CN107195874B - A kind of preparation method of the Si-C composite material of polypyrrole cladding - Google Patents
A kind of preparation method of the Si-C composite material of polypyrrole cladding Download PDFInfo
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- CN107195874B CN107195874B CN201710257184.3A CN201710257184A CN107195874B CN 107195874 B CN107195874 B CN 107195874B CN 201710257184 A CN201710257184 A CN 201710257184A CN 107195874 B CN107195874 B CN 107195874B
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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
- H01M4/366—Composites as layered products
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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
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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
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- 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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- H01M4/02—Electrodes composed of, or comprising, active material
- 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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Abstract
A kind of preparation method of the Si-C composite material of polypyrrole cladding; include the following steps: that (1) weighs graphite particle and is dissolved in distilled water to stir the first preset time and form the first mixture after mixing; it weighs in based particles the first mixture of addition and stirs the second preset time, graphite particle and based particles is made to form the second mixture after mixing；(2) it weighs pyrrole monomer and is dissolved in hydrogen chloride solution and stir evenly to form third mixture, the second mixture stirring third preset time is added in third mixture, the second mixture is made to be uniformly mixed to form the 4th mixture with third mixture；(3) it weighs ammonium persulfate and is dissolved in the 5th mixture of formation in hydrogen chloride solution, the 4th mixture is added in the 5th mixture after stirring evenly the 4th preset time of reaction after being filtered, washed and being dried, the Si-C composite material of polypyrrole cladding is made.
Description
[technical field]
The present invention relates to the Si-C composite materials of cell negative electrode material technical field more particularly to a kind of polypyrrole cladding
Preparation method.
[background technique]
Current commercialized lithium cell cathode material is mainly graphite type material, and theoretical specific capacity only has 372mAh/g,
It is unable to satisfy lithium battery high-energy density, small-size light-weight, the demand for development driven for a long time.Silica-base material has than graphite cathode
High theoretical specific capacity (4200mAh/g), and its rich reserves, are very promising lithium cell cathode materials, therefore
Recently it gets more and more people's extensive concerning.But silica-base material as negative electrode material in use, in charge and discharge process can and lithium close
Aurification, the volume expansion of silica-base material meeting at this time leads to itself dusting, and then active material can be made to peel off, fall above collector
Powder seriously affects the stability of lithium battery and the performance of reversible capacity.Therefore, it is necessary to seek one kind to improve graphite cathode
Capacity, and the method that the dusting in silicon-based anode cyclic process can be prevented, to meet wanting for lithium battery high-energy density development
It asks.However, the preparation method of existing silico-carbo material is mostly that carbon material and silica-base material progress are compound, either also with porous carbon
Simple graphite material, or first by silica-base material carry out specially treated carried out again with carbon material it is compound, finally all can be into
Row carbon coating handles to solve the expansion issues of silica-base material.But silica-base material needed in carbonisation 700 DEG C-
1000 DEG C of progress high-temperature process for a period of time, and will cause energy consumption height in carbonisation, problem at high cost.
In consideration of it, it is really necessary to provide a kind of preparation method of the Si-C composite material of novel polypyrrole cladding to overcome
Disadvantages described above.
[summary of the invention]
The object of the present invention is to provide a kind of preparation method of the Si-C composite material of polypyrrole cladding, preparation process letters
Single, low energy consumption, and then saves production cost.In addition, compound using the silicon-carbon of the polypyrrole cladding of preparation of the embodiment of the present invention
Material, expansion of the lithium battery further prepared as negative electrode material because can effectively inhibit based particles in charge and discharge process
Powder of detached, to improve the cycle performance of lithium battery.
To achieve the goals above, the present invention provides a kind of preparation method of the Si-C composite material of polypyrrole cladding, packet
Include following steps:
(1) first weigh that be dissolved in distilled water stirring first with graphite particle that the mass ratio of distilled water is 1:10-20 default
Time forms the first mixture after mixing, then weighs and is added with the mass ratio of graphite particle for the based particles of 1:2-20
The second preset time is stirred in first mixture, and graphite particle and based particles is made to form the second mixture, institute after mixing
The partial size for the based particles stated is 10nm-200nm；
(2) pyrrole monomer that the mass ratio for first weighing the gross mass with graphite particle and based particles is 1:1 is dissolved in chlorination
It stirs evenly to form third mixture in hydrogen solution, wherein the mass ratio of pyrrole monomer and hydrogen chloride solution is 1:1-5, is then existed
The second mixture stirring third preset time is added in third mixture, the second mixture is made to be uniformly mixed shape with third mixture
At the 4th mixture；
(3) it first weighs and is dissolved in hydrogen chloride solution that form the 5th mixed with ammonium persulfate that the mass ratio of pyrrole monomer is 1:1
Object is closed, wherein the mass ratio of ammonium persulfate and hydrogen chloride solution is 1:1-5, and the 4th mixture is added in the 5th mixture and is stirred
After being successively filtered, wash and dry after the 4th preset time of homogeneous reaction, the Si-C composite material of polypyrrole cladding is made.
Specifically, the first preset time described in step (1) are as follows: 1h-3h.
Specifically, the second preset time described in step (1) are as follows: 1h-3h.
Specifically, the third preset time described in step (2) are as follows: 0.5h-2h.
Specifically, the 4th preset time described in step (3) are as follows: 2h-4h.
Compared with prior art, the preparation method of the Si-C composite material of a kind of polypyrrole cladding provided by the invention, system
Standby process is simple, and low energy consumption, and then saves production cost.In addition, coated using the polypyrrole of preparation of the embodiment of the present invention
Si-C composite material, the lithium battery further prepared as negative electrode material in charge and discharge process because can effectively inhibit silicon substrate
The expansion powder of detached of grain, to improve the cycle performance of lithium battery.
[Detailed description of the invention]
Fig. 1 is the Si-C composite material structural schematic diagram of the polypyrrole cladding of preparation of the embodiment of the present invention.
Fig. 2 is the Si-C composite material that polypyrrole prepare using the embodiment of the present invention coats, as negative electrode material into one
Walk circulation-specific volume spirogram of the lithium battery of preparation.
[specific embodiment]
It is clear in order to be more clear the purpose of the present invention, technical solution and advantageous effects, below in conjunction with attached drawing and
Specific embodiment, the present invention will be described in further detail.It should be understood that specific implementation described in this specification
Mode is not intended to limit the present invention just for the sake of explaining the present invention.
The present invention provides a kind of preparation method of the Si-C composite material of polypyrrole cladding, includes the following steps:
(1) first weigh that be dissolved in distilled water stirring first with graphite particle that the mass ratio of distilled water is 1:10-20 default
Time forms the first mixture after mixing, then weighs and is added with the mass ratio of graphite particle for the based particles of 1:2-20
The second preset time is stirred in first mixture, and graphite particle and based particles is made to form the second mixture, institute after mixing
The partial size for the based particles stated is 10nm-200nm；
(2) pyrrole monomer that the mass ratio for first weighing the gross mass with graphite particle and based particles is 1:1 is dissolved in chlorination
It stirs evenly to form third mixture in hydrogen solution, wherein the mass ratio of pyrrole monomer and hydrogen chloride solution is 1:1-5, is then existed
The second mixture stirring third preset time is added in third mixture, the second mixture is made to be uniformly mixed shape with third mixture
At the 4th mixture；
(3) it first weighs and is dissolved in hydrogen chloride solution that form the 5th mixed with ammonium persulfate that the mass ratio of pyrrole monomer is 1:1
Object is closed, wherein the mass ratio of ammonium persulfate and hydrogen chloride solution is 1:1-5, and the 4th mixture is added in the 5th mixture and is stirred
After being successively filtered, wash and dry after the 4th preset time of homogeneous reaction, the Si-C composite material of polypyrrole cladding is made.
Specifically, the first preset time described in step (1) are as follows: 1h-3h.
Specifically, the second preset time described in step (1) are as follows: 1h-3h.
Specifically, the third preset time described in step (2) are as follows: 0.5h-2h.
Specifically, the 4th preset time described in step (3) are as follows: 2h-4h.
Embodiment:
(1) it first weighs to be dissolved in 1000g distilled water with the mass ratio of distilled water for the 100g graphite particle of 1:10 and stirs 1h
The first mixture is formed after mixing, and then weighing the 12.5g partial size for being 1:8 with the mass ratio of graphite particle is 200nm's
Based particles are added in the first mixture and stir 1h, and graphite particle and based particles is made to form the second mixture after mixing.
(2) pyrrole monomer for the 112.5g that the mass ratio for first weighing the gross mass with graphite particle and based particles is 1:1
It is dissolved in the hydrogen chloride solution of 450g and stirs evenly to form third mixture, the second mixture is then added in third mixture
0.5h is stirred, is that the second mixture is uniformly mixed to form the 4th mixture with third mixture.
(3) it is molten first to weigh the hydrogen chloride for being dissolved in 450g with the ammonium persulfate for the 112.5g that the mass ratio of pyrrole monomer is 1:1
In liquid formed the 5th mixture, will the 4th mixture be added the 5th mixture in stir evenly reaction 2h after be successively filtered,
After washing and drying, the Si-C composite material of polypyrrole cladding is made.
Fig. 1 is the Si-C composite material structural schematic diagram of the polypyrrole cladding of preparation of the embodiment of the present invention；Fig. 2 is using this
The Si-C composite material of the polypyrrole cladding of inventive embodiments preparation, the lithium battery further prepared as negative electrode material follow
Ring-specific volume spirogram.
By Fig. 1 to Fig. 2 it is found that the embodiment of the present invention preparation polypyrrole cladding Si-C composite material, with graphite particle
For core, polypyrrole layer is coated on outermost layer, and based particles dispersion is embedded in polypyrrole layer, and the silicon-carbon for coating polypyrrole is multiple
Condensation material has certain elasticity, can inhibit the expansion powder of detached of the based particles in charge and discharge process.In addition, application is originally
The Si-C composite material of the polypyrrole cladding of inventive embodiments preparation, the lithium battery further prepared as negative electrode material is because filling
The expansion powder of detached that based particles can effectively be inhibited in discharge process, to improve the cycle performance of lithium battery.
In conclusion a kind of preparation method of the Si-C composite material of polypyrrole cladding provided by the invention, preparation process
Simply, low energy consumption, and then saves production cost.In addition, multiple using the silicon-carbon of the polypyrrole cladding of preparation of the embodiment of the present invention
Condensation material, the lithium battery further prepared as negative electrode material in charge and discharge process because can effectively inhibit the swollen of based particles
Swollen powder of detached, to improve the cycle performance of lithium battery.
The present invention is not only in the description and the implementation described, therefore for the personnel of familiar field
Other advantage and modification is easily implemented, therefore in the essence without departing substantially from universal defined by claim and equivalency range
In the case where mind and range, the present invention is not limited to specific details, representative equipment and diagrams shown and described herein
Example.
Claims (1)
1. a kind of preparation method of the Si-C composite material of polypyrrole cladding, which comprises the steps of:
(1) it first weighs to be dissolved in distilled water with the mass ratio of distilled water for the graphite particle of 1:10 and stirs 1h-3h after mixing
The first mixture is formed, then weighs to be added in the first mixture with the mass ratio of graphite particle for the based particles of 1:8 and stir
1h-3h makes graphite particle and based particles form the second mixture after mixing, and the partial size of the based particles is
10nm-200nm；
(2) it is molten that the pyrrole monomer that the mass ratio for first weighing the gross mass with graphite particle and based particles is 1:1 is dissolved in hydrogen chloride
It stirs evenly to form third mixture in liquid, wherein the mass ratio of pyrrole monomer and hydrogen chloride solution is 1:1, then mixed in third
It closes and the second mixture stirring 0.5h-2h is added in object, the second mixture is made to be uniformly mixed to form the 4th mixing with third mixture
Object；
(3) it first weighs and is dissolved in the 5th mixture of formation in hydrogen chloride solution with the mass ratio of pyrrole monomer for the ammonium persulfate of 1:1,
Wherein the mass ratio of ammonium persulfate and hydrogen chloride solution is 1:1, and the 4th mixture is added in the 5th mixture and is stirred evenly instead
After answering 2h-4h, using graphite particle as core, polypyrrole layer is coated on outermost layer, and based particles dispersion is embedded in polypyrrole layer,
After being successively filtered, wash and drying, the Si-C composite material of polypyrrole cladding is made.
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| CN111224078A (en) * | 2018-11-27 | 2020-06-02 | 广州汽车集团股份有限公司 | Silicon-based composite negative electrode material, preparation method thereof and lithium ion battery negative electrode |
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| CN102447113A (en) * | 2011-12-12 | 2012-05-09 | 南开大学 | Lithium battery with polymer-coated sulfur/carbon composite material as anode |
| CN104332600A (en) * | 2014-10-24 | 2015-02-04 | 东莞市翔丰华电池材料有限公司 | Method for preparing graphene/sulfur/conductive polymer composite material used for lithium-sulfur battery positive electrode |
| CN105098185A (en) * | 2014-04-29 | 2015-11-25 | 华为技术有限公司 | Composite cathode material, preparation method thereof, lithium ion secondary battery negative plate and lithium ion secondary battery |
| CN105226254A (en) * | 2015-10-16 | 2016-01-06 | 李家晓 | A kind of silicon nanoparticle-graphite nano plate-carbon fibre composite and preparation method thereof and application |
| CN105958031A (en) * | 2016-06-30 | 2016-09-21 | 湖南桑顿新能源有限公司 | Sulfur-based cathode composite material and preparation method thereof |
| CN106505189A (en) * | 2015-12-08 | 2017-03-15 | 上海杉杉科技有限公司 | A kind of three-dimensional silica-polypyrrole-graphite cathode material and preparation method thereof |
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- 2017-04-19 CN CN201710257184.3A patent/CN107195874B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102447113A (en) * | 2011-12-12 | 2012-05-09 | 南开大学 | Lithium battery with polymer-coated sulfur/carbon composite material as anode |
| CN105098185A (en) * | 2014-04-29 | 2015-11-25 | 华为技术有限公司 | Composite cathode material, preparation method thereof, lithium ion secondary battery negative plate and lithium ion secondary battery |
| CN104332600A (en) * | 2014-10-24 | 2015-02-04 | 东莞市翔丰华电池材料有限公司 | Method for preparing graphene/sulfur/conductive polymer composite material used for lithium-sulfur battery positive electrode |
| CN105226254A (en) * | 2015-10-16 | 2016-01-06 | 李家晓 | A kind of silicon nanoparticle-graphite nano plate-carbon fibre composite and preparation method thereof and application |
| CN106505189A (en) * | 2015-12-08 | 2017-03-15 | 上海杉杉科技有限公司 | A kind of three-dimensional silica-polypyrrole-graphite cathode material and preparation method thereof |
| CN105958031A (en) * | 2016-06-30 | 2016-09-21 | 湖南桑顿新能源有限公司 | Sulfur-based cathode composite material and preparation method thereof |
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Effective date of registration: 20191017 Address after: 518000 Shenyu Science and Technology Park, No. 68 Lanjingbei Road, Laokeng Community, Longtian Street, Pingshan District, Shenzhen City, Guangdong Province, 101 Patentee after: Shenzhen Anding New Energy Technology Development Co., Ltd. Address before: 518000 Guangdong Province, Shenzhen City Pingshan Pingshan community Zhu Keng Industrial Zone 9 1-3 Patentee before: Shenzhen Optimum Battery Co., Ltd. |
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