CN104993112A - Preparation method for silicon-carbon composite material - Google Patents
Preparation method for silicon-carbon composite material Download PDFInfo
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- CN104993112A CN104993112A CN201510344564.1A CN201510344564A CN104993112A CN 104993112 A CN104993112 A CN 104993112A CN 201510344564 A CN201510344564 A CN 201510344564A CN 104993112 A CN104993112 A CN 104993112A
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- composite material
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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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- 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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to a preparation method for a silicon-carbon composite material, and belongs to the technical field of carbon composite material preparation. The preparation method comprises the specific steps that carbohydrate, high polymer, silicon powder and organic solvent are subjected to reaction in a sealed vessel at the temperature ranging from 150 DEG C-250 DEG C, and the silicon-carbon composite material is obtained through drying and calcination. The preparation method for the silicon-carbon composite material has the advantages that the needed material is easy to acquire, the cost is low, and the preparation process is easy. The prepared silicon-carbon composite material has the advantages of being small and controllable in size, high in the specific capacity and excellent in the cycle performance.
Description
Technical field
The present invention relates to a kind of preparation method of Si-C composite material, belong to carbon composite preparing technical field.
Background technology
Graphite negative electrodes material has high cycle efficieny and good cycle performance, has been widely used in preparing lithium ion battery negative material.But its theoretical specific capacity only has 372 mAh/g, need development of new negative material to improve the chemical property of lithium ion battery for this reason.At present, silicon materials, owing to having high power capacity, aboundresources and the advantage such as close with material with carbon element current potential, become the candidate material of lithium ion battery negative material.But, silicon materials high level de-/embedding lithium under, there is serious bulk effect, easily cause structure collapses, active material comes off, the cyclical stability of battery declines greatly.In recent years, people improve the cycle performance of silicon materials by the following method: (1) reduces particle size; (2) silicon thin film is prepared; (3) silicon based composite material is prepared; (4) prepare the nano material of special construction, as silicon nanowires, nucleocapsid structure material, spherical silicon/graphite composite material etc., make material in cyclic process, keep pattern, improve the cycle performance of electrode.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Si-C composite material.
Implementation procedure of the present invention is as follows:
A preparation method for Si-C composite material, step is as follows: in closed container, and by saccharide compound, high polymer, silica flour and organic solvent after 150 ~ 250 DEG C of reactions, drying, calcining obtain Si-C composite material,
The mass ratio of above-mentioned saccharide compound, high polymer, silica flour and organic solvent is 1:1:0.5:5 ~ 1:0.1:0.1:0.5; Described saccharide compound is selected from monose or disaccharides; Described high polymer is selected from polyvinylpyrrolidone, polyacrylic acid, polyacrylamide, polyethylene glycol, polyvinyl alcohol.
Above-mentioned saccharide compound is selected from glucose, fructose, galactolipin, sucrose, maltose, lactose.
Above-mentioned organic solvent is selected from formic acid, acetic acid, propionic acid, methyl alcohol, ethanol, ethylene glycol, isopropyl alcohol, butanols, acetonitrile, carrene, chloroform, N, dinethylformamide, DMA, dimethyl sulfoxide (DMSO), thionyl chloride, 1-METHYLPYRROLIDONE.
Dry employing freeze drying or CO 2 supercritical drying.
Optimal reaction temperature is 160 ~ 200 DEG C.
Calcining heat in above-mentioned preparation method is 300 ~ 1200 DEG C.
The application of Si-C composite material in lithium ion battery negative material prepared by said method.
Advantage of the present invention: (1) raw material of the present invention is easy to get, and cost is low, and preparation process is simple; (2) size of the Si-C composite material prepared is little and controlled; (3) composite material prepared by has higher specific capacity, excellent cycle performance; (4) in Si-C composite material, carbon is the mixed conductor of ion and electronics, and not only in charge and discharge process, change in volume is little, and has good ductility and elasticity, is conducive to improving the conductivity of silicon electrode and the change in volume of buffering silicon.
Accompanying drawing explanation
Fig. 1 is the photo of cylindric gel prepared by embodiment 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of Si-C composite material prepared by embodiment 1;
Fig. 3 is that the EDX of Si-C composite material prepared by embodiment 1 can spectrogram.
Embodiment
Embodiment 1
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30), 0.3g silica flour and 3mL glacial acetic acid, react 8 hours at 200 DEG C, obtain cylindric gel and see Fig. 1 after reaction terminates, gel after freeze drying in a nitrogen atmosphere 1000 DEG C of calcinings within 1 hour, obtain Si-C composite material.Its scanning electron microscope (SEM) photograph is shown in Fig. 2, and as can be seen from the figure, composite material is that spherical, size is about 100 nm; Its EDX power spectrum is shown in Fig. 3, and composite material contains carbon, oxygen, silicon three kinds of elements as seen from the figure.
Embodiment 2
In closed reactor, add 1g fructose, 0.1g polyacrylic acid, 0.1g silica flour and 0.5mL formic acid, at 160 DEG C react 8 hours, reaction terminate after obtain cylindric gel, gel after CO 2 supercritical drying in a nitrogen atmosphere 500 DEG C of calcinings within 4 hours, obtain Si-C composite material.
Embodiment 3
In closed reactor, add 1g maltose, 0.1g polyacrylamide, 0.2g silica flour and 3mL ethylene glycol, at 200 DEG C react 8 hours, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 300 DEG C of calcinings within 4 hours, obtain Si-C composite material.
Embodiment 4
In closed reactor, add 1g lactose, 0.5g polyvinyl alcohol, 0.5g silica flour and 5mL ethanol, at 250 DEG C react 4 hours, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 1200 DEG C of calcinings within 1 hour, obtain Si-C composite material.
Embodiment 5
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30), 0.4g silica flour and 3mL butanols, react 8 hours at 200 DEG C, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 800 DEG C of calcinings within 3 hours, obtain Si-C composite material.
Embodiment 6
In closed reactor, add 1g galactolipin, 0.1g polyacrylic acid, 0.5g silica flour and 3.5mL propionic acid, at 180 DEG C react 8 hours, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 1000 DEG C of calcinings within 1 hour, obtain Si-C composite material.
Embodiment 7
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30), 0.1g silica flour and 1mL acetonitrile, react 8 hours at 200 DEG C, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 1200 DEG C of calcinings within 1 hour, obtain Si-C composite material.
Embodiment 8
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30), 0.1g silica flour and 3mL carrene, react 8 hours at 200 DEG C, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 1000 DEG C of calcinings within 1 hour, obtain Si-C composite material.
Embodiment 9
In closed reactor, add 1g sucrose, 0.1g polyvinylpyrrolidone (K30), 0.2g silica flour and 3mL chloroform, react 8 hours at 200 DEG C, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 800 DEG C of calcinings within 4 hours, obtain Si-C composite material.
Embodiment 10
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30), 0.3g silica flour and 0.5 mL N, dinethylformamide, react 8 hours at 200 DEG C, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 800 DEG C of calcinings within 3 hours, obtain Si-C composite material.
Embodiment 11
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30), 0.4g silica flour and 3mL N, N-dimethylacetylamide, react 8 hours at 200 DEG C, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 1000 DEG C of calcinings within 1 hour, obtain Si-C composite material.
Embodiment 12
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30), 0.5g silica flour and 1mL dimethyl sulfoxide (DMSO), react 8 hours at 200 DEG C, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 1000 DEG C of calcinings within 1 hour, obtain Si-C composite material.
Embodiment 13
In closed reactor, add 1g sucrose, 1g polyethylene glycol (PEG-4000), 0.1g silica flour and 2mL methyl alcohol, at 200 DEG C react 8 hours, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 1000 DEG C of calcinings within 1 hour, obtain Si-C composite material.
Embodiment 14
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30), 0.2g silica flour and 3mL thionyl chloride, react 8 hours at 200 DEG C, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 500 DEG C of calcinings within 2 hours, obtain Si-C composite material.
Embodiment 15
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30), 0.1g silica flour and 2.5mL 1-METHYLPYRROLIDONE, react 8 hours at 200 DEG C, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 1000 DEG C of calcinings within 1 hour, obtain Si-C composite material.
Embodiment 16
In closed reactor, add 1g glucose, 1g polyvinylpyrrolidone (K30), 0.5g silica flour and 5mL isopropyl alcohol, react 10 hours at 150 DEG C, reaction terminate after obtain cylindric gel, gel after freeze drying in a nitrogen atmosphere 1200 DEG C of calcinings within 1 hour, obtain Si-C composite material.
Embodiment 17 electrochemical property test
The cycle performance of Si-C composite material prepared by testing example 1 in 2032 type button cells.
Electrode material consists of active material: conductive agent: the mass ratio of PVDF is 70:20:10;
Be metal lithium sheet to electrode;
Electrolyte is 1 mol/L LiPF
6eC/DMC(volume ratio be 1:1) solution;
Barrier film is Cellgard2400 barrier film.
Test result shows, Si-C composite material prepared by the present invention first discharge capacity is 1983.1 mAh/g, charging capacity 1685.5 mAh/g, and coulombic efficiency is 85% first.Circulate after 100 times, electrode reversible capacity is 1275.8 mAh/g, illustrates that this material has high power capacity, good stability.
Claims (8)
1. a preparation method for Si-C composite material, is characterized in that: in closed container, and by saccharide compound, high polymer, silica flour and organic solvent after 150 ~ 250 DEG C of reactions, drying, calcining obtain Si-C composite material,
The mass ratio of described saccharide compound, high polymer, silica flour and organic solvent is 1:1:0.5:5 ~ 1:0.1:0.1:0.5; Described saccharide compound is selected from monose or disaccharides; Described high polymer is selected from polyvinylpyrrolidone, polyacrylic acid, polyacrylamide, polyethylene glycol, polyvinyl alcohol.
2. the preparation method of Si-C composite material according to claim 1, is characterized in that: described saccharide compound is selected from glucose, fructose, galactolipin, sucrose, maltose, lactose.
3. according to the preparation method of the Si-C composite material described in claim 1, it is characterized in that: described organic solvent is selected from formic acid, acetic acid, propionic acid, methyl alcohol, ethanol, ethylene glycol, isopropyl alcohol, butanols, acetonitrile, carrene, chloroform, N, dinethylformamide, DMA, dimethyl sulfoxide (DMSO), thionyl chloride, 1-METHYLPYRROLIDONE.
4. according to the preparation method of the Si-C composite material described in claim 1, it is characterized in that: dry employing freeze drying or CO 2 supercritical drying.
5. according to the preparation method of the Si-C composite material described in claim 1, it is characterized in that: reaction temperature is 160 ~ 200 DEG C.
6. according to the preparation method of the Si-C composite material described in claim 1, it is characterized in that: calcining heat is 300 ~ 1200 DEG C.
7. the Si-C composite material that obtains of preparation method described in claim 1.
8. the application of Si-C composite material according to claim 7 in lithium ion battery negative material.
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| CN201510344564.1A CN104993112A (en) | 2015-06-23 | 2015-06-23 | Preparation method for silicon-carbon composite material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106129371A (en) * | 2016-08-24 | 2016-11-16 | 宁波嘉宁电池科技有限责任公司 | A kind of assembled battery of Si-C composite material |
| CN106941171A (en) * | 2017-04-26 | 2017-07-11 | 中能国盛动力电池技术（北京）股份公司 | A kind of cathode of lithium battery composite based on nano-silicone wire/carbon and preparation method thereof |
| CN108428879A (en) * | 2018-03-30 | 2018-08-21 | 河北民族师范学院 | A kind of preparation method and application of New Type of Carbon silicon based composite material |
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| CN103022442A (en) * | 2012-12-05 | 2013-04-03 | 上海锦众信息科技有限公司 | Method for preparing negative-pole silicon-carbon composite material for lithium ion battery |
| CN103022444A (en) * | 2012-12-05 | 2013-04-03 | 上海锦众信息科技有限公司 | Preparation method of carbon silicon composite material |
| CN103618071A (en) * | 2013-11-14 | 2014-03-05 | 中国科学院广州能源研究所 | Carbon-silicon composite negative electrode material of lithium ion battery and preparation method thereof |
| CN104577045A (en) * | 2014-12-20 | 2015-04-29 | 江西正拓新能源科技股份有限公司 | Silicon-carbon composite material of lithium ion battery and preparation method of silicon-carbon composite material |
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2015
- 2015-06-23 CN CN201510344564.1A patent/CN104993112A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101826612A (en) * | 2009-03-06 | 2010-09-08 | 五邑大学 | Preparation method of lithium ion battery silicon-carbon cathode material |
| CN103022442A (en) * | 2012-12-05 | 2013-04-03 | 上海锦众信息科技有限公司 | Method for preparing negative-pole silicon-carbon composite material for lithium ion battery |
| CN103022444A (en) * | 2012-12-05 | 2013-04-03 | 上海锦众信息科技有限公司 | Preparation method of carbon silicon composite material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106129371A (en) * | 2016-08-24 | 2016-11-16 | 宁波嘉宁电池科技有限责任公司 | A kind of assembled battery of Si-C composite material |
| CN106941171A (en) * | 2017-04-26 | 2017-07-11 | 中能国盛动力电池技术（北京）股份公司 | A kind of cathode of lithium battery composite based on nano-silicone wire/carbon and preparation method thereof |
| CN108428879A (en) * | 2018-03-30 | 2018-08-21 | 河北民族师范学院 | A kind of preparation method and application of New Type of Carbon silicon based composite material |
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