CN111778585A - Cobalt nanofiber lithium battery negative electrode material and preparation method thereof - Google Patents
Cobalt nanofiber lithium battery negative electrode material and preparation method thereof Download PDFInfo
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- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention discloses a cobalt nano-fiber lithium battery cathode material and a preparation method thereof, wherein 4,4' - (1, 3-propanediyl) bipyridine and cobalt metal ions are matched with metal cobalt ion salts as main raw materials, and cobalt nano-fibers are successfully prepared by utilizing an electrostatic spinning technology and a high-temperature sintering technologyIs a lithium ion battery material, and has a current density of 100 mA g‑1After charging and discharging under the condition for 150 cycles, the specific capacity is still more than 380 mAh g‑1. In the whole preparation process, the operation is simple, the cost is low, the equipment investment is low, and the method is suitable for batch production.
Description
Technical Field
The invention relates to the technical field of lithium battery materials, in particular to a cobalt nanofiber lithium battery negative electrode material and a preparation method thereof.
Background
With the progress and development of human society, problems such as energy shortage and environmental pollution become more serious, and countries around the world begin to recognize the severity and urgency of the problems, one of the solutions to the problems is to vigorously develop clean and renewable energy sources such as solar energy, wind energy, geothermal energy, tidal energy, etc., but they are easily affected by uncontrollable factors such as seasonality, regionality, instability and the like, greatly limit the application of the same, therefore, research on stable and reliable energy storage and conversion devices becomes one of the key technologies, the electric energy storage system mainly comprises a battery system and a super capacitor system, at present, the two energy storage systems are not mature enough, even if the development is sufficient, it is still insufficient to meet the requirements of new energy vehicles, the performance, cycle life and safety of battery systems require further research, and the development of new electrode materials still requires the efforts of researchers of one generation and another.
Metal-organic frameworks (MOFs), which are porous materials first defined in 1995 by O.M. Yaghi et al (Journal of the American chemical Society, 1995, 117, 10401-10402), are widely used in energy storage and conversion devices due to their advantages of high porosity, functional diversity, structural diversity and controllable chemical composition, and in the last decade, two thousand MOFs (H. Furukawa et al, Science, 2013, 341, 1230444) and their derivatives have been found to be excellent in Lithium Ion Batteries (LIBs), Lithium Sulfur Batteries (LSBs), Lithium Oxygen Batteries (LOBs) and Sodium Ion Batteries (SIBs), where LIBs are widely used and are promising batteries, and are themselves lightweight, high energy density, and high energy density batteries, The advantages of long cycle life, wide working temperature range, no memory effect, environmental friendliness and the like gradually become commonly used energy storage equipment, become an important direction for the development of secondary batteries, and are widely applied to the fields of electronic products, electric automobiles, military aerospace and the like. The theoretical specific capacitance of the traditional lithium battery graphite negative electrode material is 372 mAh g-1Theoretical specific volume thereofLow amount, poor reaction kinetics, lithium dendrite generation upon discharge to a lower voltage, easy formation of SEI film, and thus, scientists are actively developing other types of materials.
By nano-material is meant a material with a grain size on the order of nanometers (10)-9nm) and nano-materials have wide application prospect due to unique surface effect, volume effect and quantum size effect. The synthesis method of the one-dimensional nano material mainly comprises a phase transfer method, a hydrothermal method, an electrostatic spinning method, a chemical vapor deposition method, a vapor phase evaporation method and the like, wherein the electrostatic spinning technology is the simplest and most effective method for preparing the continuous nano fiber. The electrostatic spinning device mainly comprises three parts: the electrostatic spinning fiber appearance is mainly influenced by system parameters (such as molecular weight of polymer, conductivity, viscosity and dielectric constant of precursor solution), operation parameters (such as specification of a needle head, voltage, flow rate, distance between a spinning nozzle and a collecting plate), environmental parameters (such as humidity, temperature and the like, and annealing temperature, calcining atmosphere, temperature rise and the like of spinning fibers).
Chinese invention patent CN107579238A discloses a cobaltosic oxide-FTO nanowire lithium battery negative electrode material and a preparation method thereof. The patent adopts a nano-fiber material with surface micropores prepared by an air spinning method, and the nano-fiber material is prepared at 400 mA g-1After 20 cycles at the current density of (1), the discharge capacity and the charge capacity were respectively 801 mAh g-1And 750 mAh g-1The coulombic efficiency was 93.63%. The coulombic efficiency of the nanofiber material still needs to be improved.
The invention aims to solve the technical problem of the prior art and provides a cobalt nanofiber lithium battery cathode material and a preparation method thereof.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a cobalt nanofiber lithium battery cathode material and a preparation method thereof.
The technical scheme of the invention is as follows:
a preparation method of a cobalt nanofiber lithium battery cathode material comprises the steps of taking 4,4' - (1, 3-propanediyl) bipyridine and cobalt acetate tetrahydrate as main raw materials, adding a proper amount of high-molecular polyacrylonitrile as an adhesive, magnetically stirring for a period of time to obtain a clear and transparent spinning precursor solution, preparing an electrostatic spinning product under a high-voltage condition by using an electrostatic spinning technology, and then annealing and sintering in a tubular furnace at the temperature of 650-850 ℃ under the nitrogen condition.
A preparation method of a cobalt nanofiber lithium battery negative electrode material specifically comprises the following steps:
(1) adding N, N-dimethylformamide into a beaker, adding 4,4' - (1, 3-propanediyl) bipyridine and cobalt acetate tetrahydrate, adding a proper amount of Polyacrylonitrile (PAN) serving as a binder into the beaker, and magnetically stirring to obtain a red gel spinning solution;
(2) the red gel spinning solution is filled into an injector, the voltage is 15-19 kV, the distance between a spinning needle and a receiver is 10-20 cm, and the propelling flow rate is 0.8 mL h-1Carrying out electrostatic spinning at the relative humidity of 22-27% and the temperature of 30 ℃, collecting spinning products after 8-12 h of spinning, and drying the spinning products in a blast drying oven at the temperature of 85-95 ℃ for 30-40 min;
(3) adding methanol into a beaker, adding 3.0mmol of cobalt acetate tetrahydrate, and magnetically stirring to obtain a 0.05mmol/mL cobalt acetate methanol solution;
(4) immersing the dried electrostatic spinning product into the cobalt acetate methanol solution for 8-12 h, taking out the spinning product, and drying in a forced air drying oven at 85-95 ℃ for 30-40 min to obtain a spinning product with cobalt acetate attached to the surface;
(5) and (3) placing the spinning product with the cobalt acetate attached to the surface in a porcelain boat, carrying out procedure annealing at 650-850 ℃ in a tubular furnace under the nitrogen atmosphere, and cooling to room temperature to obtain the cobalt nanofiber lithium battery cathode material.
Preferably, in the step (1), the molar ratio of 4,4' - (1, 3-propanediyl) bipyridine to cobalt acetate tetrahydrate is 1: 1.
preferably, in the step (5), the process annealing step is: heating from room temperature to 200 deg.C for 120min to stabilize fiber configuration, and heating at 2 deg.C for min-1(ii) a Heating from 200 ℃ to 650-850 ℃ and keeping for 120min, wherein the heating rate is 3 ℃ for min-1。
The obtained cobalt nanofiber is used as a negative electrode material of a lithium battery and has a current density of 100 mA g-1Under the condition, after 150 times of charge-discharge circulation, the specific discharge capacity can be kept at 380 mAh g-1Above that, the coulombic efficiency can be maintained at 99.98%.
The invention has the advantages that:
(1) the electrostatic spinning technology is adopted to firstly synthesize the organic metal framework nanofiber, then the oxygen-insulated high-temperature sintering technology is adopted to convert the organic components into the carbon/nitrogen-containing two-dimensional material, so that the cobalt ions reduce the nano cobalt simple substance, and the carbon/nitrogen two-dimensional material is coated on the surface of the cobalt simple substance, thereby improving the specific energy storage capacity of the material;
(2) the prepared nano-fibers are uniform, have the diameter of 300-350 nm and large specific surface area, support the intercalation/deintercalation of lithium ions in a larger range and are beneficial to improving the lithium ion conduction rate in the charging and discharging process;
(3) the prepared nano-fiber is used as a lithium ion battery cathode material and has a current density of 100 mA g-1Under the condition, after charging and discharging are circulated for 150 circles, the specific capacity can still be kept at 380 mAh g-1Greater than the theoretical specific capacity of graphite (372 mAh g)-1) The performance is excellent;
(4) the XRD of the prepared nano-fiber is shown in figure 1, the stability is high, the crystallinity is good (ICCD file No: 00-015-0806), and the peak with the angle of 25 degrees is the peak of a carbon or nitrogen matrix.
Drawings
FIG. 1 is an XRD pattern of a negative electrode material of a cobalt nanofiber lithium battery prepared in example 3 of the present invention;
FIG. 2 is an SEM image of the cathode material of the cobalt nanofiber lithium battery prepared in example 3 of the present invention;
fig. 3 is a charge-discharge cycle diagram of the negative electrode material of the cobalt nanofiber lithium battery prepared in example 3 of the present invention.
Detailed Description
The solvents and synthetic raw materials described in the following examples are all chemically pure.
Example 1
15 mL of N, N-dimethylformamide as a solvent was added to a 50 mL beaker, and 0.5 mmoL (0.0991 g) of 4,4' - (1, 3-propanediyl) bipyridine and 0.5 mmoL (0.1245 g) of cobalt acetate tetrahydrate (C)4H6CoO4·4H2O), adding 1.45 g of Polyacrylonitrile (PAN) serving as a binder into the beaker, and magnetically stirring for 2 hours to obtain a red gel spinning solution; the red gel spinning solution was loaded into a 10 mL syringe at a spinning needle to receiver distance of 10 cm at 15 kV and a boost flow rate of 0.8 mL h-1Carrying out electrostatic spinning at the temperature of 30 ℃ and the box body humidity of 22%, collecting spinning products in a beaker after spinning for 12 hours, and drying for 30min in a blast drying oven at the temperature of 85 ℃; adding 60 mL of methanol into a 100 mL beaker, adding 3.0mmol of cobalt acetate tetrahydrate, and magnetically stirring for 0.5 h to completely dissolve the cobalt acetate tetrahydrate to obtain a 0.05mmol/mL cobalt acetate methanol solution; immersing the dried electrostatic spinning product into the cobalt acetate methanol solution, taking out the electrostatic spinning product after 8 hours, naturally airing, and drying in an air blast drying oven at 95 ℃ for 0.5 hour to obtain a spinning product with the cobalt acetate attached to the surface; placing the spinning product with the cobalt acetate attached on the surface in a porcelain boat, carrying out programmed annealing at 650 ℃ in a tube furnace under the nitrogen atmosphere, setting a heating program, heating from room temperature to 200 ℃ and keeping for 120min, wherein the heating rate is 2 ℃ for min-1(ii) a Heating from 200 deg.C to 650 deg.C for 120min at a heating rate of 3 deg.C for min-1Cooling to room temperature to obtain a cobalt nanofiber lithium battery cathode material; subjecting the product to X-ray powder diffraction test, scanning electron microscope test and test on100 mAg-1And testing the charge-discharge cycle performance of the lithium ion battery cathode material under the current density.
Example 2
15 mL of N, N-dimethylformamide as a solvent was added to a 50 mL beaker, and 0.5 mmoL (0.0991 g) of 4,4' - (1, 3-propanediyl) bipyridine and 0.5 mmoL (0.1245 g) of cobalt acetate tetrahydrate (C)4H6CoO4·4H2O), adding 1.45 g of Polyacrylonitrile (PAN) serving as a binder into the beaker, and magnetically stirring for 2 hours to obtain a red gel spinning solution; the red gel spinning solution was loaded into a 10 mL syringe at a voltage of 19 kV with a spinning needle 20cm from the receiver and a push flow rate of 0.8 mL h-1Carrying out electrostatic spinning at the temperature of 30 ℃ and the box body humidity of 27%, collecting spinning products in a beaker after spinning for 8 hours, and drying for 40min in a blast drying oven at the temperature of 95 ℃; adding 60 mL of methanol into a 100 mL beaker, adding 3.0mmol of cobalt acetate tetrahydrate, and magnetically stirring for 0.5 h to completely dissolve the cobalt acetate tetrahydrate to obtain a 0.05mmol/mL cobalt acetate methanol solution; immersing the dried electrostatic spinning product into the cobalt acetate methanol solution, taking out the electrostatic spinning product after 12 hours, naturally airing, and drying in a forced air drying oven at 85 ℃ for 30min to obtain a spinning product with cobalt acetate attached to the surface; placing the spinning product with the cobalt acetate attached on the surface in a porcelain boat, carrying out programmed annealing at 850 ℃ in a tube furnace under the nitrogen atmosphere, heating to 200 ℃ from room temperature, keeping the temperature for 120min to stabilize the fiber configuration, and heating at the rate of 2 ℃ for min-1(ii) a Heating from 200 deg.C to 850 deg.C for 120min at a heating rate of 3 deg.C for min-1Cooling to room temperature to obtain a cobalt nanofiber lithium battery cathode material; the product was subjected to X-ray powder diffraction testing, scanning electron microscopy and at 100 mA g-1And testing the charge-discharge cycle performance of the lithium ion battery cathode material under the current density.
Example 3
15 mL of N, N-dimethylformamide as a solvent was added to a 50 mL beaker, followed by 0.5 mmoL (0.0991 g) of 4,4' - (1, 3-propanediyl) bipyridine and 0.5 mmoL (0.1245 g) of cobalt acetate-tetrakisAdding 1.45 g of polyacrylonitrile serving as a binder into the beaker after the hydrate is hydrated, and magnetically stirring for 2 hours to obtain a red gel spinning solution; the red gel spinning solution was loaded into a 10 mL syringe at a 17 kV voltage with a spinning needle 15 cm from the receiver and a boost flow rate of 0.8 mL h-1Carrying out electrostatic spinning at the temperature of 30 ℃ and the box body humidity of 25%, collecting spinning products in a beaker after 10 hours of spinning, and drying for 35min in a 90 ℃ blast drying oven; adding 60 mL of methanol into a 100 mL beaker, adding 3.0mmol of cobalt acetate tetrahydrate, and magnetically stirring for 0.5 h to completely dissolve the cobalt acetate tetrahydrate to obtain a 0.05mmol/mL cobalt acetate methanol solution; immersing the dried electrostatic spinning product into the cobalt acetate methanol solution, taking out the electrostatic spinning product after 10 hours, naturally airing, and drying in a forced air drying oven at 90 ℃ for 32min to obtain a spinning product with cobalt acetate attached to the surface; placing the spinning product with the cobalt acetate attached on the surface in a porcelain boat, carrying out programmed annealing at 750 ℃ in a tube furnace under the nitrogen atmosphere, heating to 200 ℃ from room temperature and keeping for 120min, wherein the heating rate is 2 ℃ for min-1(ii) a Heating from 200 deg.C to 750 deg.C for 120min at a heating rate of 3 deg.C for min-1Cooling to room temperature to obtain a cobalt nanofiber lithium battery cathode material; the product was subjected to X-ray powder diffraction testing (FIG. 1), scanning electron microscopy testing (FIG. 2) and at 100 mA g-1The lithium ion battery negative electrode material is tested to have charge-discharge cycle performance under current density, and after 150 times of charge-discharge cycle, the specific discharge capacity can be maintained at 380 mAh.g-1Above, the coulombic efficiency can be maintained at 99.98% (fig. 3).
The following examples 1 to 3 were conducted on the negative electrode material of cobalt nanofiber lithium battery prepared in accordance with the present invention at a current density of 100 mA g-1Under the condition, the specific discharge capacity and the coulombic efficiency after 150 times of charge-discharge circulation are detected, and specific data are shown in table 1.
Table 1:
| example 1 | Example 2 | Example 3 | |
| Specific discharge capacity (mAh. g) after 150 cycles of charge and discharge-1） | 375 | 372 | 380 |
| Coulombic efficiency (%) | 99.92 | 99.94 | 99.98 |
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. The preparation method of the cobalt nanofiber lithium battery negative electrode material is characterized by comprising the following steps of: the preparation method comprises the steps of taking 4,4' - (1, 3-propanediyl) bipyridine and cobalt acetate tetrahydrate as main raw materials, adding a proper amount of high-molecular polyacrylonitrile as an adhesive, magnetically stirring for a period of time to obtain a clear and transparent spinning precursor solution, preparing an electrostatic spinning product by using an electrostatic spinning technology under a high-voltage condition, and then annealing and sintering in a tubular furnace at 650-850 ℃ under a nitrogen condition.
2. The preparation method of the negative electrode material of the cobalt nanofiber lithium battery as claimed in claim 1, which comprises the following steps:
(1) adding N, N-dimethylformamide into a beaker, adding 4,4' - (1, 3-propanediyl) bipyridine and cobalt acetate tetrahydrate, adding a proper amount of polyacrylonitrile serving as a binder into the beaker, and magnetically stirring to obtain a red gel spinning solution;
(2) the red gel spinning solution is filled into an injector, the voltage is 15-19 kV, the distance between a spinning needle and a receiver is 10-20 cm, and the propelling flow rate is 0.8 mL h-1Carrying out electrostatic spinning at the relative humidity of 22-27% and the temperature of 30 ℃, collecting spinning products after 8-12 h of spinning, and drying the spinning products in a blast drying oven at the temperature of 85-95 ℃ for 30-40 min;
(3) adding methanol into a beaker, adding 3.0mmol of cobalt acetate tetrahydrate, and magnetically stirring to obtain a 0.05mmol/mL cobalt acetate methanol solution;
(4) immersing the dried electrostatic spinning product into the cobalt acetate methanol solution for 8-12 h, taking out the spinning product, and drying in a forced air drying oven at 85-95 ℃ for 30-40 min to obtain a spinning product with cobalt acetate attached to the surface;
(5) and (3) placing the spinning product with the cobalt acetate attached to the surface in a porcelain boat, carrying out procedure annealing at 650-850 ℃ in a tubular furnace under the nitrogen atmosphere, and cooling to room temperature to obtain the cobalt nanofiber lithium battery cathode material.
3. The method for preparing the negative electrode material of the cobalt nanofiber lithium battery as claimed in claim 2, wherein in the step (1), the molar ratio of 4,4' - (1, 3-propanediyl) bipyridine to cobalt acetate tetrahydrate is 1: 1.
4. the method for preparing the negative electrode material of the cobalt nanofiber lithium battery as claimed in claim 2, wherein in the step (5), the process annealing step is: heating from room temperature to 200 deg.C for 120min to stabilize fiber configuration, and heating at 2 deg.C for min-1(ii) a Heating from 200 ℃ to 650-850 ℃ and keeping for 120min, wherein the heating rate is 3 ℃ for min-1。
5. The method for preparing a negative electrode material for a cobalt nanofiber lithium battery as claimed in any one of claims 2 to 4, wherein the obtained negative electrode material for a cobalt nanofiber lithium battery has a current density of 100 mA g-1Under the condition, after 150 times of charge-discharge circulation, the specific discharge capacity can be kept at 380 mAh g-1Above that, the coulombic efficiency can be maintained at 99.98%.
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| CN115746321A (en) * | 2022-11-01 | 2023-03-07 | 华中科技大学 | Metal organic gel, preparation method and application thereof |
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| CN115746321A (en) * | 2022-11-01 | 2023-03-07 | 华中科技大学 | Metal organic gel, preparation method and application thereof |
| CN115746321B (en) * | 2022-11-01 | 2023-08-01 | 华中科技大学 | Metal organic gel, preparation method and application thereof |
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Application publication date: 20201016 |