CN107195874A - 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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- CN107195874A CN107195874A CN201710257184.3A CN201710257184A CN107195874A CN 107195874 A CN107195874 A CN 107195874A CN 201710257184 A CN201710257184 A CN 201710257184A CN 107195874 A CN107195874 A CN 107195874A
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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
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- 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, comprises the following steps：(1) weigh graphite particle be dissolved in distilled water stir the first preset time it is well mixed after form the first mixture; weigh in based particles the first mixture of addition and stir the second preset time, graphite particle is formed the second mixture after being well mixed with based particles；(2) weigh pyrrole monomer and be dissolved in hydrogen chloride solution and stir to form the 3rd mixture, the second mixture is added in the 3rd mixture and stirs the 3rd preset time, makes the second mixture be well mixed to form the 4th mixture with the 3rd mixture；(3) weigh ammonium persulfate and be dissolved in the 5th mixture of formation in hydrogen chloride solution, the 4th mixture is added after being filtered, washed and dried after the 4th preset time of reaction that stirred in the 5th mixture, the Si-C composite material of polypyrrole cladding is made.
Description
【Technical field】
The present invention relates to cell negative electrode material technical field, more particularly to a kind of polypyrrole cladding Si-C composite material
Preparation method.
【Background technology】
Current commercialized lithium cell cathode material is mainly graphite type material, and its theoretical specific capacity only has 372mAh/g,
Lithium battery high-energy-density, small-size light-weight, the demand for development of driving for a long time can not be met.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 get more and more people's extensive concerning.But silica-base material as negative material in use, in charge and discharge process can and lithium close
Aurification, now silica-base material meeting volumetric expansion causes itself efflorescence, and then active material can be made to peel off, fall above collector
Powder, has a strong impact on the stability of lithium battery and the performance of reversible capacity.Accordingly, it would be desirable to seek a kind of to improve graphite cathode
Capacity, the method that the efflorescence in silicon-based anode cyclic process can be prevented again, to meet wanting for lithium battery high-energy-density development
Ask.It is combined however, the preparation method of existing silico-carbo material is generally carbon material with silica-base material, either with porous carbon also
Simple graphite material, or first by silica-base material progress specially treated be combined again with carbon material, it finally can all enter
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 carry out high-temperature process for a period of time, and high energy consumption can be caused in carbonisation, the problem of cost is high.
In consideration of it, real be necessary to provide a kind of preparation method of the Si-C composite material of new polypyrrole cladding to overcome
Disadvantages described above.
【The content of the invention】
It is an object of the invention to provide a kind of preparation method of the Si-C composite material of polypyrrole cladding, preparation process letter
Single, energy consumption is low, and then saves production cost.In addition, the silicon-carbon of the polypyrrole cladding prepared using the embodiment of the present invention is combined
Material, the lithium battery further prepared as negative material in charge and discharge process because can effectively suppress the expansion of based particles
Powder of detached, so as to improve the cycle performance of lithium battery.
To achieve these goals, the present invention provides a kind of preparation method of the Si-C composite material of polypyrrole cladding, bag
Include following steps：
(1) mass ratio first weighed with distilled water is 1：10-20 graphite particle is dissolved in stirring first in distilled water and preset
The first mixture is formed after time is well mixed, the mass ratio then weighed with graphite particle is 1：2-20 based particles are added
The second preset time is stirred in first mixture, graphite particle is formed the second mixture after being well mixed with based particles；
(2) mass ratio for first weighing the gross mass with graphite particle and based particles is 1：1 pyrrole monomer is dissolved in chlorination
Stir to form the 3rd mixture in hydrogen solution, wherein the mass ratio of pyrrole monomer and hydrogen chloride solution is 1：1-5, Ran Hou
The second mixture is added in 3rd mixture and stirs the 3rd preset time, the second mixture is well mixed shape with the 3rd mixture
Into the 4th mixture；
(3) mass ratio first weighed with pyrrole monomer is 1：1 ammonium persulfate, which is dissolved in formation the 5th in hydrogen chloride solution, to be mixed
The mass ratio of compound, wherein ammonium persulfate and hydrogen chloride solution is 1：1-5, the 4th mixture is added in the 5th mixture and stirred
After being filtered, washed and dried successively after the preset time of homogeneous reaction the 4th, the Si-C composite material of polypyrrole cladding is made.
Specifically, the first preset time described in step (1) is：1h-3h.
Specifically, the second preset time described in step (1) is：1h-3h.
Specifically, the particle diameter of the based particles described in step (1) is 10nm-200nm.
Specifically, the 3rd preset time described in step (2) is：0.5h-2h.
Specifically, the 4th preset time described in step (3) is：2h-4h.
Compared with prior art, a kind of preparation method of the Si-C composite material for polypyrrole cladding that the present invention is provided, system
Standby process is simple, and energy consumption is low, and then saves production cost.In addition, the polypyrrole cladding prepared using the embodiment of the present invention
Si-C composite material, the lithium battery further prepared as negative material in charge and discharge process because can effectively suppress silicon substrate
The expansion powder of detached of grain, so as to improve the cycle performance of lithium battery.
【Brief description of the drawings】
Fig. 1 is the Si-C composite material structural representation of polypyrrole cladding prepared by the embodiment of the present invention.
Fig. 2 is the Si-C composite material of polypyrrole cladding prepared by the application embodiment of the present invention, and one is entered as negative material
Walk circulation-specific volume spirogram of the lithium battery prepared.
【Embodiment】
In order that the purpose of the present invention, technical scheme and advantageous effects become apparent from understanding, below in conjunction with accompanying drawing and
Embodiment, the present invention will be described in further detail.It should be appreciated that the 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, comprises the following steps：
(1) mass ratio first weighed with distilled water is 1：10-20 graphite particle is dissolved in stirring first in distilled water and preset
The first mixture is formed after time is well mixed, the mass ratio then weighed with graphite particle is 1：2-20 based particles are added
The second preset time is stirred in first mixture, graphite particle is formed the second mixture after being well mixed with based particles；
(2) mass ratio for first weighing the gross mass with graphite particle and based particles is 1：1 pyrrole monomer is dissolved in chlorination
Stir to form the 3rd mixture in hydrogen solution, wherein the mass ratio of pyrrole monomer and hydrogen chloride solution is 1：1-5, Ran Hou
The second mixture is added in 3rd mixture and stirs the 3rd preset time, the second mixture is well mixed shape with the 3rd mixture
Into the 4th mixture；
(3) mass ratio first weighed with pyrrole monomer is 1：1 ammonium persulfate, which is dissolved in formation the 5th in hydrogen chloride solution, to be mixed
The mass ratio of compound, wherein ammonium persulfate and hydrogen chloride solution is 1：1-5, the 4th mixture is added in the 5th mixture and stirred
After being filtered, washed and dried successively after the preset time of homogeneous reaction the 4th, the Si-C composite material of polypyrrole cladding is made.
Specifically, the first preset time described in step (1) is：1h-3h.
Specifically, the second preset time described in step (1) is：1h-3h.
Specifically, the particle diameter of the based particles described in step (1) is 10nm-200nm.
Specifically, the 3rd preset time described in step (2) is：0.5h-2h.
Specifically, the 4th preset time described in step (3) is：2h-4h.
Embodiment：
(1) mass ratio first weighed with distilled water is 1：10 100g graphite particles, which are dissolved in 1000g distilled water, stirs 1h
The first mixture is formed after well mixed, the mass ratio then weighed with graphite particle is 1：8 12.5g particle diameters are 200nm's
Based particles add in the first mixture and stir 1h, graphite particle is formed the second mixture after being well mixed with based particles.
(2) mass ratio for first weighing the gross mass with graphite particle and based particles is 1：1 112.5g pyrrole monomer
Stir to form the 3rd mixture in the hydrogen chloride solution for being dissolved in 450g, then add the second mixture in the 3rd mixture
0.5h is stirred, is that the second mixture is well mixed to form the 4th mixture with the 3rd mixture.
(3) mass ratio first weighed with pyrrole monomer is 1：The hydrogen chloride that 1 112.5g ammonium persulfate is dissolved in 450g is molten
The 5th mixture is formed in liquid, will successively be filtered after the reaction 2h that stirred in the 4th mixture the 5th mixture of addition,
After washing and drying, the Si-C composite material of polypyrrole cladding is made.
Fig. 1 is the Si-C composite material structural representation of polypyrrole cladding prepared by the embodiment of the present invention；Fig. 2 is using this
The Si-C composite material of polypyrrole cladding prepared by inventive embodiments, the lithium battery that is further prepared as negative material is followed
Ring-specific volume spirogram.
From Fig. 1 to Fig. 2, the Si-C composite material of polypyrrole cladding prepared by the embodiment of the present invention, with graphite particle
For core, polypyrrole layer is coated on outermost layer, and based particles are scattered to be embedded in polypyrrole layer, answers the silicon-carbon that polypyrrole is coated
Condensation material has certain elasticity, can suppress 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 polypyrrole cladding prepared by inventive embodiments, the lithium battery further prepared as negative material is because filling
The expansion powder of detached of based particles can effectively be suppressed in discharge process, so as to improve the cycle performance of lithium battery.
In summary, a kind of preparation method of the Si-C composite material for polypyrrole cladding that the present invention is provided, preparation process
Simply, energy consumption is low, and then saves production cost.In addition, the silicon-carbon of the polypyrrole cladding prepared using the embodiment of the present invention is answered
Condensation material, the lithium battery further prepared as negative material in charge and discharge process because can effectively suppress the swollen of based particles
Swollen powder of detached, so as to improve the cycle performance of lithium battery.
The present invention is not restricted to described in specification and embodiment, therefore for the personnel of familiar field
Additional advantage and modification is easily achieved, therefore in the essence of the universal limited without departing substantially from claim and equivalency range
In the case of refreshing and scope, the present invention is not limited to specific details, representational equipment and shown here as the diagram with description
Example.
Claims (6)
1. a kind of preparation method of the Si-C composite material of polypyrrole cladding, it is characterised in that comprise the following steps：
(1) mass ratio first weighed with distilled water is 1：10-20 graphite particle, which is dissolved in distilled water, stirs the first preset time
The first mixture is formed after well mixed, the mass ratio then weighed with graphite particle is 1：2-20 based particles add first
The second preset time is stirred in mixture, graphite particle is formed the second mixture after being well mixed with based particles；
(2) mass ratio for first weighing the gross mass with graphite particle and based particles is 1：It is molten that 1 pyrrole monomer is dissolved in hydrogen chloride
Stir to form the 3rd mixture in liquid, wherein the mass ratio of pyrrole monomer and hydrogen chloride solution is 1：1-5, then the 3rd
The second mixture is added in mixture and stirs the 3rd preset time, makes the second mixture be well mixed to form the with the 3rd mixture
Four mixtures；
(3) mass ratio first weighed with pyrrole monomer is 1：1 ammonium persulfate is dissolved in the 5th mixture of formation in hydrogen chloride solution,
Wherein the mass ratio of ammonium persulfate and hydrogen chloride solution is 1：1-5, the 4th mixture is added and stirred in the 5th mixture
React after being filtered, washed and dried successively after the 4th preset time, the Si-C composite material of polypyrrole cladding is made.
2. the preparation method of the Si-C composite material of polypyrrole cladding according to claim 1, it is characterised in that：Step
(1) the first preset time described in is：1h-3h.
3. the preparation method of the Si-C composite material of polypyrrole cladding according to claim 1, it is characterised in that：Step
(1) the second preset time described in is：1h-3h.
4. the preparation method of the Si-C composite material of polypyrrole cladding according to claim 1, it is characterised in that：Step
(1) particle diameter of the based particles described in is 10nm-200nm.
5. the preparation method of the Si-C composite material of polypyrrole cladding according to claim 1, it is characterised in that：Step
(2) the 3rd preset time described in is：0.5h-2h.
6. the preparation method of the Si-C composite material of polypyrrole cladding according to claim 1, it is characterised in that：Step
(3) the 4th preset time described in is：2h-4h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| 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 |
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| 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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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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Granted publication date: 20190528 Termination date: 20200419 |