CN105261733A - Preparation method of nano silicon-based/carbon composite material - Google Patents
Preparation method of nano silicon-based/carbon composite material Download PDFInfo
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- CN105261733A CN105261733A CN201510566512.9A CN201510566512A CN105261733A CN 105261733 A CN105261733 A CN 105261733A CN 201510566512 A CN201510566512 A CN 201510566512A CN 105261733 A CN105261733 A CN 105261733A
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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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- 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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- 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
Abstract
The invention provides a preparation method of a nano silicon-based/carbon composite material. The method comprises the following steps: firstly, coating a nano silicon surface with a micro-pore carbon layer by organic resin and a pore forming material in a liquid phase; and then adopting fermented starch as a carbon source, and carrying out coating and high-temperature carbonization to prepare the nano silicon-based/carbon composite material. The nano silicon-based/carbon composite material with pomegranate-type structure characteristics can be prepared by the method provided by the invention. When the nano silicon-based/carbon composite material is applied to a preparation of a lithium-ion battery anode material, the problems of a rapid volume expansion in a lithium intercalation process and grain breakage, pulverization and falling in a circulating process can be effectively solved; the specific capacity of the material can be up to 450-950mAh/g; and the capacity retention ratio is 85%-92% after circulating charge and discharge for 500 cycles.
Description
Technical field
The present invention relates to a kind of preparation method of nano silicon material, particularly a kind of nano silicon-based/preparation method of carbon composite.
Background technology
The theoretical specific capacity of the graphite-like carbon negative pole material of now widely used lithium ion battery is only 372mAh/g, limits the application of lithium ion battery to high-energy-density direction.Silica-base material is due to its high embedding lithium capacity, and high-lithium ion diffusivity, has become the first-selection of lithium ion battery negative material carbon substitution material.But, because Si is in Electrochemical lithiation process, there is complicated phase transformation simultaneously with great change in volume, up to the change in volume of more than 300% in silica-base material doff lithium process, make it break in charge and discharge process, efflorescence, to come off, cause cycle performance of battery sharply to decline.For overcoming these defects, what research was more at present is carry out the change in volume of elimination Si in doff lithium process partly by the method at the coated one deck carbon of Si particle surface.This method only can promote the cycle performance of material to a certain extent, really can not solve that active material particle breaks, efflorescence, gradually from the problem that collector comes off.Nano material can effectively suppress breakage of particles, efflorescence, promotes cycle performance.Research shows, when silicon nano particle diameter reaches 10nm, even if through long-time circulation, particle also can not break, efflorescence.But current commercialization nano silica fume average grain diameter, substantially all at more than 50nm, therefore still occurs breaking, the phenomenon of efflorescence.
Summary of the invention
The present invention aim to provide a kind of nano silicon-based/preparation method of carbon composite, preparation silica-based/carbon composite is when for lithium ion battery negative material, the volume avoided in embedding lithium process sharply expands, thus do not occur Particle Breakage, efflorescence in circulating battery process, comes off.The present invention is realized by following scheme:
A preparation method for nano silicon-based/carbon composite, comprises the following steps:
(I) preparation of carbon-coated nano silicon: after organic resin is dissolved in organic solvent; be 1:(0.1 ~ 1 in resin and organic pore-forming agents mol ratio) ratio; add the pore creating material dissolving in organic solvent wherein; after pore creating material dissolves; be 1:(10 ~ 1 in the mass ratio of organic resin and silicon) ratio add nano silica fume wherein again; again through vacuumize after ultrasonic disperse,---high temperature cabonization under protective atmosphere condition---is pulverized, and high temperature cabonization can adopt the existing high temperature cabonization technique prepared in graphitic carbon negative electrode MATERIALS METHODS.It take nano Si as the band micropore hard carbon layer of core Surface coating one deck about 10 ~ 50 nanometer thickness that this step has obtained, the carbon-coated nano silicon in " pomegranate seed " feature.
(II) preparation of silicon-carbon compound precursor thing: after starch dispersion is formed suspension in water, add dried yeast powder, be 1:(0.1 ~ 1 in the mass ratio of starch and composite particles afterwards) ratio, the composite particles of the nano-silicon coated with carbon bed that the Ith step obtains is added, in 5 ~ 10 DEG C of vacuumizes after dispersed with stirring in starch suspension.
(III) predecessor carbonization: by silicon-carbon compound precursor thing obtained for the IIth step after room temperature leaves standstill certain hour, then DEG C heating in room temperature ~ 100, be incubated after 5-10 hour, then in protective atmosphere 800 ~ 1200 DEG C carry out high temperature cabonization.Material after carbonization, through pulverizing, obtains the silicon-carbon composite cathode material particle in " pomegranate type " architectural feature.
The preferred phenolic resins of organic resin in described Ith step or and Petropols.The preferred naphthalene of pore creating material, menthol or borneol.
Experiment finds, in described IIth step, is 1:(0.01 ~ 0.05 by the mass ratio of starch and dried yeast powder) add dried yeast powder, material property is better.
In order to reduce specific area and strengthen through the IIIth step obtain nano silicon-based/carbon composite particle between conductive capability, after described IIIth step, adopt the technique of existing liquid phase coating graphite, at Surface coating pitch or the glucose of nano silicon-based/carbon composite, after again through vacuum or spraying dry---high temperature cabonization.
Compared with the prior art, advantage applies of the present invention exists:
1. adopt method of the present invention to obtain the architectural feature of nano silicon-based/carbon composite particle in " pomegranate " type, when being applied to making lithium ion battery negative material, effectively can solve volume in embedding lithium process sharply to expand and Particle Breakage, efflorescence in cyclic process, the problem come off, the specific capacity of material is up to 450-950mAh/g, and cycle charge-discharge 500 weeks rear capability retentions are 85 ~ 92%.
2. in preparation technology of the present invention, utilize amylofermentation can produce the characteristic of micropore, the carbon-coated nano silicon of " pomegranate seed " feature is scattered in the carbon base body of band micropore, further for the release of silicon swelling stress provides cushion space, penetrating power and the electrical conductivity speed of electrolyte can be improved simultaneously, thus improve the cyclical stability of electrode material.
Embodiment
embodiment 1
A preparation method for nano silicon-based/carbon composite, prepares according to the following steps:
The preparation of (I) step carbon-coated nano silicon: after phenolic resins is dissolved in absolute ethyl alcohol, be the ratio of 1:1 in the mol ratio of resin and organic pore-forming agents naphthalene, adding naphthalene wherein, after naphthalene dissolves, is the ratio of 1:10 in the mass ratio of phenolic resins and silicon, add the nano silica fume that particle diameter D50 is 50nm wherein, ultrasonic disperse 60min, 200 DEG C of final vacuum dryings, under blanket of nitrogen condition, is incubated 360min with heating rate 10 DEG C/min to 800 DEG C, naturally cool to room temperature, then pulverize;
The preparation of (II) step silicon-carbon compound precursor thing: cornstarch is scattered in water after forming suspension, be that 1:0.05 adds dried yeast powder by the mass ratio of starch and dried yeast powder, be the ratio of 1:1 in the mass ratio of starch and composite particles afterwards, the composite particles of the nano-silicon coated with carbon bed that the Ith step obtains is added in starch suspension, stir 120min, by Granular composite, then in 5 DEG C of vacuumizes;
(III) step predecessor carbonization: by silicon-carbon compound precursor thing obtained for the IIth step in 30 DEG C of standing 300min, then after 90 DEG C of heating, then in blanket of nitrogen 1200 DEG C carry out high temperature cabonization, carbonization time is 360min.Material after carbonization is through pulverizing, and the obtained silicon-carbon composite cathode material particle in " pomegranate type " architectural feature, the Task-size Controlling of particle is at 3 ~ 5 μm.
After (IV) step liquid phase is coated on described IIIth step again, at the coated pitch of surperficial liquid phase method of nano silicon-based/carbon composite, after again through vacuum or spraying dry---high temperature cabonization.Obtain nano silicon-based/carbon composite.
Obtained nano silicon-based/carbon composite is used for lithium ion battery negative, specific capacity is about 950mAh/g, and cycle charge-discharge 500 weeks afterwards capability retention is 85 ~ 92%; Contrastingly, adopt elementary silicon as lithium-ion negative pole, although specific capacity 1200mAh/g, at 500 weeks circulation volume conservation rates 23%; Adopt existing nucleocapsid structure Si-C composite material as negative pole, specific capacity 550mAh/g, 500 weeks circulation volume conservation rates 72%.Material prepared by the inventive method is more excellent in the combination property of specific capacity and 500 weeks circulation volume conservation rates.
As stated above obtained nano silicon-based/carbon composite is made into lithium ion battery negative, battery is after 100 weeks charge and discharge cycles, adopt scanning electron microscope sem to observe electrode slice surface topography, result shows that obvious crackle does not appear in electrode surface, powder of detached phenomenon.
embodiment 2
Method substantially the same manner as Example 1 and step, but have following difference:
1. in the Ith step, the mol ratio of resin and organic pore-forming agents naphthalene is 1:0.1, the mass ratio of phenolic resins and silicon is the ratio of 1:1, the particle diameter D50 of nano silica fume is 10nm, ultrasonic disperse 60min is 200 DEG C of final vacuum dryings, under blanket of nitrogen condition, with heating rate 10 DEG C/min to 800 DEG C of insulation 10 hours.
2. in the IIth step, the mass ratio of starch and dried yeast powder is 1:0.01, and the mass ratio of starch and composite particles is 1:0.1.
3. do not need the IVth step.
Claims (6)
1. a preparation method for nano silicon-based/carbon composite, is characterized in that: comprise the following steps,
(I) preparation of carbon-coated nano silicon: after organic resin is dissolved in organic solvent, be 1:(0.1 ~ 1 in resin and organic pore-forming agents mol ratio) ratio, add the pore creating material dissolving in organic solvent wherein, after pore creating material dissolves, be 1:(10 ~ 1 in the mass ratio of organic resin and silicon) ratio add nano silica fume wherein again, again through vacuumize after ultrasonic disperse,---high temperature cabonization under protective atmosphere condition---is pulverized;
(II) preparation of silicon-carbon compound precursor thing: after starch dispersion is formed suspension in water, add dried yeast powder, be 1:(0.1 ~ 1 in the mass ratio of starch and composite particles afterwards) ratio, the composite particles of the nano-silicon coated with carbon bed that the Ith step obtains is added in starch suspension, dispersed with stirring, in 5 ~ 10 DEG C of vacuumizes;
(III) predecessor carbonization: by silicon-carbon compound precursor thing obtained for the IIth step after room temperature leaves standstill certain hour, then DEG C heating in room temperature ~ 100, be incubated after 5-10 hour, then in protective atmosphere 800 ~ 1200 DEG C carry out high temperature cabonization, finally pulverize.
2. the preparation method of nano silicon-based/carbon composite as claimed in claim 1, is characterized in that: the preferred phenolic resins of organic resin in described Ith step or and Petropols.
3. the preparation method of nano silicon-based/carbon composite as claimed in claim 1, is characterized in that: the preferred naphthalene of pore creating material, menthol, borneol in described Ith step.
4. as described in one of claims 1 to 3 nano silicon-based/preparation method of carbon composite, it is characterized in that: in described IIth step, is 1:(0.01 ~ 0.05 by the mass ratio of starch and dried yeast powder) add dried yeast powder.
5. as described in one of claims 1 to 3 nano silicon-based/carbon composite preparation method, it is characterized in that: after described IIIth step, again through vacuum or spraying dry---high temperature cabonization after the surface of nano silicon-based/carbon composite adopts the coated pitch of liquid phase method or glucose.
6. nano silicon-based/carbon composite preparation method as claimed in claim 4, it is characterized in that: after described IIIth step, again through vacuum or spraying dry---high temperature cabonization after the surface of nano silicon-based/carbon composite adopts the coated pitch of liquid phase method or glucose.
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Cited By (12)
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| CN105633380A (en) * | 2016-03-04 | 2016-06-01 | 中国科学院新疆理化技术研究所 | Preparation method for starch-based porous hard carbon negative electrode material of lithium ion battery |
| CN105932320A (en) * | 2016-05-18 | 2016-09-07 | 河南田园新能源科技有限公司 | Method for preparing composite cathode material by modification of graphite |
| CN106410164A (en) * | 2016-11-24 | 2017-02-15 | 盐城工学院 | High-performance composite material and preparation method and application thereof |
| CN106784707A (en) * | 2016-12-28 | 2017-05-31 | 江西正拓新能源科技股份有限公司 | A kind of preparation method of nano-silicone wire/carbon composite lithium ion battery cathode material |
| CN106898756A (en) * | 2017-04-24 | 2017-06-27 | 广东烛光新能源科技有限公司 | A kind of silicon-carbon cathode material and preparation method thereof |
| CN107170962A (en) * | 2017-04-17 | 2017-09-15 | 厦门高容新能源科技有限公司 | A kind of lithium ion battery silicium cathode electrode slice and preparation method thereof |
| CN107204431A (en) * | 2016-03-16 | 2017-09-26 | 比亚迪股份有限公司 | A kind of lithium ion battery anode active material and preparation method thereof, negative pole and battery comprising the negative active core-shell material |
| CN108565431A (en) * | 2018-04-24 | 2018-09-21 | 中国矿业大学 | A method of preparing lithium ion battery silicon-carbon compound cathode materials by carbon source of konjaku flour |
| CN108701809A (en) * | 2016-02-17 | 2018-10-23 | 瓦克化学股份公司 | The method for preparing Si/C composite particles |
| CN111540896A (en) * | 2020-05-07 | 2020-08-14 | 七台河万锂泰电材有限公司 | Preparation method of silicon-carbon composite negative electrode material |
| CN112736237A (en) * | 2021-01-19 | 2021-04-30 | 贵州大学 | Preparation method of green low-cost silicon-carbon anode material with three-dimensional porous structure |
| CN114142005A (en) * | 2021-11-09 | 2022-03-04 | 广东凯金新能源科技股份有限公司 | Long-circulation low-expansion inner hole structure silicon-carbon composite material, and preparation method and application thereof |
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Cited By (20)
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| CN108701809B (en) * | 2016-02-17 | 2021-11-09 | 瓦克化学股份公司 | Method for producing Si/C composite particles |
| US11063249B2 (en) | 2016-02-17 | 2021-07-13 | Wacker Chemie Ag | Method for producing Si/C composite particles |
| CN108701809A (en) * | 2016-02-17 | 2018-10-23 | 瓦克化学股份公司 | The method for preparing Si/C composite particles |
| CN105633380A (en) * | 2016-03-04 | 2016-06-01 | 中国科学院新疆理化技术研究所 | Preparation method for starch-based porous hard carbon negative electrode material of lithium ion battery |
| CN107204431B (en) * | 2016-03-16 | 2020-02-21 | 比亚迪股份有限公司 | Lithium ion battery negative electrode active material, preparation method thereof, negative electrode containing negative electrode active material and battery |
| CN107204431A (en) * | 2016-03-16 | 2017-09-26 | 比亚迪股份有限公司 | A kind of lithium ion battery anode active material and preparation method thereof, negative pole and battery comprising the negative active core-shell material |
| CN105932320A (en) * | 2016-05-18 | 2016-09-07 | 河南田园新能源科技有限公司 | Method for preparing composite cathode material by modification of graphite |
| CN106410164B (en) * | 2016-11-24 | 2019-02-12 | 盐城工学院 | A kind of anode material and its preparation method and application |
| CN106410164A (en) * | 2016-11-24 | 2017-02-15 | 盐城工学院 | High-performance composite material and preparation method and application thereof |
| CN106784707B (en) * | 2016-12-28 | 2019-06-04 | 江西正拓新能源科技股份有限公司 | A kind of preparation method of nano-silicon-carbon composition lithium ion battery cathode material |
| CN106784707A (en) * | 2016-12-28 | 2017-05-31 | 江西正拓新能源科技股份有限公司 | A kind of preparation method of nano-silicone wire/carbon composite lithium ion battery cathode material |
| CN107170962A (en) * | 2017-04-17 | 2017-09-15 | 厦门高容新能源科技有限公司 | A kind of lithium ion battery silicium cathode electrode slice and preparation method thereof |
| CN106898756B (en) * | 2017-04-24 | 2020-02-14 | 广东烛光新能源科技有限公司 | Silicon-carbon negative electrode material and preparation method thereof |
| CN106898756A (en) * | 2017-04-24 | 2017-06-27 | 广东烛光新能源科技有限公司 | A kind of silicon-carbon cathode material and preparation method thereof |
| CN108565431A (en) * | 2018-04-24 | 2018-09-21 | 中国矿业大学 | A method of preparing lithium ion battery silicon-carbon compound cathode materials by carbon source of konjaku flour |
| CN108565431B (en) * | 2018-04-24 | 2021-08-20 | 中国矿业大学 | Method for preparing silicon-carbon composite negative electrode material of lithium ion battery by taking konjac flour as carbon source |
| CN111540896A (en) * | 2020-05-07 | 2020-08-14 | 七台河万锂泰电材有限公司 | Preparation method of silicon-carbon composite negative electrode material |
| CN112736237A (en) * | 2021-01-19 | 2021-04-30 | 贵州大学 | Preparation method of green low-cost silicon-carbon anode material with three-dimensional porous structure |
| CN112736237B (en) * | 2021-01-19 | 2023-05-02 | 贵州大学 | Preparation method of green low-cost silicon-carbon anode material with three-dimensional porous structure |
| CN114142005A (en) * | 2021-11-09 | 2022-03-04 | 广东凯金新能源科技股份有限公司 | Long-circulation low-expansion inner hole structure silicon-carbon composite material, and preparation method and application thereof |
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