CN105870496A - Podiform silicon @ amorphous carbon @ graphene nanoscroll composite material for lithium ion battery negative material - Google Patents
Podiform silicon @ amorphous carbon @ graphene nanoscroll composite material for lithium ion battery negative material Download PDFInfo
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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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- 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
- H01M4/13—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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- 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
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
- 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
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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 discloses a podiform silicon @ amorphous carbon @ graphene nanoscroll composite material for a lithium ion battery negative material. The podiform silicon @ amorphous carbon @ graphene nanoscroll composite material is prepared from the following steps: stirring and dispersing commercial silicon nano powder into absolute ethyl alcohol, adding a Tris-HCl buffer solution and dopamine in sequence, washing a product obtained after stirring with distilled water and ethanol, and drying in a vacuum drying oven so as to obtain silicon @ dopamine powder; adding the silicon @ dopamine powder into graphene suspension, adding hydrazine hydrate, heating so as to reduce graphene, subsequently transferring the mixed suspension into a liquid nitrogen environment for rapidly freezing, and performing vacuum freeze-drying so as to obtain silicon @ dopamine graphene nanoscroll columns; and performing annealing reduction on the freeze-dried silicon @ dopamine graphene nanoscroll columns a reductive atmosphere, thereby transforming dopamine into amorphous carbon. Due to the structure of the composite material disclosed by the invention, completeness of a podiform structure is maintained, the lithium storage capacity and the rate capability of the composite matieral are increased, and the circulation stability of the composite material is improved.
Description
Technical field
The present invention relates to a kind of pod-like silicon@amorphous charcoal@graphene nano for lithium ion battery negative material and roll up composite, belong to lithium ion battery negative material field.
Background technology
The fast development of portable electric appts, wearable device and electric automobile proposes the highest requirement to energy storage device.In numerous energy storage devices, lithium ion battery is little with its high-quality energy density, volume energy density, self discharge, memory-less effect, working range width and the advantage such as non-maintaining are favored by consumers in general.The lithium ion battery negative material of commercialization at present is based on graphite carbon negative material, but its specific capacity is only 372mAh/g, and its intercalation potential platform is close to lithium metal, easily occurs " Li dendrite " phenomenon to cause potential safety hazard during fast charging and discharging.Additionally the solvent compatibility of graphite is poor, glass is easily occurred to cause capacity attenuation in containing low-temperature electrolytes such as Allyl carbonaties, seriously limiting its extensive application in fields such as electric motor car energy-storage batteries, this also requires that scientific research personnel researches and develops the lithium ion battery negative material that performance is the most excellent.In alternative several negative materials, silicon rapidly becomes the study hotspot of lithium ion battery negative material of future generation with the theoretical specific capacity (4200mAh/g) of its superelevation, relatively low intercalation potential (below 0.5V) and abundant earth's crust reserves.But, the cyclical stability of silicon is excessively poor, and its specific capacity fails rapidly along with the increase of cycle-index, this 400% cubical expansivity mainly caused with its alloying in process of intercalation and ultralow electric conductivity (6.7 × 10-4S/cm) relevant.Serious volumetric expansion can produce bigger internal stress in process of intercalation, and then causes the broken of silicon grain and efflorescence, and then and current collector between lose electric transmission approach and lost efficacy so that the specific capacity of silicon declines rapidly.Ultralow electric conductivity then makes silicon electric charge transmission during embedding and removing be obstructed.Therefore, research and development high conductivity, the silicon based composite material of high volumetric expansion carrying capacity are the key point improving silicium cathode material electrochemical performance.
Preparing silicon/carbon composite is a kind of cyclical stability improving silicon and the effective measures reducing irreversible capacity.Compound by with Carbon Materials, on the one hand can be greatly improved the electric conductivity of silicon, reduce the interface transmission resistance in electrochemical reaction process, and on the other hand high elastic modulus and the mechanical strength of Carbon Materials can effectively suppress silicon volumetric expansion in process of intercalation.Additionally, charcoal clad also can effectively suppress the electrical contact loss during de-lithium between silicon alloy fragment and current collector, and then the irreversible capacity loss of suppression silicon improves the cyclical stability of silicon.At present, it has been reported that silicon/carbon composite mainly include silicon/carbon mixture, silicon/charcoal laminated composites, nucleocapsid structure type silicon/carbon composite and yolk-eggshell type silicon/charcoal nanostructured.In above-mentioned silicon/carbon composite, only yolk-eggshell type silicon/charcoal nanostructured can effectively buffer silicon volumetric expansion in charge and discharge process, but its charcoal protective layer is the most easily rupturable and needs in preparation process to use the dangerous chemical materials such as Fluohydric acid..In this context, research and development performance is the most excellent the egg yolk@eggshell type silicon/green of carbon composite, low cost preparation technology are still that a huge challenge.
Summary of the invention
It is an object of the invention to provide a kind of pod-like silicon@amorphous charcoal@graphene nano for lithium ion battery negative material and roll up composite.
A kind of pod-like silicon@amorphous charcoal@graphene nano for lithium ion battery negative material rolls up composite, it is characterised in that this composite is prepared by the following method and obtains:
A by commercialization silicon nano power body dispersed with stirring in dehydrated alcohol, then Tris-HCl(trishydroxymethylaminomethane it is sequentially added into) buffer solution and dopamine, stirring reaction 6～24 hours, products therefrom distilled water and washing with alcohol, is drying to obtain the silicon nano power body (named silicon@dopamine) of dopamine coating decoration in vacuum drying oven；
B adds described silicon@dopamine powder body in Graphene suspension, is subsequently adding hydrazine hydrate in 40～80oUnder the conditions of C, mixing suspension is transferred to quick freeze vacuum freeze-drying in liquid nitrogen environment forms silicon@dopamine@graphene nano volume column with reduced graphene by heating for 10～60 minutes subsequently；
C by after lyophilizing silicon@dopamine@graphene nano roll up column anneal in reducing atmosphere reduction make dopamine be changed into amorphous charcoal thus prepare silicon@amorphous charcoal@graphene nano roll up composite.
Described in step A, commercial silicon nano power body is 1:1 with the mass ratio of dopamine.
The pH of described Tris-HCl buffer solution is 8.5.
Silicon in the dopamine of silicon@described in step B is 20:1～80:1 with the mass ratio of the Graphene in described Graphene suspension.
Described hydrazine hydrate is 20:1～80:1 with the mass ratio of Graphene.
Described reducing atmosphere is H2/ Ar or H2/N2Atmosphere, wherein H2Percent by volume be 2～20%.
Described silicon@amorphous charcoal@graphene nano volume composite directly or can be mixed for lithium ion battery secondary battery cathode material with other negative materials.
Other negative materials described are graphite-based charcoal (native graphite, MCMB, Delanium etc.), hard charcoal (resin carbon, organic polymer pyrolytic carbon) or transition metal oxide (nickel, cobalt, the oxide of manganese or multi-element metal oxide).
Mixing suspension of the present invention needed to be placed in quick freeze in liquid nitrogen environment before lyophilizing and solidifies Graphene with nano-particle to avoid the segregation phenomena occurred in slow freeze-drying process.
The advantage of pod-like silicon@amorphous charcoal@graphene nano of the present invention volume composite:
(1) in silicon@amorphous charcoal nucleocapsid structure is uniformly wrapped in the passage of graphene nano volume.
(2) there is enough gaps between silicon@amorphous charcoal granule and can ensure silicon volumetric expansion in charging process.
(3) graphene nano volume outer layer and amorphous charcoal internal layer collectively constitute double layer of charcoal protection silicon active material and avoid the deposition repeatedly of SEI film in charge and discharge process.
(4) contour structures of tubular graphene alkene nanotube not only can be greatly improved the electric conductivity of composite but also the electrical contact that still prevents in charge and discharge process granule abjection after silica flour and cause was lost efficacy, and the service efficiency of silicon can be greatly improved.
(5) during composite of the present invention can effectively stop embedding lithium/de-lithium, the interfacial reaction layer of silicon face is formed, its rich in a large amount of holes also provide adequate space for the volumetric expansion of silicon, be conducive to keeping the integrity of pod-like structures, avoid the efflorescence of silicon in electrochemical reaction process, and then be effectively increased the lithium storage content of composite, high rate performance and cyclical stability.
Accompanying drawing explanation
The stereoscan photograph of 73.6wt% silicon@amorphous charcoal@graphene nano volume composite prepared by Fig. 1 present invention.
The transmission electron microscope photo of 73.6wt% silicon@amorphous charcoal@graphene nano volume composite prepared by Fig. 2 present invention.
The cyclic voltammetry curve of 73.6wt% silicon@amorphous charcoal@graphene nano volume composite prepared by Fig. 3 present invention.The number of turns of digitized representation cyclic voltammetry scan in figure, represents scanning the 1st, 2,3,4 circle the most respectively.
Front four charging and discharging curves of the 73.6wt% silicon@amorphous charcoal@graphene nano volume composite prepared by Fig. 4 present invention.
The high rate performance of the 73.6wt% silicon@amorphous charcoal@graphene nano volume composite prepared by Fig. 5 present invention.
The cyclical stability of the 73.6wt% silicon@amorphous charcoal@graphene nano volume composite prepared by Fig. 6 present invention.
Detailed description of the invention
Embodiment 1
Take 500mg commercialization silicon nano power body dispersed with stirring in dehydrated alcohol, stir speed (S.S.) is that 200-1000rpm is allowed to form homogeneous suspension, it is subsequently adding 25mL Tris-HCl(10mM, pH=8.5) buffer solution and 50mg dopamine, stirring reaction was filtered to remove remaining unreacted dopamine after 24 hours at ambient temperature, gained filtration product distilled water and ethanol cyclic washing are the silicon nano power body that dopamine is modified, named silicon@dopamine after being dried 24 hours in vacuum drying oven.Take 100mL Graphene suspension (0.05mg/mL), add 73.5 μ L hydrazine hydrates in 60oReduced graphene under the conditions of C, the time is 30 minutes, is subsequently adding silicon@dopamine 5mg prepared by above-mentioned steps, and above-mentioned mixing suspension is transferred to freezing in tubular plastic container after 10 minutes and is placed on vacuum freezing lyophilizing in freeze dryer by agitating heating；Silicon@dopamine@graphene nano after lyophilizing is rolled up column anneal in reducing atmosphere, temperature 700oC, annealing time is 2 hours, takes out composite and be silicon@amorphous charcoal@graphene nano volume composite after natural cooling.Thermogravimetric test test result shows, in this composite, the actual mass mark of silicon is 58.9%.
With N-Methyl pyrrolidone (NMP) solution as solvent, it is applied in copper foil current collector, 110 with acetylene black conductor, polyvinylidene fluoride (PVDF) 8:1:1 in mass ratio mixed grinding uniformly slurry by by obtained silicon@amorphous charcoal@graphene nano volume compositeoAfter being vacuum dried 12 hours under C, natural cooling takes out.With composite for test electrode, with lithium metal for electrode, with 1MLiPF6 as electrolyte, with ethylene carbonate/diethyl carbonate (EC:DEC, 1:1, v:v) for solvent, with Celgard2400 as barrier film, in argon glove box, it is assembled into button cell.Prepared composite is at 0.01-1.6V blanking voltage window, and under 400mA/g electric current density, it discharges first and charging capacity is respectively 2736mAh/g and 1940mAh/g, and corresponding coulombic efficiency is 70.9%.After 3 Reversible Cycle, coulombic efficiency reaches more than 98.1%.High rate performance test result shows, this composite is under the electric current density of 3000mA/g, and its charging capacity, up to 839.7mAh/g, has good high rate performance.After lower 110 loop tests of electric current density of 2000mA/g, specific capacity is up to 972.6mAh/g, and specific capacity conservation rate is 92.1%.
Embodiment 2
Take 100mL Graphene suspension (0.05mg/mL), add 73.5 μ L hydrazine hydrates in 60oReduced graphene under the conditions of C, the time is 30 minutes, is subsequently adding in embodiment 1 the silicon@dopamine powder body 10mg of preparation, and above-mentioned mixing suspension is transferred to freezing in tubular plastic container after 10 minutes and is placed on vacuum freezing lyophilizing in freeze dryer by agitating heating；Silicon@dopamine@graphene nano after lyophilizing is rolled up column anneal in reducing atmosphere, temperature 700oC, annealing time 2 hours, takes out composite and is silicon@amorphous charcoal@graphene nano volume composite after natural cooling.Thermal gravimetric analysis results shows, the actual mass mark 73.6% of silicon in this composite.
By electrode preparation method in embodiment 1, obtained silicon@amorphous charcoal@graphene nano volume composite is applied in copper foil current collector, 110 with acetylene black conductor, polyvinylidene fluoride (PVDF) 8:1:1 in mass ratio mixed grinding uniformly slurryoBe vacuum dried natural cooling after 12 hours under C to take out, use same procedure in embodiment 1 to be assembled into button cell and carry out electrochemical property test, test condition be voltage window be 0.01-1.6V, electric current density is 400mA/g-3000mA/g.Under 400mA/g electric current density, electric discharge first and the charging capacity of 73.6wt% silicon@amorphous charcoal@graphene nano volume composite are respectively 2996mAh/g and 2243mAh/g, and corresponding coulombic efficiency is 74.9%.After 3 Reversible Cycle, coulombic efficiency reaches more than 98.1%.High rate performance test result shows, this composite is under the electric current density of 3000mA/g, and its charging capacity, up to 947.8mAh/g, has good high rate performance.After lower 110 loop tests of electric current density of 2000mA/g, specific capacity is up to 1168.5mAh/g, and specific capacity conservation rate is 91.5%.
Claims (9)
1. the pod-like silicon amorphous charcoal graphene nano volume composite for lithium ion battery negative material, it is characterised in that this composite is prepared by the following method and obtains:
A by commercialization silicon nano power body dispersed with stirring in dehydrated alcohol, then Tris-HCl buffer solution and dopamine it are sequentially added into, stirring reaction 6～24 hours, products therefrom distilled water and washing with alcohol, in vacuum drying oven, it is drying to obtain the silicon nano power body of dopamine coating decoration, i.e. silicon@dopamine powder body；
B adds described silicon@dopamine powder body in Graphene suspension, is subsequently adding hydrazine hydrate in 40～80oUnder the conditions of C, mixing suspension is transferred to quick freeze vacuum freeze-drying in liquid nitrogen environment forms silicon@dopamine@graphene nano volume column with reduced graphene by heating for 10～60 minutes subsequently；
C by after lyophilizing silicon@dopamine@graphene nano roll up column anneal in reducing atmosphere reduction make dopamine be changed into amorphous charcoal thus prepare silicon@amorphous charcoal@graphene nano roll up composite.
2. composite as claimed in claim 1, it is characterised in that described in step A, commercial silicon nano power body is 1:1 with the mass ratio of dopamine.
3. composite as claimed in claim 1, it is characterised in that the pH of described Tris-HCl buffer solution is 8.5.
4. composite as claimed in claim 1, it is characterised in that the silicon in the dopamine of silicon@described in step B is 20:1～80:1 with the mass ratio of the Graphene in described Graphene suspension.
5. composite as claimed in claim 1, it is characterised in that described hydrazine hydrate is 20:1～80:1 with the mass ratio of Graphene.
6. composite as claimed in claim 1, it is characterised in that described reducing atmosphere is H2/ Ar or H2/N2Atmosphere, wherein H2Percent by volume be 2～20%.
7. composite as claimed in claim 1, it is characterised in that described silicon@amorphous charcoal@graphene nano volume composite directly or can be mixed for lithium ion battery secondary battery cathode material with other negative materials.
8. composite as claimed in claim 7, it is characterised in that other negative materials described are graphite-based charcoal, hard charcoal or transition metal oxide.
9. composite as claimed in claim 8, it is characterised in that other negative materials described are native graphite, MCMB, Delanium, resin carbon, organic polymer pyrolytic carbon or nickel, cobalt, the oxide of manganese or multi-element metal oxide.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107317000A (en) * | 2017-06-15 | 2017-11-03 | 中国科学院成都有机化学有限公司 | A kind of three-dimensional porous structure silicon/graphene composite negative pole and preparation method thereof |
| CN108400294A (en) * | 2018-01-31 | 2018-08-14 | 天津大学 | A kind of preparation method of the lithium ion battery silicium cathode of multilevel hierarchy |
| CN108417782A (en) * | 2017-02-09 | 2018-08-17 | 韩国地质资源研究院 | The method for manufacturing silico-carbo-graphene synthetic, the synthetic manufactured by the manufacturing method and the accumulator for applying the synthetic |
| CN110828809A (en) * | 2019-11-20 | 2020-02-21 | 厦门大学 | Silicon-carbon composite material in form of bubble coral and preparation method and application thereof |
| CN114005965A (en) * | 2020-07-28 | 2022-02-01 | 深圳格林德能源集团有限公司 | Graphene/carbon-coated silicon-based negative electrode and preparation method thereof |
| CN116200006A (en) * | 2023-05-04 | 2023-06-02 | 合肥工业大学 | High-heat-conductivity epoxy resin composite material and preparation method thereof |
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| CN104638253A (en) * | 2015-02-16 | 2015-05-20 | 佳木斯大学 | Preparation method of Si and C-RG core-shell composite material used as cathode of lithium ion battery |
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| CN104638253A (en) * | 2015-02-16 | 2015-05-20 | 佳木斯大学 | Preparation method of Si and C-RG core-shell composite material used as cathode of lithium ion battery |
Non-Patent Citations (1)
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108417782A (en) * | 2017-02-09 | 2018-08-17 | 韩国地质资源研究院 | The method for manufacturing silico-carbo-graphene synthetic, the synthetic manufactured by the manufacturing method and the accumulator for applying the synthetic |
| CN108417782B (en) * | 2017-02-09 | 2021-03-02 | 韩国地质资源研究院 | Method of making silicon-carbon-graphene compositions |
| US11362326B2 (en) | 2017-02-09 | 2022-06-14 | Korea Institute Of Geoscience And Mineral Resources | Method for preparing silicon-carbon-graphene composite, composite prepared according thereto, and secondary battery to which same is applied |
| CN107317000A (en) * | 2017-06-15 | 2017-11-03 | 中国科学院成都有机化学有限公司 | A kind of three-dimensional porous structure silicon/graphene composite negative pole and preparation method thereof |
| CN108400294A (en) * | 2018-01-31 | 2018-08-14 | 天津大学 | A kind of preparation method of the lithium ion battery silicium cathode of multilevel hierarchy |
| CN110828809A (en) * | 2019-11-20 | 2020-02-21 | 厦门大学 | Silicon-carbon composite material in form of bubble coral and preparation method and application thereof |
| CN114005965A (en) * | 2020-07-28 | 2022-02-01 | 深圳格林德能源集团有限公司 | Graphene/carbon-coated silicon-based negative electrode and preparation method thereof |
| CN116200006A (en) * | 2023-05-04 | 2023-06-02 | 合肥工业大学 | High-heat-conductivity epoxy resin composite material and preparation method thereof |
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Application publication date: 20160817 |