CN113921807A - Flexible lithium/sodium ion battery negative electrode material and preparation method thereof - Google Patents
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Abstract
本发明公开了一种柔性锂/钠离子电池负极材料及其制备方法，所述柔性电极材料采用静电纺丝的方法，将氧化锰均匀分布在一维碳纤维上，形成竹节状的柔性电极，碳纤维直径约为700nm。将乙酸锌、乙酸锰和聚丙烯腈搅拌分散到二甲基甲酰胺溶液中，形成均匀的纺丝前驱体；将纺丝前驱体液转移到注射器中，调整适当的纺丝条件，制备出纤维膜前驱体；随后利用热处理方法，将前驱体纤维膜进行碳化，最终制备出尺寸可控，柔性极好的竹节状氧化锰纤维膜，工艺简单、成本低廉，所得的竹节状氧化锰纤维膜具有优良的电化学性能。The invention discloses a flexible lithium/sodium ion battery negative electrode material and a preparation method thereof. The flexible electrode material adopts an electrospinning method to uniformly distribute manganese oxide on one-dimensional carbon fibers to form a bamboo-shaped flexible electrode, The carbon fiber diameter is about 700nm. Stir and disperse zinc acetate, manganese acetate and polyacrylonitrile into dimethylformamide solution to form a uniform spinning precursor; transfer the spinning precursor liquid to a syringe, adjust the appropriate spinning conditions, and prepare a fiber membrane The precursor; then the precursor fiber membrane is carbonized by a heat treatment method, and finally a bamboo-shaped manganese oxide fiber membrane with controllable size and excellent flexibility is prepared. The process is simple and the cost is low. The obtained bamboo-shaped manganese oxide fiber membrane Has excellent electrochemical properties.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to a flexible lithium/sodium ion battery negative electrode material prepared by adopting an electrostatic spinning and high-temperature calcination method and a preparation method thereof.
Background
The lithium/sodium ion battery has the advantages of high energy density, good reversibility and the like, and becomes a main energy storage device in the field of energy storage. However, how to develop a higher performance battery to meet the increasing market demand becomes a current research hotspot. In flexible wearable devices, flexible energy storage batteries become critical, wherein flexible electrode materials are also important. The manganese-based metal oxide has the advantages of rich raw materials, safety, no toxicity, no pollution to the environment, high theoretical specific capacity and the like, and meanwhile, the manganese-based oxide has a lower working voltage platform, so that when the manganese-based oxide is used as a battery negative electrode material, the manganese-based metal oxide has higher output voltage, can improve the output current of a battery, and is low in price, so that the manganese-based metal oxide is favored by scientists.
In recent years, manganese oxide has been the focus of research on lithium/sodium ion batteries with its good electrochemical properties, however, during the research, it was found that when manganese oxide is used as a lithium/sodium ion negative electrode material, there are the following disadvantages: during charging and discharging, the volume changes greatly; the pulverization phenomenon is easy to generate, so that the active substance is not in contact with the current collector, and the cycle performance is poor; its electron conductivity is poor during charging and discharging.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the flexible lithium/sodium ion battery cathode material and the preparation method thereof, the production process is simple, the cost is low, and the prepared manganese oxide has a bamboo-joint-shaped structure, ultrahigh flexibility and excellent electrochemical performance.
The purpose of the invention is realized by the following technical scheme:
the battery cathode material consists of carbon fibers and manganese oxide particles uniformly distributed on the surfaces of the carbon fibers, wherein the diameter of the carbon fibers is 100-1000 nm, and the diameter of the manganese oxide particles distributed on the surfaces of the carbon fibers is 100-1000 nm.
Furthermore, the manganese oxide is distributed on the surface of the carbon fiber in a bamboo joint shape, the diameter of the carbon fiber is 700nm, and the diameter of manganese oxide particles distributed on the surface of the carbon fiber is 200-900 nm.
The preparation method of the flexible lithium/sodium ion battery negative electrode material comprises the following steps:
(1) stirring and dispersing zinc acetate, manganese acetate and polyacrylonitrile into a dimethylformamide solution to form a uniform spinning precursor solution;
(2) transferring the spinning precursor solution obtained in the step (1) into an injector, and preparing a precursor fiber film through electrostatic spinning;
(3) putting the precursor fiber film obtained in the step (2) into a tubular furnace for pre-oxidation, wherein the protective atmosphere is nitrogen, and the heating and cooling speeds are both 1 ℃/min, so as to obtain a pre-oxidized precursor fiber film;
(4) and (4) putting the preoxidized precursor fiber film obtained in the step (3) into a tubular furnace, and carrying out high-temperature carbonization, wherein the heating and cooling speeds are both 1 ℃/min, and the protective atmosphere is nitrogen, so as to finally obtain the flexible lithium/sodium ion battery negative electrode material.
Further, the mass ratio of the zinc acetate to the manganese acetate to the polyacrylonitrile is 0.01-0.6: 0.01-0.8: 0.1 to 1.5.
Further, the volume of the dimethylformamide solution was 6 ml.
Further, the advancing speed of the injection pump in the spinning condition is 0.01-0.5 cm/min, the spinning voltage is 8-15 Kv, and the distance between the receiving roller and the foremost end of the injector is 8-20 cm.
Further, the precursor fiber film is put into a tube furnace for pre-oxidation treatment, in order to ensure good flexibility, the pre-oxidation temperature is 200-400 ℃, and the pre-oxidation treatment is carried out by heating to the pre-oxidation temperature at the speed of 1 ℃/min.
Further, carbonizing the pre-oxidized fiber membrane in a tubular furnace to realize the oxidation of zinc source volatile manganese acetate, wherein the high-temperature carbonization time is set to be 1-5h and the carbonization temperature is set to be 700-1200 ℃ to obtain the bamboo-like structure.
The invention can prepare the flexible lithium/sodium ion battery cathode material with uniform and controllable size, the manganese oxide with the structure takes the carbon fiber as a conductor, and the manganese oxide is connected in series to form a bamboo-joint structure, thereby greatly improving the conductivity of the electrode material and inhibiting the pulverization phenomenon to a great extent; meanwhile, the structure of the electrode material does not need an additional current collector, and compared with a copper foil, the mass density of the carbon fiber is far lower than that of the copper foil, so that the overall mass energy density of the electrode material is greatly improved; the electrode material prepared by the method has good flexibility, can still recover the original shape after being bent for many times, and simultaneously keeps the original electrochemical performance; in addition, the production process adopted by the invention is simple, the cost is low, and the prepared bamboo-shaped manganese oxide has excellent electrochemical performance.
Drawings
FIG. 1 is a field emission topographic map of the negative electrode material of the flexible lithium/sodium ion battery prepared in example 4 of the present invention;
FIG. 2 is a transmission electron microscope topography of the negative electrode material of the flexible lithium/sodium ion battery prepared in embodiment 4 of the invention;
FIG. 3 is a charge-discharge cycle curve of the flexible bamboo-like manganese oxide prepared in example 5 of the present invention as a negative electrode material of a lithium ion battery;
fig. 4 is a flexibility test chart of the flexible bamboo-like manganese oxide prepared in example 5 of the present invention as a negative electrode material of a lithium ion battery.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Example 1
The preparation method of the flexible lithium/sodium ion battery negative electrode material specifically comprises the following steps:
1) stirring and dispersing 0.01g of zinc acetate, 0.02g of manganese acetate and 0.2g of polyacrylonitrile into 6ml of dimethylformamide solution to form a spinning precursor solution;
2) transferring the obtained precursor solution into an injector, wherein the propelling speed of an injection pump is 0.01cm/min, the spinning voltage is 13kV, and the distance between a receiving roller and the foremost end of the injector is 8cm, so as to prepare a precursor fiber film;
3) putting the obtained precursor fiber film into a tube furnace for pre-oxidation, wherein the temperature is set to be 200 ℃, the temperature rising speed is 1 ℃/min, the pre-oxidation time is 1h, and the pre-oxidation precursor fiber film is obtained in a nitrogen atmosphere;
4) and putting the obtained pre-oxidized precursor fiber film into a tubular furnace, and carrying out high-temperature carbonization at 700 ℃, with the temperature rise and temperature reduction speed of 1 ℃/min, the carbonization time of 2h and the nitrogen atmosphere to finally obtain the flexible lithium/sodium ion battery cathode material, wherein the size of the prepared carbon fiber is about 400nm, and the diameter of manganese oxide distributed on the surface of the carbon fiber is about 300 nm.
Example 2
1) Stirring and dispersing 0.02g of zinc acetate, 0.04g of manganese acetate and 0.3g of polyacrylonitrile into 6ml of dimethylformamide solution to form a spinning precursor solution;
2) transferring the obtained precursor solution into an injector, wherein the propelling speed of an injection pump is 0.02cm/min, the spinning voltage is 13.5kV, and the distance between a receiving roller and the foremost end of the injector is 8.5cm, so as to prepare a precursor fiber film;
3) putting the obtained precursor fiber film into a tube furnace for pre-oxidation, setting the temperature at 210 ℃, the heating and cooling speeds at 1 ℃/min, the pre-oxidation time at 1h and nitrogen atmosphere to obtain a pre-oxidized precursor fiber film;
4) and putting the obtained pre-oxidized precursor fiber film into a tubular furnace, and carrying out high-temperature carbonization at the temperature of 750 ℃, at the temperature rise and temperature reduction speeds of 1 ℃/min and in the carbonization time of 2h in a nitrogen atmosphere to finally obtain the flexible lithium/sodium ion battery cathode material, wherein the size of the prepared carbon fiber is about 500nm, and the diameter of manganese oxide distributed on the surface of the carbon fiber is 400 nm.
Example 3
1) Stirring and dispersing 0.05g of zinc acetate, 0.1g of manganese acetate and 0.6g of polyacrylonitrile into 6ml of dimethylformamide solution to form a spinning precursor solution;
2) transferring the obtained precursor solution into an injector, wherein the propelling speed of an injection pump is 0.05cm/min, the spinning voltage is 14 kV, and the distance between a receiving roller and the foremost end of the injector is 8.5cm, so as to prepare a precursor fiber film;
3) placing the obtained precursor fiber film into a tube furnace for pre-oxidation, setting the temperature at 220 ℃, the heating and cooling speeds at 1 ℃/min, the pre-oxidation time at 1h and nitrogen atmosphere to obtain a pre-oxidized precursor fiber film;
4) and putting the obtained pre-oxidized precursor fiber film into a tubular furnace, and carrying out high-temperature carbonization at the temperature of 750 ℃, at the temperature rise and temperature reduction speeds of 1 ℃/min and in the carbonization time of 2h in a nitrogen atmosphere to finally obtain the flexible lithium/sodium ion battery cathode material, wherein the size of the prepared carbon fiber is about 600nm, and the diameter of manganese oxide distributed on the surface of the carbon fiber is about 500 nm.
Example 4
1) Stirring and dispersing 0.1g of zinc acetate, 0.2g of manganese acetate and 0.7g of polyacrylonitrile into 6ml of dimethylformamide solution to form a spinning precursor solution;
2) transferring the obtained precursor solution into an injector, wherein the propelling speed of an injection pump is 0.1cm/min, the spinning voltage is 15kV, and the distance between a receiving roller and the foremost end of the injector is 8.5cm, so as to prepare a precursor fiber film;
3) putting the obtained precursor fiber film into a tubular furnace for pre-oxidation, setting the temperature at 240 ℃, the heating and cooling speeds at 1 ℃/min, the pre-oxidation time at 1h and nitrogen atmosphere to obtain a pre-oxidized precursor fiber film;
4) and (2) putting the obtained pre-oxidized precursor fiber membrane into a tubular furnace, performing high-temperature carbonization at 800 ℃, with the temperature rise and temperature reduction speed of 1 ℃/min, the carbonization time of 2h and the nitrogen atmosphere, and finally obtaining the flexible lithium/sodium ion battery cathode material, wherein the size of the prepared carbon fiber is 700nm, the manganese oxide is bamboo-shaped and is uniformly distributed on the surface of the carbon fiber, and the electrode material prepared by the process has good uniformity as shown in figure 2.
Example 5
1) Stirring and dispersing 0.15g of zinc acetate, 0.3g of manganese acetate and 0.8g of polyacrylonitrile into 6ml of dimethylformamide solution to form a spinning precursor solution;
2) transferring the obtained precursor solution into an injector, wherein the propelling speed of an injection pump is 0.1cm/min, the spinning voltage is 15kV, and the distance between a receiving roller and the foremost end of the injector is 9cm, so as to prepare a precursor fiber film;
3) putting the obtained precursor fiber film into a tubular furnace for pre-oxidation, setting the temperature at 240 ℃, the heating and cooling speeds at 1 ℃/min, the pre-oxidation time at 1h and nitrogen atmosphere to obtain a pre-oxidized precursor fiber film;
4) and putting the obtained pre-oxidized precursor fiber film into a tubular furnace, and carrying out high-temperature carbonization at 850 ℃, wherein the temperature is set to be 1 ℃/min, the temperature rising and reducing speed is 2 ℃/min, the carbonization time is 2h, and the nitrogen atmosphere is adopted, so that the flexible lithium/sodium ion battery cathode material is finally obtained, the size of the prepared carbon fiber is about 800nm, and the diameter of manganese oxide distributed on the surface of the carbon fiber is about 700 nm.
In a charging and discharging circulation curve of the flexible bamboo-like manganese oxide serving as the lithium ion battery cathode material in the graph of fig. 3, the flexible bamboo-like manganese oxide circulates for 100 circles under the current density of 100 mA/g, and the discharge capacity of the flexible bamboo-like manganese oxide reaches 851 mAh/g, which shows that the flexible bamboo-like manganese oxide prepared by the method has good charging and discharging circulation performance and charging and discharging capacity.
In the figure 4, when the flexible bamboo-shaped manganese oxide is used as the negative electrode material of the lithium ion battery, the material can be bent for many times and still can rebound after being bent, which shows that the material has good flexibility.
Example 6
1) Stirring and dispersing 0.2g of zinc acetate, 0.4g of manganese acetate and 0.9g of polyacrylonitrile into 6ml of dimethylformamide solution to form a spinning precursor solution;
2) transferring the obtained precursor solution into an injector, wherein the propelling speed of an injection pump is 0.1cm/min, the spinning voltage is 15kV, and the distance between a receiving roller and the foremost end of the injector is 11cm, so as to prepare a precursor fiber film;
3) putting the obtained precursor fiber film into a tubular furnace for pre-oxidation, setting the temperature at 270 ℃, the heating and cooling speeds at 1 ℃/min, the pre-oxidation time at 1h, the carbonization time at 2h, and obtaining a pre-oxidized precursor fiber film in a nitrogen atmosphere;
4) and putting the obtained pre-oxidized precursor fiber film into a tubular furnace, and carrying out high-temperature carbonization at 850 ℃, wherein the temperature is set to be 1 ℃/min, the temperature rising and reducing speed is 2 ℃/min, the carbonization time is 2h, and the nitrogen atmosphere is adopted, so that the flexible lithium/sodium ion battery cathode material is finally obtained, the size of the prepared carbon fiber is about 900nm, and the diameter of manganese oxide distributed on the surface of the carbon fiber is about 800 nm.
Example 7
1) Stirring and dispersing 0.2g of zinc acetate, 0.4g of manganese acetate and 1g of polyacrylonitrile into 6ml of dimethylformamide solution to form spinning precursor solution;
2) transferring the obtained precursor solution into an injector, wherein the propelling speed of an injection pump is 0.3cm/min, the spinning voltage is 15V, and the distance between the receiving roller and the foremost end of the injector is 13cm, so as to prepare a precursor fiber film;
3) putting the obtained precursor fiber film into a tubular furnace for pre-oxidation, setting the temperature at 280 ℃, the heating and cooling speeds at 1 ℃/min, the pre-oxidation time at 1h and nitrogen atmosphere to obtain a pre-oxidized precursor fiber film;
4) and putting the obtained pre-oxidized precursor fiber film into a tubular furnace, and carrying out high-temperature carbonization at 900 ℃, wherein the temperature rise and temperature fall speed is 1 ℃/min, the carbonization time is 2h, and the nitrogen atmosphere is adopted, so that the flexible lithium/sodium ion battery cathode material is finally obtained, the size of the prepared carbon fiber is about 1000nm, and the diameter of manganese oxide distributed on the surface of the carbon fiber is 900 nm.
Example 8
1) Stirring and dispersing 0.2g of zinc acetate, 0.4g of manganese acetate and 1.2g of polyacrylonitrile into 6ml of dimethylformamide solution to form a spinning precursor solution;
2) transferring the obtained precursor solution into an injector, wherein the propelling speed of an injection pump is 0.35cm/min, the spinning voltage is 15kV, and the distance between the receiving roller and the foremost end of the injector is 15cm, so as to prepare a precursor fiber film;
3) putting the obtained precursor fiber film into a tubular furnace for pre-oxidation, setting the temperature at 290 ℃, the heating and cooling speeds at 1 ℃/min, the pre-oxidation time at 1h and nitrogen atmosphere to obtain a pre-oxidized precursor fiber film;
4) and putting the obtained pre-oxidized precursor fiber film into a tubular furnace, and carrying out high-temperature carbonization at 950 ℃, wherein the temperature rise and temperature reduction speed is 1 ℃/min, the carbonization time is 2h, and the nitrogen atmosphere is adopted, so that the flexible lithium/sodium ion battery cathode material is finally obtained, the size of the prepared carbon fiber is about 1000nm, and the diameter of manganese oxide distributed on the surface of the carbon fiber is about 1000 nm.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in the embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
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Application publication date: 20220111 |