CN111082028A - High-capacity negative electrode material, preparation method and lithium ion battery - Google Patents
High-capacity negative electrode material, preparation method and lithium ion battery Download PDFInfo
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Abstract
A high capacity negative electrode includes a negative current collecting foil and a negative electrode material; the negative electrode material comprises a negative electrode active material, a conductive agent and a binder; the negative active material comprises an active carbon material, and nano spherical phosphorus particles are embedded in the active carbon material; the conductive agent, the binder and the negative active material are uniformly mixed and then coated on the negative current collector. In the invention, the conductivity of the phosphorus material is effectively improved by compounding the activated carbon and the red phosphorus, the nano spherical phosphorus particles are uniformly dispersed on the activated carbon, the contact area of the electrolyte is increased, more importantly, the P-C bond can stabilize the structure of the material, the volume expansion of the phosphorus material in the charge-discharge cycle process is effectively relieved, and the cycle performance of the battery is ensured.
Description
Technical Field
The invention relates to a lithium ion battery, in particular to a high-capacity negative electrode material, a preparation method and a lithium ion battery.
Background
In the world, with the increasing environmental pollution and global warming caused by the burning of fossil fuels, countries are changing the economic model based on fossil fuels to the economic model based on new energy, and the development of renewable energy and clean energy is a major strategic task for the economic and social development of China. The high-speed development of the society demands high-safety and low-cost energy storage technology urgently. Lithium ion batteries are considered one of the most promising energy storage technologies to meet these demands, and have been successfully used in portable electronic devices, plug-in hybrid vehicles, and pure electric vehicles, effectively reducing the amount of carbon dioxide emissions generated during urban transportation.
The lithium ion battery is a device for converting chemical energy into electric energy through chemical reaction, is one of important ways for storing and converting energy, is widely applied in almost all fields, and is an important product for relieving the current energy crisis and reducing environmental pollution. Among secondary batteries, lithium ion batteries are rapidly becoming the first choice for rechargeable power sources of portable electronic products today due to their advantages of high operating voltage, long cycle life, large capacity, small volume, small self-discharge, no memory effect, little environmental pollution, etc. For lithium ion batteries, the negative electrode material has a decisive role in the capacity of the battery and is closely related to the cost and the safety performance of the battery, and the negative electrode material becomes a key factor for restricting the further improvement of the overall performance of the lithium ion battery. Therefore, the development of a novel lithium ion battery cathode material is very important.
The red phosphorus in the cathode active material of the lithium ion battery is a cathode material with higher capacity, has proper potential for lithium, has large storage capacity and lower cost compared with the conventional cathode material, but the red phosphorus has poor conductivity and expands in volume during charge and discharge, thereby causing poor cycle performance. CN107749467A discloses a carbon-coated iron phosphide electrode material with a fusiform structure and a preparation method thereof, wherein carbon-coated iron phosphide particles in the electrode material are gathered together in the fusiform structure, the particle size of the carbon-coated iron phosphide particles is 10-80 nm, the mass fraction of iron phosphide is 50-90%, and the carbon-coated iron phosphide electrode material with the fusiform structure is prepared by polymerization and heat treatment. However, when the composite material is assembled into a battery for electrochemical test, the initial reversible discharge capacity is 680 mAh g < -1 > under the test current of 100 mA g < -1 > and the voltage range of 0.02-3V, the capacity tends to be stable after 15 times of circulation, and the capacity is attenuated to 600 mAh g < -1 > after 100 times of circulation, which indicates that the reversible capacity of the material is low.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a phosphorus-based negative electrode material which has high specific capacity and meets the requirement on cycle performance, a preparation method and a lithium ion battery.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a high capacity negative electrode includes a negative current collecting foil and a negative electrode material; the negative electrode material comprises a negative electrode active material, a conductive agent and a binder; the negative active material comprises an activated carbon material, and nano spherical phosphorus particles are embedded in the activated carbon material; and the conductive agent, the binder and the negative active material are uniformly mixed and then coated on the negative current collector.
In the above-described negative electrode having a high capacity, the activated carbon is preferably doped with nitrogen atoms.
In the above negative electrode with high capacity, preferably, the conductive agent includes one or more of carbon black, acetylene black, conductive graphite, and carbon nanotubes.
In the above-described negative electrode with a high capacity, the binder preferably includes one or more of polyvinyl alcohol, polytetrafluoroethylene, polyvinylidene fluoride, and polyurethane.
A method for preparing a high-capacity negative electrode includes the steps of,
1) grinding activated carbon, sieving with a 200-mesh sieve, fully cleaning powder smaller than 200 meshes with deionized water and absolute ethyl alcohol, and drying;
2) ball-milling the activated carbon powder and red phosphorus in the step 1) for at least 3 hours, sintering in the atmosphere of rare gas at the sintering temperature of more than 500 ℃, and preserving heat for more than 6 hours; obtaining a carbon-phosphorus composite material, wherein nano spherical phosphorus particles are embedded on an active carbon material;
3) and (3) uniformly mixing the conductive agent, the binder and the carbon-phosphorus composite material obtained in the step 2), and coating the mixture on a negative current collector to obtain a negative electrode with high capacity.
In the preparation method of the high-capacity anode material, preferably, the activated carbon in the step 1) is doped with nitrogen, and the mixed powder in the step 1) is uniformly mixed with melamine, wherein the weight ratio of the melamine to the mixed powder in the step 1) is 1:5-1: 15; sintering under the protection of nitrogen or rare gas, wherein the sintering temperature is over 400 ℃, and keeping the temperature for 1 hour; obtaining the nitrogen-doped activated carbon material.
Preferably, in the step 2), the silicon material is added, and the silicon material, red phosphorus and the activated carbon powder in the step 1) are mixed together, ball-milled and then sintered; the weight of the silicon material accounts for 1-5% of the weight of the mixed material.
In the above method for preparing a negative electrode material with high capacity, preferably, the silicon material includes one or more of lithium monosilicate, lithium disilicate and lithium pentasilicate.
A lithium ion battery comprises the negative electrode with high capacity.
Compared with the prior art, the invention has the advantages that: in the invention, the conductivity of the phosphorus material is effectively improved by compounding the activated carbon and the red phosphorus, the nano spherical phosphorus particles are uniformly dispersed on the activated carbon, the contact area of the electrolyte is increased, more importantly, the P-C bond can stabilize the structure of the material, the volume expansion of the phosphorus material in the charge-discharge cycle process is effectively relieved, and the cycle performance of the battery is ensured.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
It should be particularly noted that when an element is referred to as being "fixed to, connected to or communicated with" another element, it can be directly fixed to, connected to or communicated with the other element or indirectly fixed to, connected to or communicated with the other element through other intermediate connecting components.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
A high capacity negative electrode includes a negative current collecting foil and a negative electrode material; the negative electrode material comprises a negative electrode active material, a conductive agent and a binder; the negative active material comprises an activated carbon material, and nano spherical phosphorus particles are embedded in the activated carbon material; and the conductive agent, the binder and the negative active material are uniformly mixed and then coated on the negative current collector. In the invention, the electronic conductivity of the phosphorus material is effectively improved by compounding carbon and phosphorus, the nano spherical phosphorus particles are uniformly dispersed on the nitrogen-doped activated carbon, the contact area with the electrolyte is increased, and the synergistic effects are beneficial to the exertion of the capacity of the carbon-phosphorus composite material and the maintenance of the cycling stability of the battery. Meanwhile, the P-C bond existing after carbon and phosphorus are compounded can stabilize the structure of the material, and effectively relieve the volume expansion of the material in the charging and discharging processes.
In the present invention, the activated carbon is doped with nitrogen atoms. The active carbon doped with nitrogen atoms can provide more active micro-points, so that stable P-C bonds are formed in the material.
In the present invention, the conductive agent includes one or more of carbon black, acetylene black, conductive graphite, and carbon nanotubes.
In the present invention, the binder includes one or more of polyvinyl alcohol, polytetrafluoroethylene, polyvinylidene fluoride, and polyurethane.
A method for preparing a high-capacity negative electrode includes the steps of,
1) grinding activated carbon, sieving with a 200-mesh sieve, fully cleaning powder smaller than 200 meshes with deionized water and absolute ethyl alcohol, and drying;
2) ball-milling the activated carbon powder and red phosphorus in the step 1) for at least 3 hours, sintering in the atmosphere of rare gas at the sintering temperature of more than 500 ℃, and preserving heat for more than 6 hours; obtaining a carbon-phosphorus composite material, wherein nano spherical phosphorus particles are embedded on an active carbon material;
3) and (3) uniformly mixing the conductive agent, the binder and the carbon-phosphorus composite material obtained in the step 2), and coating the mixture on a negative current collector to obtain a negative electrode with high capacity.
In the invention, the activated carbon in the step 1) is doped with nitrogen, the mixed powder in the step 1) and melamine are uniformly mixed, and the weight ratio of the melamine to the mixed powder in the step 1) is 1:5-1: 15; sintering under the protection of nitrogen or rare gas, wherein the sintering temperature is over 400 ℃, and keeping the temperature for 1 hour; obtaining the nitrogen-doped activated carbon material.
In the invention, silicon material is added in the step 2), the silicon material, red phosphorus and the activated carbon powder in the step 1) are mixed together and ball-milled, and then sintered; the weight of the silicon material accounts for 1-5% of the weight of the mixed material.
In the present invention, the silicon material includes one or more of lithium monosilicate, lithium disilicate, and lithium pentasilicate. In the invention, the addition of the silicon material can further improve the capacity of the battery, and the addition of the silicon material in the form of lithium salt can reduce the irreversible capacity generated during charging.
The invention also provides a lithium ion battery which comprises the negative electrode with high capacity.
Example 1
A high capacity negative electrode includes a negative current collecting foil and a negative electrode material; the negative electrode material comprises a negative electrode active material, a conductive agent and a binder; the negative active material comprises an activated carbon material, and nano spherical phosphorus particles are embedded in the activated carbon material; and the conductive agent, the binder and the negative active material are uniformly mixed and then coated on the negative current collector. In this embodiment, the activated carbon is doped with nitrogen atoms.
In this embodiment, the conductive agent is acetylene black; the binder is polyvinylidene fluoride.
The method for producing a high-capacity negative electrode according to this example includes the steps of,
1) grinding activated carbon, sieving with a 200-mesh sieve, fully cleaning powder smaller than 200 meshes with deionized water and absolute ethyl alcohol, and drying; carrying out nitrogen doping on the activated carbon obtained in the step 1), and uniformly mixing the mixed powder obtained in the step 1) with melamine, wherein the weight ratio of the melamine to the mixed powder obtained in the step 1) is 1:5-1: 15; sintering under the protection of nitrogen or rare gas, wherein the sintering temperature is over 400 ℃, and keeping the temperature for 1 hour; obtaining the nitrogen-doped activated carbon material.
2) Ball-milling the activated carbon powder and red phosphorus in the step 1) for at least 3 hours, sintering in the atmosphere of rare gas at the sintering temperature of more than 500 ℃, and preserving heat for more than 6 hours; obtaining a carbon-phosphorus composite material, wherein nano spherical phosphorus particles are embedded on an active carbon material; FIG. 1 is an SEM image of activated carbon material with nano-spherical phosphorus particles embedded therein.
3) And (3) uniformly mixing the conductive agent, the binder and the carbon-phosphorus composite material obtained in the step 2), and coating the mixture on a negative current collector to obtain a negative electrode with high capacity.
The embodiment also provides a lithium ion battery which adopts the above negative electrode. Fig. 2 shows the results of the rate capability test of the lithium ion battery. As can be seen from fig. 2, the cycling performance of the battery was satisfactory.
In other embodiments, a silicon material may also be added in step 2), the silicon material, red phosphorus and the activated carbon powder in step 1) are mixed together and ball-milled, and then sintered; the weight of the silicon material accounts for 1-5% of the weight of the mixed material. The silicon material includes one or more of lithium monosilicate, lithium disilicate, and lithium pentasilicate.
Claims (9)
1. A high-capacity negative electrode characterized in that: the negative current collecting foil and the negative material are included; the negative electrode material comprises a negative electrode active material, a conductive agent and a binder; the negative active material comprises an activated carbon material, and nano spherical phosphorus particles are embedded in the activated carbon material; and the conductive agent, the binder and the negative active material are uniformly mixed and then coated on the negative current collector.
2. The high capacity negative electrode of claim 1, wherein: the activated carbon is doped with nitrogen atoms.
3. The high capacity negative electrode of claim 1, wherein: the conductive agent includes one or more of carbon black, acetylene black, conductive graphite, and carbon nanotubes.
4. The high capacity negative electrode of claim 1, wherein: the binder comprises one or more of polyvinyl alcohol, polytetrafluoroethylene, polyvinylidene fluoride and polyurethane.
5. The method for producing a high-capacity negative electrode according to any one of claims 1 to 4, characterized in that: comprises the following steps of (a) carrying out,
1) grinding activated carbon, sieving with a 200-mesh sieve, fully cleaning powder smaller than 200 meshes with deionized water and absolute ethyl alcohol, and drying;
2) ball-milling the activated carbon powder and red phosphorus in the step 1) for at least 3 hours, sintering in the atmosphere of rare gas at the sintering temperature of more than 500 ℃, and preserving heat for more than 6 hours; obtaining a carbon-phosphorus composite material, wherein nano spherical phosphorus particles are embedded on an active carbon material;
3) and (3) uniformly mixing the conductive agent, the binder and the carbon-phosphorus composite material obtained in the step 2), and coating the mixture on a negative current collector to obtain a negative electrode with high capacity.
6. The method for producing a high-capacity anode material according to claim 5, characterized in that: carrying out nitrogen doping on the activated carbon obtained in the step 1), and uniformly mixing the mixed powder obtained in the step 1) with melamine, wherein the weight ratio of the melamine to the mixed powder obtained in the step 1) is 1:5-1: 15; sintering under the protection of nitrogen or rare gas, wherein the sintering temperature is over 400 ℃, and keeping the temperature for 1 hour; obtaining the nitrogen-doped activated carbon material.
7. The method for producing a high-capacity anode material according to claim 5, characterized in that: adding a silicon material in the step 2), mixing the silicon material, red phosphorus and the activated carbon powder in the step 1), ball-milling, and sintering; the weight of the silicon material accounts for 1-5% of the weight of the mixed material.
8. The method for producing a high-capacity anode material according to claim 7, characterized in that: the silicon material includes one or more of lithium monosilicate, lithium disilicate, and lithium pentasilicate.
9. A lithium ion battery, characterized by: a negative electrode comprising the high capacity negative electrode according to any one of claims 1 to 4.
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| CN114784251A (en) * | 2022-05-13 | 2022-07-22 | 中国科学技术大学 | Phosphorus-coated negative electrode material and preparation method and application thereof |
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Application publication date: 20200428 |