CN107311140B - Preparation method of lithium ion battery negative electrode material - Google Patents
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- CN107311140B CN107311140B CN201710388348.6A CN201710388348A CN107311140B CN 107311140 B CN107311140 B CN 107311140B CN 201710388348 A CN201710388348 A CN 201710388348A CN 107311140 B CN107311140 B CN 107311140B
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Abstract
The invention provides a preparation method of a lithium ion battery cathode material, and relates to the technical field of battery material preparation. The method comprises the following steps: polymerizing cysteine in the presence of an oxidant to obtain a cystine polymer, mixing the cystine polymer with a nitrogen source and a sulfur source to obtain a mixture, and carbonizing the mixture at 240-630 ℃ in an inert atmosphere to obtain the lithium ion battery cathode material, wherein the ratio of the nitrogen source to the sulfur source in the nitrogen-sulfur source is 1: 0.5-3. The method has simple process and low cost, is suitable for industrial production, and in addition, the doping ratio of nitrogen and sulfur can be controlled by the ratio of the cystine polymer, the nitrogen source and the sulfur source and the carbonization temperature, and the specific capacity and the cyclicity of the amorphous porous carbon anode material prepared by the method are obviously improved by the nitrogen/sulfur co-doping.
Description
Technical Field
The invention belongs to the field of battery material preparation, and particularly relates to a preparation method of a lithium ion battery cathode material.
Background
The lithium ion battery is the most important power supply device for portable electronic equipment and electric vehicles at present, and along with the popularization of the portable electronic equipment, the demand for the lithium ion battery is more and more due to the coming times of electric vehicles and smart power grids. The electrode material is a main component of the lithium ion battery, and the quality of the electrode material directly affects the performance of the lithium ion battery, such as specific capacity, voltage, cycle performance or rate performance. Currently, research on electrode materials of lithium ion batteries mainly focuses on positive electrode materials, and research on negative electrode materials is relatively less. In fact, the performance of the lithium ion battery can be more stable due to the proper negative electrode material, and therefore, the search for the proper negative electrode material is crucial to the development of the lithium ion battery technology.
At present, the commercially used negative electrode material is mainly a graphite carbon material, but the lower theoretical specific capacity (372mA h g)-1) Further improvement of the energy density of the lithium ion battery is severely restricted. Therefore, the new energy market urgently needs to develop a novel anode material. The novel carbon-based material is still the most potential lithium ion battery negative electrode material at present. In order to improve the performance of the negative electrode of the lithium ion battery, the negative electrode material is generally required to be doped with hetero atoms. The N/S co-doping is another important means for improving the lithium storage capacity and the rate capability of the lithium ion battery by utilizing the synergistic effect of the diatomic doping after single heteroatom doping such as N doping, S doping and the like. The method not only utilizes N doping to improve the defect position and the conductivity of the carbon material, but also increases the spacing between carbon layers by virtue of S doping, thereby being beneficial to improving the lithium storage capacity and the insertion-extraction of lithium ions between the carbon layers and improving the rate capability of the lithium ion battery.
However, when N, S co-doped carbon is prepared by using the prior art, a synthesis process such as Chemical Vapor Deposition (CVD) is required, a 3D graphene material is prepared by using Graphene Oxide (GO) as a material, or a hollow graphite-like nanosphere is prepared by using metal Ni as a template, so that the preparation process is complex, the preparation cost is high, the preparation can be realized only in a laboratory scale, and the industrialization is difficult. In addition, the doping level of the N, S in the existing preparation process is too low, and the doping amount is uncontrollable, so that the prepared anode material has low specific capacity and poor cycle performance.
Disclosure of Invention
The invention provides a preparation method of a lithium ion battery cathode material, which aims to solve the problems that the conventional preparation method of the lithium ion battery cathode material is complex in process, high in manufacturing cost and difficult to realize industrialization, and also solves the problems that the conventional preparation method N, S is low in doping level, uncontrollable in doping amount, low in specific capacity of the prepared material and poor in cyclicity.
The invention provides a preparation method of a lithium ion battery cathode material, which comprises the following steps:
polymerizing cysteine in the presence of an oxidizing agent to form cystine;
mixing the cystine polymer, a nitrogen source and a sulfur source to obtain a mixture;
carbonizing the mixture at the temperature of 240-630 ℃ in an inert atmosphere to obtain the lithium ion battery negative electrode material;
wherein the molar ratio of the cystine to the nitrogen source to the sulfur source is 2: 1-2: 0.5-3.
According to the preparation method of the lithium ion battery cathode material, provided by the invention, the cystine, the nitrogen and the sulfur source are mixed and then carbonized to obtain the lithium ion battery cathode material, the process is simple, the cost is low, and the preparation method is suitable for industrial production. In the preparation process, the doping ratio of nitrogen and sulfur can be controlled by controlling the ratio of cystine, a nitrogen source and a sulfur source and the carbonization temperature, so that the specific capacity and the cyclicity of the amorphous porous carbon anode material prepared are obviously improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention.
FIG. 1 is a schematic flow chart of a method for preparing a lithium ion battery anode material according to the present invention;
FIG. 2 is a scanning electron microscope test chart of the material prepared by the first embodiment of the present invention;
FIG. 3 is a SEM image of a material prepared according to a fourth embodiment of the present invention.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent 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.
Referring to fig. 1, fig. 1 is a schematic flow chart illustrating an implementation of a method for preparing a negative electrode material of a lithium ion battery according to an embodiment of the present invention, where the method for preparing the negative electrode material of the lithium ion battery shown in fig. 1 mainly includes the following steps:
s101, polymerizing cysteine in the presence of an oxidant to obtain a cystine polymer;
s102, mixing the cystine polymer, a nitrogen source and a sulfur source to obtain a mixture;
s103, carbonizing the mixture at the temperature of 240-630 ℃ in an inert atmosphere to obtain the lithium ion battery negative electrode material.
Wherein the molar ratio of the cystine polymer to the nitrogen source to the sulfur source is 2: 1-2: 0.5-3.
According to the preparation method of the lithium ion battery cathode material provided by the embodiment of the invention, the higher the proportion of the nitrogen source and the sulfur source is, and the lower the carbonization temperature is, the higher the nitrogen-sulfur doping amount of the prepared material is. The material prepared by the embodiment of the invention is amorphous porous carbon, and because the amorphous porous carbon has large specific surface area, a large number of active sites are provided for the storage of lithium ions, the diffusion of electrolyte is facilitated, and the diffusion distance of the lithium ions is reduced due to the porosity of the amorphous porous carbon. In addition, the conductivity of the material is improved by increasing the doping amount of nitrogen elements, the interlayer distance between the materials can be increased by increasing the doping amount of sulfur elements, the improvement of the storage capacity of lithium ions and the insertion-depletion process are facilitated, and the multiplying power performance of the lithium ions can be improved. The prepared amorphous porous carbon material is applied to a lithium ion battery cathode material, the first reversible specific capacity and the first coulombic efficiency are both at a high level, and the reversible specific capacity and the coulombic efficiency are still at a high level after circulation for multiple times. It should be noted that the reversible specific capacity of the lithium ion battery is the specific capacity of the battery. Therefore, the material can be used as the negative electrode material of the lithium ion battery to greatly improve the specific capacity and the cycle performance. In conclusion, the cathode material of the lithium ion battery is obtained by mixing and carbonizing the cystine polymer, the nitrogen source and the sulfur source, and is simple in process, low in cost and suitable for industrial production. In the preparation process, the doping ratio of nitrogen and sulfur can be controlled by controlling the ratio of the cystine polymer, the nitrogen source and the sulfur source and the carbonization temperature, so that the specific capacity and the cyclicity of the amorphous porous carbon anode material prepared are obviously improved.
Further, the oxidative polymerization of cysteine and an oxidizing agent to form a cystine polymer specifically comprises:
preparing cysteine solution and oxidant solution from the cysteine and the oxidant;
specifically, the mass fractions of the cysteine solution and the oxidizing agent solution are not limited. The oxidant is at least one of hydrogen peroxide, ammonium persulfate, nitric acid or ferric chloride.
Dropwise adding the oxidant solution into the cysteine solution to obtain a white precipitate;
in practical application, the cysteine solution and the oxidant solution are sufficiently oxidized and polymerized when the molar ratio is 2:1, and a white precipitated cystine polymer is obtained.
The precipitated cystine polymer was filtered and dried.
Specifically, the cystine polymer, the nitrogen source and the sulfur source are uniformly mixed, and the mixture is carbonized at the temperature of 240 ℃ and 630 ℃ for the following time: 1-4 hours, the flow rate of inert gas is: carbonizing treatment is carried out under the condition of 20-100mL/min to form the amorphous porous carbon lithium ion battery negative electrode material.
Wherein the molar ratio of the cystine to the nitrogen source to the sulfur source is 2: 1-2: 0.5-3. Preferably, the carbonization temperature is 240-500 ℃, the carbonization time is 2-3 hours, the flow rate of inert gas is 50-100mL/min, the molar ratio of cystine, nitrogen source and sulfur source is 2:1: 0.5-3, more preferably, the carbonization temperature is 300-400 ℃, the carbonization time is 2-2.5 hours, the flow rate of inert gas is 50-80mL/min, and the molar ratio of nitrogen source and sulfur source is 2: 1-3.
Specifically, the nitrogen source is one or more of thiourea, melamine, polyaniline or vinyl pyrrolidone. The sulfur source is one or more of thiourea, sulfur or sodium dodecyl benzene sulfonate. And putting cystine, a nitrogen source and a sulfur source into a tube furnace for carbonization treatment.
Example 1
Mixing a cystine polymer, a nitrogen source and a sulfur source according to a molar ratio of 2:1: 3, uniformly mixing, and carbonizing the mixture at the temperature of 400 ℃ for the following time: 2 hours, inert gas flow rate: and carbonizing at the speed of 80mL/min to obtain the amorphous porous carbon lithium ion battery negative electrode material.
The amorphous porous carbon material obtained in example 1 had nitrogen and sulfur doping levels of 13.95 wt% and 21.13 wt%, respectively. The resulting material is amorphous porous carbon in sheet form, as shown in fig. 2. The specific surface area reaches 304m2(ii) in terms of/g. The material is used as a lithium ion battery cathode material and is added at 100mA g-1Under the current density, the first reversible specific capacity reaches 1188mAhg-1The first coulombic efficiency is 76 percent, and the reversible specific capacity is increased to 861mAhg after 50 cycles-1. The material is 1Ag-1Under the condition of current density, 653mAhg can be obtained after 500 cycles-1The reversible specific capacity of (a). At a level of up to 5Ag-1Under the condition of current density of (3), 465mAhg can be obtained-1When the current density is reduced to 100mAg-1When the specific capacity is increased to 918mAhg again-1The level of (c). The material shows very good specific capacity and cycle performance.
Example 2
Adding cystine, a nitrogen source and a sulfur source into the mixture according to a molar ratio of 2:1: 2, uniformly mixing, and carbonizing the mixture at the temperature of 400 ℃ for the following time: 2 hours, inert gas flow rate: carbonizing treatment is carried out under the condition of 80mL/min to form the amorphous porous carbon lithium ion battery negative electrode material.
The amorphous porous carbon material obtained in example 2 had nitrogen-sulfur doping levels of 13.4 wt% and 14.3 wt%, respectively.
Example 3
Adding cystine, a nitrogen source and a sulfur source into the mixture according to a molar ratio of 2:1: 2, uniformly mixing, and carbonizing the mixture at the temperature of 500 ℃ for the following time: 2 hours, inert gas flow rate: and carbonizing at the speed of 80mL/min to obtain the amorphous porous carbon lithium ion battery negative electrode material.
The amorphous porous carbon material prepared in example 3 had nitrogen-sulfur doping levels of 10.18% and 7.57%, respectively.
Example 4
Adding cystine, a nitrogen source and a sulfur source into the mixture according to a molar ratio of 2:1: 2, uniformly mixing, and carbonizing the mixture at the temperature of 600 ℃ for the following time: 2 hours, inert gas flow rate: and carbonizing at the speed of 80mL/min to obtain the amorphous porous carbon lithium ion battery negative electrode material.
The nitrogen-sulfur doping levels of the amorphous porous carbon material prepared from example 4 were 6.88 wt% and 2.15 wt%, respectively. The resulting material was porous, flake-like amorphous carbon, as shown in fig. 3. The specific surface area reaches 93m2(ii) in terms of/g. Interlayer spacing d of carbon Material002Is 0.38 nm. At 100mAg-1Under the current density, the first reversible specific capacity reaches 970mAhg-1The first coulombic efficiency is 68 percent, and the reversible specific capacity is increased to 656mAhg after 50 cycles-1(ii) a At 1A g-1Under the condition of current density, 506mAhg can be obtained after 500 circles-1The reversible specific capacity of (a). At a level of up to 5Ag-1At a current density of 325mAhg, a current density of 325mAhg can be obtained-1When the current density is reduced to 100mA g-1When the specific capacity rises to 750mAhg again-1The level of (c).
As can be seen from the first and second examples, the lower the mass ratio of the nitrogen source to the sulfur source, the lower the nitrogen-sulfur doping in the prepared material, and as can be seen from the second, third, and fourth examples, the lower the carbonization temperature, the higher the nitrogen-sulfur doping in the prepared material, for the same nitrogen source to sulfur source ratio. Meanwhile, the amorphous porous anode material prepared by the preparation method provided by the technical scheme of the invention still has good specific capacity and cycle characteristics even when the nitrogen and sulfur doping levels are respectively 6.88 wt% and 2.15 wt%.
The above embodiments are illustrative of the present invention, and not restrictive, and any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A preparation method of a lithium ion battery negative electrode material is characterized by comprising the following steps:
polymerizing cysteine in the presence of an oxidant to obtain a cystine polymer;
mixing the cystine polymer, a nitrogen source and a sulfur source to obtain a mixture;
carbonizing the mixture at the temperature of 240-630 ℃ in an inert atmosphere to obtain the lithium ion battery negative electrode material;
wherein the molar ratio of the cystine polymer to the nitrogen source to the sulfur source is 2: 1-2: 0.5-3;
the nitrogen source is at least one of thiourea, melamine, polyaniline and vinyl pyrrolidone;
the sulfur source is at least one of thiourea, sulfur and sodium dodecyl benzene sulfonate.
2. The method according to claim 1, characterized in that the preparation method of the cystine polymer comprises the following steps:
preparing cysteine solution and oxidant solution from the cysteine and the oxidant respectively;
dropwise adding the oxidant solution into the cysteine solution to obtain a white precipitate;
filtering and drying the white precipitated cystine polymer.
3. The method as claimed in claim 1, wherein the carbonization temperature is 240-500 ℃.
4. The method according to claim 1, wherein the carbonization time for carbonizing the mixture is: 1-4 hours, the flow rate of inert gas is: 20-100 mL/min.
5. The method according to claim 1, characterized in that the molar ratio of the cystine polymer, the nitrogen source and the sulfur source is 2:1: 2.
6. a lithium ion battery comprising a negative electrode material prepared by the method of any one of claims 1 to 5.
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