CN107293708A - The improved method that solvent-thermal method prepares graphene silicon composite - Google Patents
The improved method that solvent-thermal method prepares graphene silicon composite Download PDFInfo
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- CN107293708A CN107293708A CN201710350287.4A CN201710350287A CN107293708A CN 107293708 A CN107293708 A CN 107293708A CN 201710350287 A CN201710350287 A CN 201710350287A CN 107293708 A CN107293708 A CN 107293708A
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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
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M4/62—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
- 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 present invention relates to technical field of lithium ion battery negative, the improved method that a kind of solvent-thermal method prepares graphene silicon composite is particularly disclosed.The improved method that the solvent-thermal method prepares graphene silicon composite, it is characterized in that：Graphene oxide is distributed in deionized water or ethanol equal solvent, silica flour is added, disperseed, solvent thermal reaction is carried out, reaction product is dried, grind, sieved；Pitch is distributed in tetrahydrofuran, product is added and disperses, add graphite, disperse, stirring and drying tetrahydrofuran；Product is calcined, dry, grind, sieved, then deposited carbon, obtain product；Or, by the first deposited carbon of reaction product, redisperse, graphite is added, disperseed, calcining obtains product.The present invention has the advantages of simple to operate, easy realization, good repetitiveness, easy industrialization.
Description
（One）Technical field
The present invention relates to technical field of lithium ion battery negative, more particularly to a kind of solvent-thermal method prepares graphene silicon and is combined
The improved method of material.
（Two）Background technology
As lithium ion battery is in the application in electrokinetic cell, energy-storage battery field, its energy density and cycle life to battery
Higher requirement is proposed, and the key factor of battery performance is electrode material, so research and development new electrode materials turn into focus.
The theoretical specific capacity of the most frequently used graphite negative electrodes of lithium ion battery is 372mAh/g, and theoretical specific capacity maximum
Negative material silicon is 4200mAh/g, is more than 10 times of graphite negative electrodes material.Although the theoretical capacity of silicon is high, its shortcoming
It is also obvious that due to the embedded abjection of lithium ion in charge and discharge process, Volume Changes are larger, powder phenomenon-tion easily occur, hold
Amount decay is very fast.
Graphene is combined with silicon using the method for solvent heat, using graphene coated silica flour, the volume of limitation silica flour becomes
Change, alleviate silica flour efflorescence, but when material is when with larger circulation, decay still more apparent.
（Three）The content of the invention
The present invention in order to make up the deficiencies in the prior art there is provided a kind of simple to operate, product favorable reproducibility, easy industrialization it is molten
The improved method that the hot method of agent prepares graphene silicon composite.
The present invention is achieved through the following technical solutions：
The improved method that a kind of solvent-thermal method prepares graphene silicon composite, comprises the following steps：
（1）Graphene oxide is distributed in deionized water or ethanol equal solvent, silica flour is added, disperseed, solvent thermal reaction is carried out,
Reaction product is dried, grind, sieved；
（2）Pitch is distributed in tetrahydrofuran, step is added（1）Product, disperse, add graphite, disperse, stirring and drying
Tetrahydrofuran；
（3）By step（2）Product calcining；
（4）By step（3）Product drying, grinding, sieving, then deposited carbon obtains product；
Or, step（2）In, by step（1）The first deposited carbon of reaction product, redisperse, add graphite, disperse, stirring is dried
Dry tetrahydrofuran, most afterwards through step（3）Obtain product.
The present invention forms uniform agraphitic carbon clad by Carbon deposition in silicon powder surface, and graphene, silica flour is close
Parcel；The agraphitic carbon clad can control the embedding lithium depth of silicon to a certain extent, and auxiliary graphene limits the body of silica flour
Product expansion, reduces silica flour structural damage degree, delays silica flour efflorescence, strengthens the stability of Si-C composite material, improves material
Big circulation performance.
The present invention more excellent technical scheme be：
The method of the deposition carbon is gas-phase carbon sedimentation, and its carbon source is methane or acetylene gas.
The method of the deposition carbon is liquid-phase C sedimentation, and carbon source is kerosene.
The temperature of the deposition carbon is 800-1400 DEG C, and the time is 0.5-8h.
The present invention has the advantages of simple to operate, easy realization, good repetitiveness, easy industrialization.
（Four）Brief description of the drawings
The present invention is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is the scanning electron microscope (SEM) photograph of product of the present invention；
Fig. 2 is the IC cycle performance contrast schematic diagrams for the material that embodiment 1 is prepared with comparative example.
（Five）Embodiment
Embodiment 1：
0.500g graphene oxides are weighed, are distributed in 100mL deionized waters, magnetic agitation 1h；0.500g nano silica fumes are weighed,
It is added in the deionized water dispersion liquid of graphene oxide, continues magnetic agitation 1h；By the deionized water of graphene oxide, silica flour
Dispersion liquid is transferred in hydrothermal reaction kettle, and 12h is reacted at 150 DEG C；Hydro-thermal reaction product is taken out, 60 DEG C of drying, grinding, powder
Broken, 400 mesh sieves excessively, load porcelain boat, are warming up to 1200 DEG C of insulation 2h with 5 DEG C/min programming rate in tube furnace, heat up
Lead to argon gas in journey, lead to acetylene in insulating process, after the completion of flow is 100sccm, deposition, 400 mesh sieves are crossed in grinding；Weigh
0.625g coal tar pitchs, are scattered in 50mL tetrahydrofurans, magnetic agitation 1h, add the product of previous step, magnetic agitation
1h, adds 4.000g crystalline flake graphites, magnetic agitation 1h；Mixture is warming up to 80 DEG C, stirring is evaporated tetrahydrofuran；Will mixing
Thing is transferred in porcelain boat, and 1000 DEG C of insulation 3h, heating and insulating process are warming up to 5 DEG C/min programming rate in tube furnace
In lead to argon gas protection；After the completion of calcining, material is taken out, crushes, grind, cross 400 mesh sieves, produce.
Embodiment 2：
0.500g graphene oxides are weighed, are distributed in 100mL deionized waters, magnetic agitation 1h；0.500g nano silica fumes are weighed,
It is added in the deionized water dispersion liquid of graphene oxide, continues magnetic agitation 1h；By the deionized water of graphene oxide, silica flour
Dispersion liquid is transferred in hydrothermal reaction kettle, and 12h, lyophilized products are reacted at 150 DEG C；0.625g coal tar pitchs are weighed, are disperseed
In 50mL tetrahydrofurans, magnetic agitation 1h adds hydro-thermal reaction product, and magnetic agitation 1h adds 4.000g crystalline flake graphites, magnetic
Power stirs 1h, heats the mixture to 80 DEG C, stirring is evaporated tetrahydrofuran；Mixture is transferred in porcelain boat, in tube furnace
1000 DEG C of insulation 3h are warming up to 5 DEG C/min programming rate, argon gas protection are led in heating and insulating process, flow is
100sccm；After the completion of calcining, material is taken out, crushes, grind, cross 400 mesh sieves, porcelain boat is put into, with 5 DEG C/min in tube furnace
Heating rate be warming up to 1200 DEG C of insulation 2h, argon gas is led in temperature-rise period, acetylene is led in insulating process, flow is
100sccm；After the completion of Carbon deposition, material is taken out, crushes, grind, cross 400 mesh sieves, produce.
Embodiment 3：
0.500g graphene oxides are weighed, are distributed in 100mL deionized waters, magnetic agitation 1h；0.500g nano silica fumes are weighed,
It is added in the deionized water dispersion liquid of graphene oxide, continues magnetic agitation 1h；By the deionized water of graphene oxide, silica flour
Dispersion liquid is transferred in hydrothermal reaction kettle, and 12h is reacted at 150 DEG C；Hydro-thermal reaction product is taken out, 60 DEG C of drying, grinding, powder
Broken, 400 mesh sieves excessively, load porcelain boat, are warming up to 1200 DEG C of insulation 2h with 5 DEG C/min programming rate in tube furnace, heat up
Lead in journey in argon gas, insulating process and argon gas is passed through in kerosene, using argon gas as carrier gas, using kerosene as carbon source, flow is
After the completion of 100sccm, deposition, 400 mesh sieves are crossed in grinding；0.625g coal tar pitchs are weighed, are scattered in 50mL tetrahydrofurans,
Magnetic agitation 1h, adds the product of previous step, and magnetic agitation 1h adds 4.000g crystalline flake graphites, magnetic agitation 1h；Will be mixed
Compound is warming up to 80 DEG C, and stirring is evaporated tetrahydrofuran；Mixture is transferred in porcelain boat, with 5 DEG C/min liter in tube furnace
Warm speed is warming up to 1000 DEG C of insulation 3h, and argon gas protection is led in heating and insulating process；After the completion of calcining, material is taken out, crush,
Grind, cross 400 mesh sieves, produce.
Embodiment 4：
0.500g graphene oxides are weighed, are distributed in 100mL deionized waters, magnetic agitation 1h；0.500g nano silica fumes are weighed,
It is added in the deionized water dispersion liquid of graphene oxide, continues magnetic agitation 1h；By the deionized water of graphene oxide, silica flour
Dispersion liquid is transferred in hydrothermal reaction kettle, and 12h is reacted at 150 DEG C；Hydro-thermal reaction product is taken out, 60 DEG C of drying, grinding, powder
Broken, 400 mesh sieves excessively, load porcelain boat, are warming up to 1000 DEG C of insulation 2h with 5 DEG C/min programming rate in tube furnace, heat up
Lead to argon gas in journey, lead to acetylene in insulating process, after the completion of flow is 100sccm, deposition, 400 mesh sieves are crossed in grinding；Weigh
0.625g coal tar pitchs, are scattered in 50mL tetrahydrofurans, magnetic agitation 1h, add the product of previous step, magnetic agitation
1h, adds 4.000g crystalline flake graphites, magnetic agitation 1h；Mixture is warming up to 80 DEG C, stirring is evaporated tetrahydrofuran；Will mixing
Thing is transferred in porcelain boat, and 1000 DEG C of insulation 3h, heating and insulating process are warming up to 5 DEG C/min programming rate in tube furnace
In lead to argon gas protection；After the completion of calcining, material is taken out, crushes, grind, cross 400 mesh sieves, produce.
Embodiment 5：
0.500g graphene oxides are weighed, are distributed in 100mL deionized waters, magnetic agitation 1h；0.500g nano silica fumes are weighed,
It is added in the deionized water dispersion liquid of graphene oxide, continues magnetic agitation 1h；By the deionized water of graphene oxide, silica flour
Dispersion liquid is transferred in hydrothermal reaction kettle, and 12h is reacted at 150 DEG C；Hydro-thermal reaction product is taken out, 60 DEG C of drying, grinding, powder
Broken, 400 mesh sieves excessively, load porcelain boat, are warming up to 1200 DEG C of insulation 1h with 5 DEG C/min programming rate in tube furnace, heat up
Lead to argon gas in journey, lead to acetylene in insulating process, after the completion of flow is 100sccm, deposition, 400 mesh sieves are crossed in grinding；Weigh
0.625g coal tar pitchs, are scattered in 50mL tetrahydrofurans, magnetic agitation 1h, add the product of previous step, magnetic agitation
1h, adds 4.000g crystalline flake graphites, magnetic agitation 1h；Mixture is warming up to 80 DEG C, stirring is evaporated tetrahydrofuran；Will mixing
Thing is transferred in porcelain boat, and 1000 DEG C of insulation 3h, heating and insulating process are warming up to 5 DEG C/min programming rate in tube furnace
In lead to argon gas protection；After the completion of calcining, material is taken out, crushes, grind, cross 400 mesh sieves, produce.
Comparative example：
0.500g graphene oxides are weighed, are distributed in 100mL deionized waters, magnetic agitation 1h；0.500g nano silica fumes are weighed,
It is added in the deionized water dispersion liquid of graphene oxide, continues magnetic agitation 1h；By the deionized water of graphene oxide, silica flour
Dispersion liquid is transferred in hydrothermal reaction kettle, and 12h is reacted at 150 DEG C；Hydro-thermal reaction product is taken out, 60 DEG C of drying, grinding, powder
Broken, 400 mesh sieves excessively；0.625g coal tar pitchs are weighed, are scattered in 50mL tetrahydrofurans, magnetic agitation 1h adds hydro-thermal anti-
Product is answered, magnetic agitation 1h adds 4.000g crystalline flake graphites, magnetic agitation 1h；Mixture is warming up to 80 DEG C, stirring is evaporated
Tetrahydrofuran；Mixture is transferred in porcelain boat, 1000 DEG C of insulations are warming up to 5 DEG C/min programming rate in tube furnace
Lead to argon gas protection in 3h, heating and insulating process；After the completion of calcining, material is taken out, crushes, grind, cross 400 mesh sieves, produce.
Claims (4)
1. the improved method that a kind of solvent-thermal method prepares graphene silicon composite, it is characterized in that, comprise the following steps：（1）Will
Graphene oxide is distributed in deionized water or ethanol equal solvent, adds silica flour, is disperseed, and carries out solvent thermal reaction, and reaction is produced
Thing drying, grinding, sieving；（2）Pitch is distributed in tetrahydrofuran, step is added（1）Product, disperse, add graphite,
It is scattered, stirring and drying tetrahydrofuran；（3）By step（2）Product calcining；（4）By step（3）Product drying, grinding, mistake
Sieve, then deposited carbon, obtain product；Or, step（2）In, by step（1）The first deposited carbon of reaction product, redisperse plus
Enter graphite, disperse, stirring and drying tetrahydrofuran, most afterwards through step（3）Obtain product.
2. the improved method that solvent-thermal method according to claim 1 prepares graphene silicon composite, it is characterised in that：Institute
The method for stating deposition carbon is gas-phase carbon sedimentation, and its carbon source is methane or acetylene gas.
3. the improved method that solvent-thermal method according to claim 1 prepares graphene silicon composite, it is characterised in that：Institute
The method for stating deposition carbon is liquid-phase C sedimentation, and carbon source is kerosene.
4. the improved method that solvent-thermal method according to claim 1 prepares graphene silicon composite, it is characterised in that：Institute
The temperature for stating deposition carbon is 800-1400 DEG C, and the time is 0.5-8h.
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| CN201710350287.4A CN107293708A (en) | 2017-05-18 | 2017-05-18 | The improved method that solvent-thermal method prepares graphene silicon composite |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108258214A (en) * | 2018-01-08 | 2018-07-06 | 北京科技大学 | A kind of preparation method of lithium ion battery negative material silicon@graphene/carbons |
| CN108807924A (en) * | 2018-06-21 | 2018-11-13 | 梁汝腾 | A kind of lithium battery silicon composite and preparation method thereof |
| CN111082036A (en) * | 2019-12-31 | 2020-04-28 | 桑顿新能源科技有限公司 | Silicon-coated graphene oxide negative electrode slurry, preparation method thereof, lithium ion battery negative electrode and lithium ion battery |
| CN113555536A (en) * | 2021-06-04 | 2021-10-26 | 惠州锂威新能源科技有限公司 | Preparation method of negative electrode material, negative electrode material and application |
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| CN101153358A (en) * | 2006-09-28 | 2008-04-02 | 深圳市比克电池有限公司 | Method of producing silicon carbon negative pole material of lithium ion battery |
| CN101244814A (en) * | 2007-02-13 | 2008-08-20 | 深圳市比克电池有限公司 | Method for producing lithium cell silicon carbon negative pole material and produced silicon carbon negative pole material |
| CN102306757A (en) * | 2011-08-26 | 2012-01-04 | 上海交通大学 | Silicon graphene composite anode material of lithium ion battery and preparation method of silicon graphene composite anode material |
| CN103035890A (en) * | 2011-10-09 | 2013-04-10 | 海洋王照明科技股份有限公司 | Silicon and graphene composite electrode material and preparation method thereof |
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| CN101153358A (en) * | 2006-09-28 | 2008-04-02 | 深圳市比克电池有限公司 | Method of producing silicon carbon negative pole material of lithium ion battery |
| CN101244814A (en) * | 2007-02-13 | 2008-08-20 | 深圳市比克电池有限公司 | Method for producing lithium cell silicon carbon negative pole material and produced silicon carbon negative pole material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108258214A (en) * | 2018-01-08 | 2018-07-06 | 北京科技大学 | A kind of preparation method of lithium ion battery negative material silicon@graphene/carbons |
| CN108807924A (en) * | 2018-06-21 | 2018-11-13 | 梁汝腾 | A kind of lithium battery silicon composite and preparation method thereof |
| CN108807924B (en) * | 2018-06-21 | 2021-07-23 | 吉林中溢炭素科技有限公司 | Silicon composite material for lithium battery and preparation method thereof |
| CN111082036A (en) * | 2019-12-31 | 2020-04-28 | 桑顿新能源科技有限公司 | Silicon-coated graphene oxide negative electrode slurry, preparation method thereof, lithium ion battery negative electrode and lithium ion battery |
| CN111082036B (en) * | 2019-12-31 | 2021-01-12 | 桑顿新能源科技有限公司 | Silicon-coated graphene oxide negative electrode slurry, preparation method thereof, lithium ion battery negative electrode and lithium ion battery |
| CN113555536A (en) * | 2021-06-04 | 2021-10-26 | 惠州锂威新能源科技有限公司 | Preparation method of negative electrode material, negative electrode material and application |
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Application publication date: 20171024 |