultrasonic dispersion to obtain a nitrogen and boron co-doped carbon quantum dot solution;
step S3, uniformly mixing a lithium source and a nickel-cobalt-aluminum precursor in a high-speed mixer according to a certain molar ratio, then sintering in an oxygen atmosphere furnace, naturally cooling to room temperature after the reaction is finished, and obtaining a nickel-cobalt lithium aluminate single crystal primary sintering semi-finished product cathode material after crushing, sieving and iron removing;
step S4, mixing the nitrogen and boron co-doped carbon quantum dot solution with the nickel-cobalt lithium aluminate monocrystal calcined semi-finished positive electrode material, uniformly mixing, drying in a vacuum drying oven, and cooling to obtain the nitrogen and boron co-doped carbon quantum dot coated nickel-cobalt lithium aluminate positive electrode material; in the step S4, the addition amount of the nitrogen and boron co-doped carbon quantum dots is 0.05-0.5% of the mass of the nickel-cobalt lithium aluminate single crystal primary sintered semi-finished positive electrode material, and the vacuum drying time is 2-8 h;
in step S1, the concentration of the citric acid solution is 0.5-2g/mL, the adding amount of the boron element in the boron source and the nitrogen element in the nitrogen-containing compound is 0.5-3% of the molar amount of the citric acid, and the nitrogen-containing compound is one or more of urea, ammonia water and ethylenediamine.
2. The method for preparing the positive electrode material of the nickel-cobalt-aluminum acid lithium battery coated with the nitrogen and boron co-doped carbon quantum dots as claimed in claim 1, wherein in the step S2, the temperature rise rate of the oven is 10 ℃/min, the constant temperature is kept after the temperature rises to 200 ℃, and then the reaction is continued for 2.5 hours.
3. The method for preparing the positive electrode material of the nickel-cobalt-aluminum acid lithium battery coated with the nitrogen and boron co-doped carbon quantum dots as claimed in claim 1, wherein in the step S3, the ratio of the molar amount of the lithium element in the lithium source to the molar sum of the metal elements in the nickel-cobalt-aluminum precursor is 1.01:1, the temperature of the oxygen atmosphere furnace is 770-800 ℃, and the sintering time is 12 hours.
4. The positive electrode material of the nitrogen and boron codoped carbon quantum dot coated nickel cobalt lithium aluminate battery is prepared by the method of any one of claims 1 to 3.
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