CN106941157B - Carbon-silicon composite material for lithium ion battery cathode and preparation method thereof - Google Patents
Carbon-silicon composite material for lithium ion battery cathode and preparation method thereof Download PDFInfo
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- CN106941157B CN106941157B CN201710165176.6A CN201710165176A CN106941157B CN 106941157 B CN106941157 B CN 106941157B CN 201710165176 A CN201710165176 A CN 201710165176A CN 106941157 B CN106941157 B CN 106941157B
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 25
- 239000002153 silicon-carbon composite material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 13
- 239000010703 silicon Substances 0.000 claims abstract description 13
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 11
- 229920001940 conductive polymer Polymers 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- 239000011812 mixed powder Substances 0.000 claims abstract description 7
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 5
- 239000011790 ferrous sulphate Substances 0.000 claims description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 5
- 229920000123 polythiophene Polymers 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 229960002089 ferrous chloride Drugs 0.000 claims description 4
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 4
- 229920000128 polypyrrole Polymers 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000011856 silicon-based particle Substances 0.000 abstract description 18
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 230000002401 inhibitory effect Effects 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 239000003575 carbonaceous material Substances 0.000 description 10
- 239000007773 negative electrode material Substances 0.000 description 10
- 239000007789 gas Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to a carbon-silicon composite material for a lithium ion battery cathode and a preparation method thereof, wherein the method comprises the following steps: the method comprises the following steps: mixing nano silicon, conductive polymer, conductive carbon and iron-containing compound according to the weight ratio of 30-40: 20: 20: 1, mixing; step two: adding the mixed powder prepared in the first step into an agate mortar for grinding for 40-60 min; step three: putting the powder ground in the step two into a tubular furnace, introducing inert gas for heating, and preserving heat for 2 hours at 600 ℃; step four: and cooling and grinding the powder prepared in the step three to obtain the carbon-silicon composite material for the lithium ion battery cathode. The battery prepared by the method has high specific capacity, and meanwhile, the pole piece material not only has an inhibiting effect on silicon expansion, but also can simultaneously generate a recycling effect on crushed silicon particles.
Description
Technical Field
The invention belongs to the field of lithium ion battery materials, and particularly relates to a carbon-silicon composite material for a lithium ion battery cathode and a preparation method thereof.
Background
The application of the lithium ion battery in various mobile devices brings great convenience to social life. However, as the demand for battery life of various devices has increased, the battery capacity has begun to be too great today. Many devices, such as mobile phones, electric vehicles, etc., are waiting for an increase in battery capacity for upgrading. Starting from the negative electrode material of lithium ion batteries, one has seen the desire for an increase in battery capacity, silicon having a theoretical capacity of 4200mAh/g compared to the capacity of 370mAh/g of graphite, which is the negative electrode material of conventional batteries. Therefore, when the silicon is used as the cathode of the lithium ion battery, the battery capacity can be greatly improved theoretically. However, the use of silicon materials has a significant drawback that during the adsorption and desorption cycle of lithium ions, a volume change of about 3 times is generated, and the volume change can cause the damage of the surface structure of the pole piece, thereby damaging the cycle performance of the battery. In order to apply the silicon material to the negative electrode of the battery, researchers have improved the cycle performance of the battery by reducing the diameter of silicon particles, using a silicon-containing alloy material, blending with a carbon material, and the like. These measures can bring certain promotion to the battery performance to a certain extent. However, the method is to inhibit the silicon particles from being broken, the content of silicon is lower and generally does not exceed 10%, so the specific capacity of the battery is improved to a limited extent. Once the usage amount of the silicon simple substance is increased, the battery can obtain higher specific capacity at the initial stage of use, but after a plurality of cycles, the capacity is greatly reduced, even the silicon particles are completely failed, so that the effect of increasing the capacity is lost.
Disclosure of Invention
The invention aims to provide a carbon-silicon composite material for a lithium ion battery cathode and a preparation method thereof, and solves the problem of low specific capacity of a conventional cathode material in the prior art.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of a carbon-silicon composite material for a lithium ion battery cathode comprises the following steps:
the method comprises the following steps: mixing nano silicon, conductive polymer, conductive carbon and iron-containing compound according to the weight ratio of 30-40: 20: 20: 1, mixing;
step two: adding the mixed powder prepared in the first step into an agate mortar for grinding for 40-60 min;
step three: putting the powder ground in the step two into a tubular furnace, introducing inert gas for heating, and preserving heat for 2 hours at 600 ℃;
step four: and cooling and grinding the powder prepared in the step three to obtain the carbon-silicon composite material for the lithium ion battery cathode.
The nano silicon is silicon simple substance particles with the particle size of less than 100 nm.
The conductive polymer is one of polypyrrole or polythiophene.
The iron-containing compound is one of ferrous chloride or ferrous sulfate.
The inert gas is one of nitrogen or argon.
The carbon-silicon composite material for the lithium ion battery cathode prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
1. the battery prepared by the method for preparing the spongy structure by the linear carbon material for the lithium ion battery cathode and wrapping the silicon particles has high specific capacity: the theoretical specific capacity of the traditional conventional carbon material negative electrode is 370mAh/g, the theoretical specific capacity is about 300mAh/g in actual use, and the specific capacity of 600-800mAh/g can be generated by part of the negative electrode material doped with silicon simple substance in the battery; the battery cathode prepared by using the carbon-silicon composite material for the lithium ion battery cathode can generate the specific capacity of more than 1500 mAh/g, and can still retain the specific capacity of more than 800mAh/g even after being cycled for 100 times;
2. when the material is applied to a battery pole piece, silicon particles are distributed in a spongy space generated by the linear carbon material, and the high strength of the linear material can effectively slow down the expansion and crushing process of the silicon particles. Meanwhile, when the silicon particles are crushed, the silicon particles can be separated from the original bonding points, but the surrounding spongy space is not damaged, and the silicon fragments which are positioned in the gaps of the spongy space and have no effect can be continuously connected with the pole piece through the clamping effect of the linear carbon material, so that the pole piece material not only can partially inhibit the silicon expansion, but also can simultaneously generate a certain reutilization effect on the crushed silicon particles.
Drawings
FIG. 1 is a microscopic morphology of a negative electrode after a pole piece is made of the negative electrode material.
Detailed Description
The invention is described in further detail below with reference to specific embodiments, but the scope of the invention is not limited to the following:
a preparation method of a carbon-silicon composite material for a lithium ion battery cathode comprises the following steps:
the method comprises the following steps: mixing nano silicon, conductive polymer, conductive carbon and iron-containing compound according to the weight ratio of 30-40: 20: 20: 1, mixing;
step two: adding the mixed powder prepared in the first step into an agate mortar for grinding for 1 hour;
step three: putting the powder ground in the step two into a tubular furnace, introducing inert gas for heating, and preserving heat for 2 hours at 600 ℃;
step four: and cooling and grinding the powder prepared in the step three to obtain the carbon-silicon composite material for the lithium ion battery cathode.
The nano silicon is silicon simple substance particles with the particle size of less than 100 nm.
The conductive polymer is one of polypyrrole or polythiophene.
The iron-containing compound is one of ferrous chloride or ferrous sulfate.
The inert gas is one of nitrogen or argon.
The microscopic morphology of the cathode after the carbon-silicon composite material for the lithium ion battery cathode prepared by the preparation method is prepared into a pole piece is shown in figure 1.
The principle of the invention is that under the catalysis of iron, the conductive polymer is carbonized at high temperature to form a linear carbon material; a high-strength linear carbon material is used for generating a spongy structure, the space can ensure that silicon fragments are closely connected with the pole piece when the silicon expands and is crushed, and the nano silicon material is mixed in the space; when the silicon particles are large, the silicon particles are easy to expand and break, and broken silicon cannot be separated from the pole piece in the spongy structure, so that the lithium storage effect is continuously exerted. When the particles are small, the particles exist in the linear carbon material directly, and silicon particles are bound in the expansion and contraction process and are difficult to separate from the pole piece. Thus, a battery cathode with high capacity and high repeatability can be obtained. But simple blending of carbon nanotubes with silicon particles is difficult to achieve all of the above objectives. The invention mixes the conductive polymer before carbonizing, so that the iron element with catalytic action is partially embedded into the silicon particles, and the conductive polymer is close to the silicon particles at the initial position of the formation of partial linear carbon material under the catalytic carbonization action of the iron element, so that the linear carbon material is more tightly combined with the silicon particles when forming and forming a sponge-shaped space. Thereby improving the utilization rate of the silicon particles.
Several embodiments of the invention are described below:
example 1
A preparation method of a carbon-silicon composite material for a lithium ion battery cathode comprises the following steps of mixing nano-silicon, polypyrrole, conductive carbon and ferrous chloride according to a ratio of 40: 20: 20: 1, mixing; putting the mixed powder into an agate mortar for grinding for 1 hour; putting the ground powder into a tube furnace, introducing argon gas for heating, and preserving heat for 2 hours at 600 ℃; and after cooling, grinding the obtained powder to be used as a negative electrode material. After the negative electrode material obtained by the method is prepared into a battery, the specific capacity of 1200mAh/g can still be reserved after the battery is cycled for 100 times.
Example 2
A preparation method of a carbon-silicon composite material for a lithium ion battery cathode comprises the following steps of mixing nano-silicon, polythiophene, conductive carbon and ferrous sulfate according to the weight ratio of 35: 20: 20: 1, mixing; putting the mixed powder into an agate mortar for grinding for 1 hour; putting the ground powder into a tube furnace, introducing argon gas for heating, and preserving heat for 2 hours at 600 ℃; and after cooling, grinding the obtained powder to be used as a negative electrode material. After the negative electrode material obtained by the method is made into a battery, the specific capacity of 1000mAh/g is still reserved after the battery is cycled for 100 times.
Example 3
A preparation method of a carbon-silicon composite material for a lithium ion battery cathode comprises the following steps of mixing nano-silicon, polythiophene, conductive carbon and ferrous sulfate according to the weight ratio of 30: 20: 20: 1, mixing; putting the mixed powder into an agate mortar for grinding for 1 hour; putting the ground powder into a tube furnace, introducing argon gas for heating, and preserving heat for 2 hours at 600 ℃; and after cooling, grinding the obtained powder to be used as a negative electrode material. After the negative electrode material obtained by the method is prepared into a battery, the specific capacity of 800mAh/g is still reserved after the battery is cycled for 100 times.
The invention is not limited to the examples, and any equivalent changes to the technical solution of the invention by a person skilled in the art after reading the description of the invention are covered by the claims of the invention.
Claims (2)
1. A preparation method of a carbon-silicon composite material for a lithium ion battery cathode is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: mixing nano silicon, conductive polymer, conductive carbon and iron-containing compound according to the weight ratio of 30-40: 20: 20: 1, mixing;
step two: adding the mixed powder prepared in the first step into an agate mortar for grinding for 40-60 min;
step three: putting the powder ground in the step two into a tubular furnace, introducing inert gas for heating, and preserving heat for 2 hours at 600 ℃;
step four: cooling and grinding the powder prepared in the step three to obtain the carbon-silicon composite material for the lithium ion battery cathode;
the nano silicon is silicon simple substance particles with the particle size of less than 100 nm;
the conductive polymer is one of polypyrrole or polythiophene;
the iron-containing compound is one of ferrous chloride or ferrous sulfate;
the inert gas is one of nitrogen or argon.
2. The carbon-silicon composite material for the negative electrode of the lithium ion battery prepared by the preparation method according to claim 1.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101210112A (en) * | 2006-12-29 | 2008-07-02 | 比亚迪股份有限公司 | Silicon-containing composite material and its preparation method and application |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101210112A (en) * | 2006-12-29 | 2008-07-02 | 比亚迪股份有限公司 | Silicon-containing composite material and its preparation method and application |
Non-Patent Citations (3)
| Title |
|---|
| "Novel Pyrolyzed Polyaniline-Grafted Silicon Nanoparticles Encapsulated in Graphene Sheets As Li-Ion Battery Anodes";Zhe-Fei Li，et al.;《ACS Appl. Mater. Interfaces》;20140404;第6卷(第8期);第5996-6002页 * |
| "硅/石墨/碳负极材料的制备及其在全电池中的应用研究";金继凯;《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》;20170228(第2期);第C042-2951页 * |
| "锂离子电池用硅/石墨/碳复合负极材料的电化学性能";亓鹏等;《功能材料》;20120315;第43卷(第5期);第657-659页 * |
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