CN108767223A - A kind of preparation method of micro-nano structure algaroth-carbon complex lithium ion battery negative material - Google Patents
A kind of preparation method of micro-nano structure algaroth-carbon complex lithium ion battery negative material Download PDFInfo
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- CN108767223A CN108767223A CN201810522057.6A CN201810522057A CN108767223A CN 108767223 A CN108767223 A CN 108767223A CN 201810522057 A CN201810522057 A CN 201810522057A CN 108767223 A CN108767223 A CN 108767223A
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- cmk
- ion battery
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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
- H01M4/58—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
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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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- 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 belongs to lithium ion battery material technical fields, and in particular to a kind of micro-nano structure Sb4O5Cl2The preparation method of-CMK-5 complex lithium ion battery cathode materials.Ordered mesopore carbon (CMK-5) is first weighed to be handled in concentrated nitric acid solution.Then the processed CMK-5 of concentrated nitric acid is washed respectively with deionized water and ethanol solution, centrifuge.Antimony chloride, deionized water and ethylene glycol solution are then sequentially added in CMK-5, continue to stir after mixing ultrasound, mixed solution is finally moved into reaction kettle, is placed at certain temperature and reacts the specific time, obtain Sb4O5Cl2- CMK-5 compounds.The method of the present invention is simple for process, and inexpensive, low energy consumption, favorable reproducibility, and the material being prepared has higher reversible specific capacity and good cyclical stability.
Description
Technical field
The invention belongs to lithium ion battery material technical fields, and in particular to a kind of micro-nano structure Sb4O5Cl2- CMK-5 is multiple
Close the preparation method of object lithium ion battery negative material.
Background technology
Environmental pollution caused by being consumed excessively due to fossil fuel so that people pay close attention to the development of renewable and clean energy resource
With use.Lithium ion battery is because it is high with energy density, have extended cycle life, the advantages such as environmental-friendly obtain on many fields
Application.In recent years, lithium ion battery mixed the use on dynamic formula automobile in electric vehicle and plug-in, had further pushed novel
The development of electrode material.However, commercialized graphite, as lithium ion battery negative material, theoretical capacity is relatively low（372 mA h
g-1）, high rate performance is poor and security performance is bad, it is difficult to meet the needs of people are growing.Therefore, high-performance is worked out
Novel cathode material for lithium ion battery is very necessary.
Antimony sill is based on alloy mechanism as energy storage lithium ion battery material, have theoretical capacity is high, safety it is good with
And the advantage that charge and discharge platform is moderate, it is considered as a kind of very promising electrode material.However, it is of good performance to obtain storage lithium
Antimony sill will usually use the means such as high-power magnetron sputtering, microwave synthesis, high-temperature calcination, cause that energy consumption is higher, condition
Harshness, preparation process is complicated, limits its practical application.In contrast, important branch of the algaroth as antimony sill is closed
Simple at method, excellent fireproof performance can reduce cost as lithium/sodium ion battery electrode material, improve safety
Energy.
Invention content
The purpose of the present invention is to provide a kind of micro-nano structure Sb4O5Cl2The preparation method of-CMK-5 compounds, and for the first time
As lithium ion battery negative material.This method is simple for process, and inexpensive, low energy consumption, and favorable reproducibility is had excellent performance.
To achieve the above object, the present invention adopts the following technical scheme that：
The micro-nano structure Sb4O5Cl2The preparation method of-CMK-5 compounds, specific steps include：It is orderly first to weigh 0.008 g
Mesoporous carbon (CMK-5) stirs 1 h in concentrated nitric acid solution at a temperature of 60 DEG C.Then deionized water and absolute ethyl alcohol are used
Solution washs the processed CMK-5 of concentrated nitric acid tri- times respectively, and is centrifuged.Then sequentially added in CMK-5
0.4500 g antimony chlorides, 5 mL deionized waters, 25 mL ethylene glycol solutions move to after mixing 30 min of ultrasound under magnetic stirring apparatus
Continue to stir 30 min, mixed solution is finally moved into 50 mL reaction kettles, is placed in 180 DEG C of baking ovens and reacts 24 h, obtain
Sb4O5Cl2- CMK-5 compounds.Lithium battery assembles：Sb in mass ratio4O5Cl2- CMK-5 compounds：Kynoar：Acetylene black
=60：30：It is equably coated on copper foil after 10 mixed grindings and does cathode, reference electrode and be lithium metal, electrolyte to electrode
By 1M LiPF6EC+DMC+EMC (v/v of EC/DMC/EMC=1/1/1) solution.All assemblings carry out in glove box.
The remarkable advantage of the present invention is：The method of the present invention is simple for process, and inexpensive, low energy consumption, favorable reproducibility, prepares
Obtained micro-nano structure Sb4O5Cl2- CMK-5 composite materials have higher reversible specific capacity and better cyclical stability.
Description of the drawings
Fig. 1 Sb4O5Cl2And Sb4O5Cl2The XRD diagram of-CMK-5；
Fig. 2 is pure Sb4O5Cl2The scanning electron microscope (SEM) photograph of sample and inventive samples；Wherein (a) figure is Sb4O5Cl2；(b) figure
For Sb4O5Cl2- CMK-5 compounds；
Fig. 3 a are in 800 mA g-1Sb under current density4O5Cl2- CMK-5 and Sb4O5Cl2Electrochemistry cycle performance figure；
Fig. 3 b Sb under different current densities4O5Cl2- CMK-5 and Sb4O5Cl2High rate performance figure.
Specific implementation mode
Further to disclose rather than the present invention is limited, the present invention is described in further detail below in conjunction with example.
Embodiment 1
The micro-nano structure Sb4O5Cl2The preparation method of-CMK-5 compounds, specific steps include：First weigh 0.008 g
CMK-5 stirs 1 h in concentrated nitric acid solution at a temperature of 60 DEG C.Then deionized water and ethanol solution is used to distinguish
It washs the processed CMK-5 of concentrated nitric acid tri- times, and is centrifuged.0.4500 g chlorinations are then sequentially added in CMK-5
Antimony, 5 mL deionized waters, 25 mL ethylene glycol solutions move under magnetic stirring apparatus after mixing ultrasound 30 min and continue stirring 30
Mixed solution is finally moved to the reaction kettle that 50 mL liners are polytetrafluoroethylene (PTFE), is placed in 180 DEG C of baking ovens and reacts 24 h by min,
Obtain Sb4O5Cl2- CMK-5 compounds.Lithium battery assembles：Sb in mass ratio4O5Cl2- CMK-5 compounds：Kynoar：Second
Acetylene black=60：30：It is equably coated on copper foil after 10 mixed grindings and does cathode, reference electrode and be lithium metal to electrode, electricity
Matter is solved by 1M LiPF6EC+DMC+EMC (v/v of EC/DMC/EMC=1/1/1) solution.It is all assembling in glove box into
Row.
The present invention passes through solvent structure micro-nano structure Sb4O5Cl2- CMK-5 composite materials, for the first time as lithium
Ion battery cathode, in 800 mAh g-1Current density under, micro-nano structure Sb4O5Cl2- CMK-5 compounds are in 100 circle of cycle
Afterwards, discharge capacity can be stably held in 406.6 mA h g-1.Under same current density, pure Sb4O5Cl2Electrode material follows
After ring to 100 circles, capacity has decayed to 90.5 mA h g-1.The result shows that this compound has higher reversible specific capacity
With better cyclical stability, main cause may be related with its micro-nano structure characteristic：The porosity of micro-nano structure material has
Conducive to Li+Diffusion in electrode interior improves the contact between electrolyte and electrode material, and CMK-5 is compound can both change
The electric conductivity of kind electrode, and stability of the material in charge and discharge process can be improved.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (3)
1. a kind of micro-nano structure algaroth-carbon complex Sb4O5Cl2The preparation method of-CMK-5 lithium ion battery negative materials,
It is characterized in that：Specific steps include：
（1）Ordered mesopore carbon CMK-5 stir process in the concentrated nitric acid solution of warm is first weighed, deionized water and anhydrous is then used
Ethanol solution washs the processed CMK-5 of concentrated nitric acid tri- times respectively, and is centrifuged；
（2）Antimony chloride, deionized water and ethylene glycol solution are then sequentially added into CMK-5, are moved to after 30 min of mixing ultrasound
Continue to stir 30 min under magnetic stirring apparatus, finally mixed solution is moved in the reaction kettle that liner is polytetrafluoroethylene (PTFE), be placed in
It is reacted in baking oven, obtains lithium ion battery negative material Sb4O5Cl2- CMK-5 compounds.
2. a kind of preparation method of micro-nano structure lithium ion battery negative material according to claim 1, it is characterised in that：
Step（1）Middle stir process is specially：1 h is stirred at a temperature of 60 DEG C.
3. a kind of preparation method of micro-nano structure lithium ion battery negative material according to claim 1, it is characterised in that：
Step（2）Reaction condition is in baking oven：24 h are reacted at 180 DEG C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63248724A (en) * | 1987-04-03 | 1988-10-17 | Mitsubishi Metal Corp | Production of fibrous antimony oxide |
| CN102386382A (en) * | 2011-11-03 | 2012-03-21 | 大连理工大学 | CMK-5 type mesoporous carbon-nano inorganic substance composite material, preparation method and application thereof |
| CN107162053A (en) * | 2017-06-12 | 2017-09-15 | 湘潭大学 | A kind of bar-shaped Sb of sub-micron4O5Cl2Simple hydrothermal preparing process |
| CN107275603A (en) * | 2017-06-09 | 2017-10-20 | 福州大学 | MoSe2The preparation of OMC compounds and its application in lithium ion battery |
-
2018
- 2018-05-28 CN CN201810522057.6A patent/CN108767223A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63248724A (en) * | 1987-04-03 | 1988-10-17 | Mitsubishi Metal Corp | Production of fibrous antimony oxide |
| CN102386382A (en) * | 2011-11-03 | 2012-03-21 | 大连理工大学 | CMK-5 type mesoporous carbon-nano inorganic substance composite material, preparation method and application thereof |
| CN107275603A (en) * | 2017-06-09 | 2017-10-20 | 福州大学 | MoSe2The preparation of OMC compounds and its application in lithium ion battery |
| CN107162053A (en) * | 2017-06-12 | 2017-09-15 | 湘潭大学 | A kind of bar-shaped Sb of sub-micron4O5Cl2Simple hydrothermal preparing process |
Non-Patent Citations (1)
| Title |
|---|
| XIANG YING CHEN等: ""Hydrothermal synthesis of antimony oxychloride and oxide nanocrystals: Sb4O5Cl2,Sb8O11Cl2, and Sb2O3"", 《JOURNAL OF SOLID STATE CHEMISTRY》 * |
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