CN113896250B - Layered Co 3 O 4 Lithium ion battery negative electrode material and preparation method thereof - Google Patents
Layered Co 3 O 4 Lithium ion battery negative electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a layered Co 3 O 4 A lithium ion battery cathode material and a preparation method thereof relate to the field of batteries. The method comprises the following steps: s1, weighing Co (NO) 3 ) 2 ·6H 2 O and CoCl 3 ·6H 2 O is added into a morphology guiding agent containing ammonia water and glycol to prepare a precursor solution; s2, stirring the precursor solution, and then performing solvothermal reaction to prepare a solid suspension; s3, filtering the solid suspension to retain a solid product, and cleaning and drying the solid product to obtain a precursor beta-Co (OH) 2 The method comprises the steps of carrying out a first treatment on the surface of the S4, preparing the precursor beta-Co (OH) 2 Heating and calcining in air atmosphere to obtain layered Co 3 O 4 . In the present application layered Co with rod-like profile is obtained 3 O 4 The layered structure of the lithium ion battery is beneficial to accelerating the transmission rate of lithium ions, providing a stable discharging platform, enhancing the multiplying power of the battery and improving the specific capacity of the material.
Description
Technical Field
The invention relates to the field of batteries, in particular to a layered Co 3 O 4 A lithium ion battery cathode material and a preparation method thereof.
Background
With the rapid increase of world population, the problem of energy shortage is increasingly serious, and the main energy storage devices at present comprise chemical power supply energy storage and mechanical energy storage, wherein the mechanical energy storage has the randomness and variability which are difficult to control, and compared with the higher requirement of the mechanical energy storage on the environment, the chemical energy storage has higher energy density and power density, has portability, mainly comprises lithium ion batteries, lead-acid batteries, flow batteries and the like, and is widely applied to the consumer electronics and electric automobile industries.
Compared with the traditional secondary battery, the lithium ion battery has the advantages of high working voltage, large specific energy, stable discharge voltage, long cycle life, no environmental pollution and the like. The cathode material is one of key materials of the lithium battery, mainly is a carbon material, such as graphite, porous carbon and the like, but the carbon material has lower specific capacity, poor multiplying power performance and weak structural rigidity, is easy to agglomerate and pulverize, is unfavorable for prolonging the service life of the lithium battery, and causes that the specific capacity of the graphite cathode material used by the current commercial lithium battery is lower, the specific capacity range is 200-400mAh/g, and the energy requirement of rapid development cannot be met.
Disclosure of Invention
The invention provides a layered Co 3 O 4 The material accelerates the transmission rate of lithium ions by utilizing the layered structure of the material, improves the specific capacity and solves the technical problem of low specific capacity of the lithium battery cathode material.
In order to solve the technical problems, one of the purposes of the embodiment of the invention is to provide a layered Co 3 O 4 The preparation method of the lithium ion battery anode material comprises the following steps:
s1, weighing Co (NO) 3 ) 2 ·6H 2 O and CoCl 3 ·6H 2 O is added into the morphology guiding agent to prepare a precursor solution;
s2, stirring the precursor solution, and then performing solvothermal reaction to prepare a solid suspension;
s3, filtering the solid suspension to retain a solid product, and cleaning and drying the solid product to obtain a precursor beta-Co (OH) 2 ；
S4, preparing the precursor beta-Co (OH) 2 Heating and calcining in air atmosphere to obtain layered Co 3 O 4 ；
Wherein the morphology guiding agent is a mixed solution of ammonia water and ethylene glycol.
Through the scheme, CO 3 2+ With OH in ammonia water - The precursor beta-Co (OH) with hydrotalcite layered double hydroxyl structure is generated by the reaction 2 Organic small molecules of ammonia water and glycol in the morphology guiding agent are reacted with precursor beta-Co (OH) through hydrogen bonds 2 OH of dihydroxyl structure - Is connected and inserted between layers to avoid stacking of layers, thereby avoiding ion channel disappearance, and finally the layered Co with a bar-shaped outline is obtained through calcination and dehydration 3 O 4 The layered Co 3 O 4 Is formed by passing between different layers of sheet Co 3 O 4 Mutually stacked to form a bar-shaped outline, the original layered structure is maintained in the calcining process, the shape of the layered stacked Co is not changed in the calcining process 3 O 4 The material is more beneficial to improving the transmission speed of Li ions, is convenient for the intercalation or deintercalation of lithium ions, improves a stable discharge platform, enhances the multiplying power of a battery, improves the specific capacity of the material, and has the discharge specific capacity of 900mAh/g.
Preferably, in the step S4, the calcination is performed as β -Co (OH), which is a precursor 2 Heating to 450-550 ℃ in an air atmosphere, heating up at a rate of 1 ℃/min, and then keeping the temperature constant for 1-3 h.
By adopting the scheme, the precursor beta-Co (OH) 2 The ammonia water and glycol between layers are calcined at high temperature to form carbon, which accelerates Co 3 O 4 Is controlled by limiting the rate of rise of temperature and the final heating temperature during calcination 3 O 4 The lattice spacing is widened, and the wider lattice spacing is favorable for lithium ion transmission, so that the specific capacity of the material is improved.
In the preferred scheme, in the S1, the mass fraction of the ammonia water in the morphology guidance agent is 5% -10%.
Preferably, in the step S1, the concentration of the precursor solution is 0.2mol/L to 0.6mol/L.
Preferably, in S1, the Co (NO 3 ) 2 ·6H 2 O and CoCl 3 ·6H 2 The molar ratio of O is1：1。
In a preferred scheme, in the step S1, the solvothermal reaction is to place the precursor solution after stirring in a reaction device at 180-250 ℃ for 12-24 h.
Preferably, in the step S3, the washing is to wash the solid-phase product with ethanol and deionized water sequentially.
Preferably, in S3, the drying is performed by drying the solid-phase product at a temperature of 60 ℃ for 24 hours.
Preferably, in S2, the stirring time is 1h to 2h.
To solve the above-mentioned problems, a second object of the present invention is to provide a layered Co 3 O 4 Lithium ion battery anode material comprising layered Co for preparing lithium ion battery anode material 3 O 4 The layered Co 3 O 4 The layered Co is adopted 3 O 4 The layered Co is prepared by a preparation method of a lithium ion battery anode material 3 O 4 Is a layered stacked structure, the layered Co 3 O 4 The stacked bar-shaped profile is formed.
Compared with the prior art, the embodiment of the invention has the following beneficial effects:
1. the precursor beta-Co (OH) with hydrotalcite layered double-hydroxyl structure can be generated after solvothermal reaction 2 The organic micromolecules of ammonia water and glycol in the morphology guiding agent are inserted between layers, so that stacking of the same layers is avoided, and finally, the laminar Co with a rod-shaped profile is obtained through calcination and dehydration 3 O 4 Co of the layered stack 3 O 4 The material is more beneficial to improving the transmission speed of Li ions, improving a stable discharge platform, enhancing the multiplying power of a battery, improving the specific capacity of the material, and the specific discharge capacity of the material can reach 900mAh/g.
2. Precursor beta-Co (OH) 2 The ammonia water and glycol between layers are calcined at high temperature to form carbon, which accelerates Co 3 O 4 By limiting the rate of rise of temperature and the final heating temperature during calcinationDegree to control Co 3 O 4 The lattice spacing is widened, and the wider lattice spacing is favorable for lithium ion transmission, so that the specific capacity of the material is improved.
Drawings
Fig. 1: layered Co as one of the first embodiment of the present invention 3 O 4 XRD diffraction peak pattern of lithium ion battery cathode material;
fig. 2: layered Co as one of the first embodiment of the present invention 3 O 4 SEM image with resolution of 500nm of lithium ion battery cathode material;
fig. 3: layered Co as one of the first embodiment of the present invention 3 O 4 TEM image with resolution of 0.5 μm of the lithium ion battery cathode material;
fig. 4: layered Co as one of the first embodiment of the present invention 3 O 4 SEM image with resolution of 5nm of lithium ion battery cathode material;
fig. 5: layered Co as one of the first embodiment of the present invention 3 O 4 Charge-discharge characteristic diagram (note: 1) of lithium ion battery anode material st 、2 nd 、4 th 、5 th Respectively representing different cycles of the same sample).
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Layered Co 3 O 4 Lithium ion battery anode material comprising layered Co useful for preparing lithium ion battery anode material 3 O 4 Layered Co 3 O 4 Is of a layered stacked structure, layered Co 3 O 4 The bar-shaped profile is formed after stacking, and the bar-shaped profile is prepared by the following steps:
s1, co (NO) 3 ) 2 ·6H 2 O and CoCl 3 ·6H 2 O is 1 in mole ratio: 1, and then adding the mixture into 60mL of morphology guiding agent to prepare a precursor solution, wherein the concentration of the precursor solution is 0.33mol/L, and the morphology guiding agent is a mixed solution containing ethylene glycol and 8.3wt% ammonia water;
s2, stirring the precursor solution for 1h, then transferring the fully reacted precursor solution into a reaction kettle for solvothermal reaction, controlling the reaction temperature to 220 ℃, controlling the heating time to 18h, and standing and cooling the reaction kettle to room temperature after heating is finished to obtain a solid suspension;
s3, filtering the solid suspension, reserving solid phase products, respectively washing the solid phase products with absolute ethyl alcohol and deionized water for 3 times, then drying in a drying oven, controlling the temperature to be 60 ℃ and the drying time to be 24 hours, and obtaining a precursor beta-Co (OH) 2 ；
S4, precursor beta-Co (OH) 2 Heating and calcining in a tubular furnace in air atmosphere, controlling heating rate to 1deg.C/min, heating to 500deg.C, and maintaining constant temperature for 1 hr to obtain layered Co 3 O 4 。
Example two
Layered Co 3 O 4 Lithium ion battery anode material comprising layered Co useful for preparing lithium ion battery anode material 3 O 4 Layered Co 3 O 4 Is of a layered stacked structure, layered Co 3 O 4 The bar-shaped profile is formed after stacking, and the bar-shaped profile is prepared by the following steps:
s1, co (NO) 3 ) 2 ·6H 2 O and CoCl 3 ·6H 2 O is 1 in mole ratio: 1, and then adding the mixture into 60mL of morphology guiding agent to prepare a precursor solution, wherein the concentration of the precursor solution is 0.6mol/L, and the morphology guiding agent is a mixed solution containing ethylene glycol and 10wt% ammonia water;
s2, stirring the precursor solution for 2 hours, transferring the fully reacted precursor solution into a reaction kettle for solvothermal reaction, controlling the reaction temperature to be 180 ℃, controlling the heating time to be 24 hours, and standing and cooling the reaction kettle to room temperature after heating is finished to obtain a solid suspension;
s3, filtering the solid suspension, reserving solid phase products, respectively washing the solid phase products with absolute ethyl alcohol and deionized water for 3 times, then drying in a drying oven, controlling the temperature to be 60 ℃ and the drying time to be 24 hours, and obtaining a precursor beta-Co (OH) 2 ；
S4, precursor beta-Co (OH) 2 Heating and calcining in a tubular furnace in air atmosphere, controlling heating rate to 1deg.C/min, heating to 450deg.C, and maintaining constant temperature for 3 hr to obtain layered Co 3 O 4 。
Example III
Layered Co 3 O 4 Lithium ion battery anode material comprising layered Co useful for preparing lithium ion battery anode material 3 O 4 Layered Co 3 O 4 Is of a layered stacked structure, layered Co 3 O 4 The bar-shaped profile is formed after stacking, and the bar-shaped profile is prepared by the following steps:
s1, co (NO) 3 ) 2 ·6H 2 O and CoCl 3 ·6H 2 O is 1 in mole ratio: 1, and then adding the mixture into 60mL of morphology guiding agent to prepare a precursor solution, wherein the concentration of the precursor solution is 0.2mol/L, and the morphology guiding agent is a mixed solution containing ethylene glycol and 5wt% ammonia water;
s2, stirring the precursor solution for 2 hours, transferring the fully reacted precursor solution into a reaction kettle for solvothermal reaction, controlling the reaction temperature to 250 ℃, controlling the heating time to 12 hours, and standing and cooling the reaction kettle to room temperature after heating is completed to obtain a solid suspension;
s3, filtering the solid suspension, retaining the solid phase product, respectively washing the solid phase product with absolute ethyl alcohol and deionized water for 3 times, drying in a drying oven, controlling the temperature to be 60 ℃ and controlling the drying time to be 24 hours to obtainPrecursor beta-Co (OH) 2 ；
S4, precursor beta-Co (OH) 2 Heating and calcining in a tubular furnace in air atmosphere, controlling heating rate to be 1 deg.C/min, heating to 550 deg.C, and keeping constant temperature for 1 hr to obtain layered Co 3 O 4 。
Performance test results
As can be seen from the results of FIG. 1, the layered Co obtained in example one 3 O 4 Diffraction peak pattern formed by material and Co 3 O 4 Diffraction peak patterns formed by the standard cards correspond to each other, and the material obtained in the first embodiment is proved to be Co 3 O 4 。
As can be seen from the results of fig. 2, 3 and 5, example 1 was performed by CO 3 2+ With OH in ammonia water - The precursor beta-Co (OH) with hydrotalcite layered double hydroxyl structure is generated by the reaction 2 Organic small molecules of ammonia water and glycol in the morphology guiding agent are reacted with precursor beta-Co (OH) through hydrogen bonds 2 OH of dihydroxyl structure - Is connected and inserted between layers to avoid stacking of layers, and finally the layered Co is obtained by calcining and dehydrating 3 O 4 The original layered structure is maintained in the calcining process, the whole body is in a rod-shaped structure, and the shape change does not occur in the calcining process. As shown in FIG. 5, 1.25V and 2.0V have obvious charge-discharge plateau in the charge-discharge process, and a large difference exists between the first charge-discharge specific capacities, which indicates that the layered Co 3 O 4 Surface SEI film formation and loss of electrochemically active sites when used as a negative electrode material. Description of the layered stack Co 3 O 4 The material is more beneficial to improving the transmission speed of Li ions, improving a stable discharge platform, enhancing the multiplying power of a battery, improving the specific capacity of the material and being 1Ag -1 To make layered Co at current density of (2) 3 O 4 The specific discharge capacity of the material reaches 900mAh/g.
As can be seen from the results of FIGS. 4 and 5, the precursor β -Co (OH) 2 The ammonia water and glycol between layers are calcined at high temperature to form carbon, which accelerates Co 3 O 4 Is formed by heating during calcinationRate and final heating temperature to control Co 3 O 4 To widen the lattice spacing, layered Co 3 O 4 The crystal spacing can influence the intercalation and deintercalation of Li+ in a lithium ion battery, and layered Co is seen in high-power TEM image results 3 O 4 The lattice spacing of the lithium ion composite material is 0.46nm, and the wider lattice spacing is favorable for the transmission of lithium ions and improves the specific capacity of the material.
The foregoing embodiments have been provided for the purpose of illustrating the general principles of the present invention, and are not to be construed as limiting the scope of the invention. It should be noted that any modifications, equivalent substitutions, improvements, etc. made by those skilled in the art without departing from the spirit and principles of the present invention are intended to be included in the scope of the present invention.
Claims (9)
1. Layered Co 3 O 4 The preparation method of the lithium ion battery anode material is characterized by comprising the following steps:
s1, weighing Co (NO) 3 ) 2 ·6H 2 O and CoCl 3 ·6H 2 O is added into the morphology guiding agent to prepare a precursor solution;
s2, stirring the precursor solution, and then performing solvothermal reaction to prepare a solid suspension;
s3, filtering the solid suspension to retain a solid product, and cleaning and drying the solid product to obtain a precursor beta-Co (OH) 2 ；
S4, preparing the precursor beta-Co (OH) 2 Heating and calcining in air atmosphere to obtain layered Co 3 O 4 ；
Wherein the morphology guiding agent is a mixed solution of ammonia water and ethylene glycol; in the S1, the Co (NO 3 ) 2 ·6H 2 O and CoCl 3 ·6H 2 The molar ratio of O is 1:1.
2. a layered product as defined in claim 1Co 3 O 4 The preparation method of the lithium ion battery anode material is characterized in that in the S4, the calcination is to precursor beta-Co (OH) 2 Heating to 450-550 ℃ in an air atmosphere, heating up at a rate of 1 ℃/min, and then keeping the temperature constant for 1-3 h.
3. A layered Co according to claim 1 3 O 4 The preparation method of the lithium ion battery anode material is characterized in that in the S1, the mass fraction of ammonia water in the morphology guiding agent is 5% -10%.
4. A layered Co according to claim 1 3 O 4 The preparation method of the lithium ion battery anode material is characterized in that in the S1, the concentration of the precursor solution is 0.2mol/L-0.6mol/L.
5. A layered Co according to claim 1 3 O 4 The preparation method of the lithium ion battery anode material is characterized in that in the step S2, the solvothermal reaction is that the precursor solution after stirring is placed in reaction equipment at 180-250 ℃ for 12-24 h.
6. A layered Co according to claim 1 3 O 4 The preparation method of the lithium ion battery anode material is characterized in that in the step S3, ethanol and deionized water are adopted for cleaning the solid-phase product in sequence.
7. A layered Co according to claim 1 3 O 4 The preparation method of the lithium ion battery anode material is characterized in that in the step S3, the solid-phase product is dried for 24 hours at the temperature of 60 ℃.
8. A layered Co according to claim 1 3 O 4 The preparation method of the lithium ion battery anode material is characterized in that in the step S2, the stirring time is 1h-2h.
9. Layered Co 3 O 4 The lithium ion battery cathode material is characterized by comprising layered Co for preparing the lithium ion battery cathode material 3 O 4 The layered Co 3 O 4 Use of a layered Co according to any one of claims 1-8 3 O 4 The layered Co is prepared by a preparation method of a lithium ion battery anode material 3 O 4 Is a layered stacked structure, the layered Co 3 O 4 The stacked bar-shaped profile is formed.
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