CN113690424B - Carbon-tin-silicon negative electrode material of lithium ion battery and preparation method thereof - Google Patents
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Abstract
The invention provides a carbon-tin-silicon negative electrode material of a lithium ion battery and a preparation method thereof. The application of the carbon-tin-silicon negative electrode material of the lithium ion battery in improving the specific capacity and the cycle performance of the lithium ion battery is shown in experimental results, wherein the application comprises the following steps: the specific capacity of the cathode material prepared by the invention is up to 910mAh g‑1After 40 weeks of cycling, there was no significant decay in capacity.
Description
Technical Field
The invention belongs to the field of lithium ion battery materials, and particularly relates to a carbon tin silicon negative electrode material of a lithium ion battery and a preparation method thereof.
Background
In recent years, due to the rapid development of various portable electronic devices and new energy vehicles, there is an urgent need to improve the energy density of battery materials. Lithium ion batteries have become the main force of the mobile battery market, and carbon-containing cathode materials are the main force in the field of cathode materials of lithium ion batteriesForce. However, the theoretical capacity of the commercial carbon-containing lithium ion battery is only 372 mAh g-1It is a little bit deficient for the fast-developing mobile power supply nowadays. With the expansion of research fields of scholars, silicon-based and tin-based lithium ion battery cathode materials become hot spots and key points of lithium ion battery research. Tin and its oxide as negative pole material of lithium battery have higher volumetric specific energy and mass specific energy, and Sn theoretical specific capacity can reach 996 mAh g-1. The theoretical specific capacity of Si is up to 4200 mAh g-1The silicon-based and tin-based lithium ion battery cathode material has the advantage of low de-intercalation lithium potential, but the volume change rate of the silicon-based and tin-based lithium ion battery cathode material is as high as 300% during charging, so that the cathode material is easy to pulverize during charging and discharging of the battery, irreversible damage is caused to an electrode structure, and the performance of the battery is greatly reduced.
Disclosure of Invention
In view of the above, the present invention provides a carbon-tin-silicon negative electrode material for a lithium ion battery and a preparation method thereof, aiming to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the carbon tin silicon negative electrode material of the lithium ion battery is a double-shell structure composite negative electrode material Si @ Sn @ C which takes Si particles as a support body, tin as an interlayer and resin cracking carbon and graphite as coating layers.
A preparation method of a carbon tin silicon negative electrode material of a lithium ion battery comprises the following steps:
s1: mixing nano Si, SnC2O4After being uniformly mixed, the mixture is thermally treated to form a Si/SnO compound;
s2: adding high molecular resin into an alcohol solvent to obtain a resin-alcohol solution;
s3: adding the Si/SnO compound and graphite into a resin-alcohol solution, uniformly mixing and drying to obtain an intermediate compound taking the resin and the graphite as covering layers;
s4: and grinding the intermediate compound, transferring the intermediate compound into heating equipment, sintering the intermediate compound at a high temperature under protective gas, and finally grinding the obtained product to obtain a final product.
Preferably, the mass ratio of Si to Sn in the Si/SnO composite prepared in step S1 is 1: (0.25-4).
Preferably, the heat treatment method in the step S1 is a melting method, the heating temperature is 300-380 ℃, and the heating time is 1-4 h.
Preferably, the polymer resin in step S2 is one or more of phenolic resin, polyvinyl butyral resin, and polytrimethylene glutarate.
Preferably, the alcohol solvent in step S2 is one or more of methanol, ethanol, ethylene glycol, propanol, isopropanol, and butanol.
Preferably, the mass ratio of the polymer resin to the alcohol solvent in the step S2 is (0.01-1): 1.
preferably, the adding amount of the Si/SnO composite in the step S3 is 20-40% (w/w), the adding amount of the resin is 20-40% (w/w), and the adding amount of the graphite is 30-60% (w/w).
Preferably, the graphite in the step S3 is artificial graphite or natural graphite.
Preferably, in the step S4, the protective gas is argon or nitrogen, the heating rate is set to be 0.1-5 ℃/min, and sintering is carried out at the temperature of 600-900 ℃ for 0.5-4 h.
The nano silicon and the carbon are effectively compounded to buffer the volume change of silicon particles in the charging and discharging process, improve the conductivity of Si and avoid the agglomeration phenomenon of the silicon in the charging and discharging process. Tin is added into the cathode material in a proper amount to fill gaps among silicon and carbon, so that the conductivity and tap density of the material are enhanced, and the electrochemical performance of the cathode material is improved. The hard carbon formed by the cracking of the resin can buffer the volume expansion of the tin and silicon mixture to a certain extent. The graphite has the excellent characteristics of good softness, stable electrochemical performance and the like, and can be combined with hard carbon to well improve the physical performance and the cycling stability of the electrode material, so that the expansion and the agglomeration of tin and silicon are inhibited, and the specific capacity and the cycling stability of the battery are improved.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, a high-temperature melting method is adopted for the cathode material, the heating time and the carbon source ratio are controlled, SnO is coated on the surface of Si particles, a layer of resin and graphite is coated on the surface of the Si particles, the Si particles are used as a support body, tin is used as an interlayer, phenolic resin cracking carbon and artificial graphite are used as a novel double-shell structure composite cathode material Si @ Sn @ C of the coating layer after high-temperature carbonization, and the novel high-capacity cathode material is found after a battery is assembled. According to the invention, the resin cracking carbon and the graphite carbon material have good compatibility with the electrolyte, the volume expansion of the active material can be effectively relieved, the diffusion rate of lithium ions and electrons is promoted, tin is uniformly coated on the surface of Si particles, and a tin shell layer is formed after sintering, so that the electrochemical performance of the silicon-carbon composite material is greatly improved.
(2) The application of the carbon-tin-silicon negative electrode material of the lithium ion battery synthesized by the invention in improving the specific capacity and the cycle performance of the lithium ion battery is shown in experimental results, wherein the application comprises the following steps: the specific capacity of the cathode material prepared by the invention is up to 910mAh g-1After 40 weeks of cycling, there was no significant decay in capacity.
Drawings
Fig. 1 is an SEM photograph of a negative electrode material prepared in example 1 of the present invention;
fig. 2 is an SEM photograph of the anode material prepared in example 2 of the present invention;
fig. 3 is an SEM photograph of the anode material prepared in example 3 of the present invention;
fig. 4 is an SEM photograph of the anode material obtained in example 7 of the present invention;
fig. 5 is an SEM photograph of the anode material obtained in example 8 of the present invention;
fig. 6 is an SEM photograph of the anode material prepared in comparative example 1 of the present invention;
FIG. 7 is a graph of electrochemical performance of a negative electrode material obtained in example 1 of the present invention;
FIG. 8 is a graph of the electrochemical performance of the negative electrode material obtained in example 2 of the present invention;
FIG. 9 is a graph of the electrochemical performance of the negative electrode material obtained in example 3 of the present invention;
FIG. 10 is a graph of the electrochemical performance of the negative electrode material obtained in example 4 of the present invention;
FIG. 11 is a graph of the electrochemical performance of the negative electrode material obtained in example 5 of the present invention;
FIG. 12 is a graph of the electrochemical performance of the negative electrode material obtained in example 6 of the present invention;
FIG. 13 is a graph of the electrochemical performance of the negative electrode material obtained in example 7 of the present invention;
FIG. 14 is a graph of the electrochemical performance of the negative electrode material obtained in example 8 of the present invention;
FIG. 15 is a graph of the electrochemical performance of the negative electrode material obtained in example 9 of the present invention;
fig. 16 is a graph showing electrochemical properties of the anode material prepared in comparative example 1 of the present invention.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The invention will be described in detail with reference to the following examples.
Example 1
The preparation method of the carbon-tin-silicon negative electrode material of the lithium ion battery in the embodiment comprises the following steps:
s1: mixing nano Si, SnC2O4After mixing, carrying out heat treatment for 3h at the temperature of 350 ℃ to obtain a Si/SnO composite, and controlling the mass ratio of Si to Sn in the Si/SnO composite to be 1.5: 1;
s2: adding phenolic resin into an ethanol solvent, and placing the phenolic resin into an ultrasonic instrument for ultrasonic dissolution at 30 ℃ to obtain a phenolic resin-ethanol solution;
s3: adding the Si/SnO compound and the artificial graphite into a phenolic resin-ethanol solution, uniformly mixing and drying to obtain an intermediate compound taking resin and artificial graphite as covering layers (the mass ratio of the Si/SnO compound to the phenolic resin to the artificial graphite is 3: 3: 4);
s4: grinding the intermediate compound, transferring the intermediate compound into an atmosphere tube furnace, sintering at high temperature under the protection of nitrogen, setting the heating rate at 5 ℃/min, and sintering at 750 ℃ for 1 h. And finally, grinding the obtained product to obtain a final product.
The SEM image of the final product is shown in fig. 1, and it can be seen from fig. 1 that: SnC2O4After melting and decomposing into SnO coated silicon particles, a double-shell structure composite negative electrode material Si @ Sn @ C is formed in the process of coating phenolic resin cracking carbon and graphite, and the phenolic resin is basically carbonized at the temperature and has good crystallinity. The coating of Sn to Si is complete under the proportion, and the assembled battery has high electrode capacity and good cycling stability. The electrochemical performance chart of example 1 is shown in FIG. 7, and it can be seen that the specific capacity of the composite material is 910mAh g-1And the electrochemical performance is excellent.
Example 2
The procedure of the method for producing a negative electrode material in this example was the same as in example 1, except that the temperature of the atmosphere tube furnace in step S4 was increased to 600 ℃.
The SEM image of the final product is shown in FIG. 2, the electrochemical performance image of example 2 is shown in FIG. 8, and it can be seen that the specific capacity of the composite material is 560 mAh g-1And the electrochemical performance is excellent.
Example 3
The preparation method of the negative electrode material in this example is the same as example 1 except that the temperature of the atmosphere tube furnace in step (4) is increased to 900 ℃.
The SEM image of the final product is shown in FIG. 3, the electrochemical performance image of example 3 is shown in FIG. 9, and it can be seen that the specific capacity of the composite material is 820 mAh g-1And the electrochemical performance is excellent.
Example 4
The preparation method of the negative electrode material in the embodiment is the same as that in embodiment 1, except that the mass ratio of the Si/SnO composite, the phenolic resin and the graphite in step (3) is 2: 4: 4.
the electrochemical performance diagram of the negative electrode material obtained in example 4 is shown in fig. 10, and it can be seen that the specific capacity of the negative electrode material is 520 mAh g-1And the electrochemical performance is excellent.
Example 5
The preparation method of the negative electrode material in the embodiment is the same as that in embodiment 1, except that the mass ratio of the Si/SnO composite, the phenolic resin and the graphite in step (3) is 2: 2: 6.
the electrochemical performance chart of the negative electrode material obtained in example 5 is shown in fig. 11, and it can be seen that the specific capacity of the negative electrode material is 470 mAh g-1And the electrochemical performance is excellent.
Example 6
The preparation method of the negative electrode material in the embodiment is the same as that in embodiment 1, except that the mass ratio of the Si/SnO composite, the phenolic resin and the graphite in step (3) is 4: 3: 3.
the electrochemical performance diagram of the negative electrode material obtained in example 6 is shown in fig. 12, and it can be seen that the specific capacity of the negative electrode material is about 790mAh/g, and the negative electrode material has excellent electrochemical performance.
Example 7
The preparation method of the negative electrode material in this example is the same as that in example 1, except that the mass ratio of Si to Sn in the Si/SnO composite is controlled to 1:1.5 in step S1.
An SEM image of the negative electrode material obtained in example 7 is shown in fig. 4, and an electrochemical performance image is shown in fig. 13, and the negative electrode material has a specific capacity of about 800mAh/g and excellent electrochemical performance.
Example 8
The preparation method of the negative electrode material in this example is the same as that in example 1, except that the mass ratio of Si to Sn in the Si/SnO composite is controlled to 4: 1 in step S1.
An SEM image of the negative electrode material obtained in example 8 is shown in fig. 5, and an electrochemical performance image is shown in fig. 14, and the negative electrode material has a specific capacity of about 870mAh/g and excellent electrochemical performance.
Example 9
The preparation method of the negative electrode material in this example is the same as that in example 1, except that the mass ratio of Si to Sn in the Si/SnO composite is controlled to 1: 4 in step S1.
As shown in fig. 15, the electrochemical performance of the negative electrode material obtained in example 9 has a specific capacity of about 440mAh/g, and thus has excellent electrochemical performance.
Comparative example
The procedure of the method for producing the negative electrode material in this comparative example was the same as in example 1, except that the temperature of the atmosphere tube furnace in step (4) was raised to 400 ℃.
The SEM image of the negative electrode material obtained in the comparative example is shown in fig. 6, and the carbonization rate of the phenol resin is low at this temperature, and the crystallinity is extremely poor. The electrochemical performance chart is shown in FIG. 16, and the specific capacity is 300 mAh/g.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the invention, so that any modifications, equivalents, improvements and the like, which are within the spirit and principle of the present invention, should be included in the scope of the present invention.
Claims (8)
1. A preparation method of a carbon tin silicon negative electrode material of a lithium ion battery is characterized by comprising the following steps: the method comprises the following steps:
s1: mixing nano Si, SnC2O4After being uniformly mixed, the mixture is thermally treated to form a Si/SnO compound;
s2: adding high molecular resin into an alcohol solvent to obtain a resin-alcohol solution;
s3: adding the Si/SnO compound and graphite into a resin-alcohol solution, uniformly mixing and drying to obtain an intermediate compound taking the resin and the graphite as covering layers;
s4: grinding the intermediate compound, transferring the intermediate compound into heating equipment, sintering the intermediate compound at a high temperature under protective gas, and finally grinding the obtained product to obtain a final product;
wherein the heat treatment method in the step S1 is a melting method, the heating temperature is 300-380 ℃, and the heating time is 1-4 h;
the final product is a double-shell structure composite negative electrode material Si @ Sn @ C with Si particles as a support body, tin as an interlayer and resin cracking carbon and graphite as coating layers.
2. The preparation method of the carbon-tin-silicon negative electrode material of the lithium ion battery according to claim 1, characterized by comprising the following steps: the mass ratio of Si to Sn in the Si/SnO composite prepared in the step S1 is 1: (0.25-4).
3. The preparation method of the carbon-tin-silicon negative electrode material of the lithium ion battery according to claim 1, characterized by comprising the following steps: the polymer resin in the step S2 is one or more of phenolic resin, polyvinyl butyral resin, and poly (propylene glutarate) glycol ester.
4. The preparation method of the carbon-tin-silicon negative electrode material of the lithium ion battery according to claim 1, characterized by comprising the following steps: the alcohol solvent in the step S2 is one or more of methanol, ethanol, ethylene glycol, propanol, isopropanol and butanol.
5. The preparation method of the carbon-tin-silicon negative electrode material of the lithium ion battery according to claim 1, characterized by comprising the following steps: the mass ratio of the high molecular resin to the alcohol solvent in the step S2 is (0.01-1): 1.
6. the preparation method of the carbon-tin-silicon negative electrode material of the lithium ion battery according to claim 1, characterized by comprising the following steps: in the step S3, the adding amount of the Si/SnO compound is 20-40% (w/w), the adding amount of the resin is 20-40% (w/w), and the adding amount of the graphite is 30-60% (w/w).
7. The preparation method of the carbon-tin-silicon negative electrode material of the lithium ion battery according to claim 1, characterized by comprising the following steps: the graphite in the step S3 is artificial graphite or natural graphite.
8. The preparation method of the carbon-tin-silicon negative electrode material of the lithium ion battery according to claim 1, characterized by comprising the following steps: in the step S4, the protective gas is argon or nitrogen, the heating rate is set to be 0.1-5 ℃/min, and sintering is carried out at the temperature of 600-900 ℃ for 0.5-4 h.
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