CN106887572A - A kind of antimony carbon composite and its preparation method and application - Google Patents
A kind of antimony carbon composite and its preparation method and application Download PDFInfo
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- CN106887572A CN106887572A CN201710136133.5A CN201710136133A CN106887572A CN 106887572 A CN106887572 A CN 106887572A CN 201710136133 A CN201710136133 A CN 201710136133A CN 106887572 A CN106887572 A CN 106887572A
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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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 a kind of antimony carbon composite and its preparation method and application, composite is by antimony oxide (Sb2O3) the rheology state mixture of predecessor and organic high molecular polymer is prepared by in-situ reducing and carbon coating in situ.Preparation method includes：Add water to be tuned into rheology state by replacing reaction dissolvent thermal synthesis antimony oxide predecessor, then after organic high molecular polymer is well mixed with antimony oxide predecessor, be prepared antimony/carbon composite after roasting under inert gas shielding.Preparation process is simple of the present invention, synthesis condition is relatively easy to control, and is adapted to industrialized production；Obtained antimony/carbon composite has specific capacity higher, and good efficiency for charge-discharge, cycle efficieny and high rate capability, are a kind of very promising lithium ion batteries and anode material of lithium-ion battery.
Description
Technical field
The invention belongs to energy storage material field, more particularly to a kind of antimony-carbon composite and its preparation method and application.
Background technology
With the sternness increasingly of energy problem, within half a century in past, rechargeable battery (also known as：Secondary cell) conduct
A kind of high-efficiency energy-storage device has obtained swift and violent development.In numerous secondary cell systems, lithium ion battery is with its work electricity
The concern of the extremely global field researcher of the advantages of pressing high, the small small, self discharge of pollution, long lifespan..As lithium ion and
Anode material of lithium-ion battery, antimony sill has theoretical specific capacity higher (660mAh g-1).As lithium ion battery negative material
Material, the lithiation potential platform of antimony steadily maintains 0.85V or so.Used as anode material of lithium-ion battery, the sodium potential of antimony is put down
Platform steadily maintains 0.52V or so.This lithiumation and sodium potential are very attractive for being applied to secondary cell.Simply
Antimony sill can occur very serious volumetric expansion during lithiumation and sodium so that the material easily efflorescence of antimony base electrode
And come off from conductive current collector, cause battery capacity reduction, cycle performance to deteriorate, so as to limit its commercialized development and answer
With.For the problem that antimony sill is present, most common method is by the compound simultaneously nanosizing of antimony simple substance and carbon.The conjunction of report at present
Mainly there are colloid chemistry synthetic method, template, method of electrostatic spinning etc. into method, but the shortcoming one of these methods is preparation process
It is loaded down with trivial details, and multiplex some expensive raw material, preparation cost is increased, be not suitable for industrialized production；Two is these cumbersome sides
Method increased the difficulty of control reaction condition, reduce purity, performance and the production efficiency of product.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of antimony-carbon composite and its preparation method and application, system
Standby process is simple, synthesis condition is relatively easy to control, and is adapted to industrialized production；Obtained antimony/carbon composite has specific volume higher
Amount, good efficiency for charge-discharge, cycle efficieny and high rate capability are a kind of very promising lithium ion battery and sodium from
Sub- cell negative electrode material.
The invention provides a kind of antimony-carbon composite, by antimony oxide Sb2O3Predecessor and organic polymer are polymerized
The rheology state mixture of thing is prepared by in-situ reducing and carbon coating in situ.
The antimony oxide predecessor is multi-pore micron spherical structure.
The invention provides a kind of preparation method of antimony-carbon composite, including：
(1) by trichloride antimony SbCl3It is dissolved in absolute ethyl alcohol and obtains trichloride antimony ethanol solution, adds NaOH molten
Liquid stirring obtains mixed solution；Then mixed solution is put into reactor and reacts 1-30h in 120-150 DEG C, be centrifuged, wash,
Dry, obtain final product antimony oxide predecessor；
(2) antimony oxide predecessor and organic high molecular polymer are well mixed, add water to be tuned into rheology state, then
Roasting under an inert atmosphere obtains antimony-carbon composite；Wherein, sintering temperature is 300-600 DEG C, and roasting time is 30min-
20h。
The concentration of the trichloride antimony ethanol solution in the step (1) is 0.05-0.08molL-1。
The concentration of the sodium hydroxide solution in the step (1) is 1molL-1。
Trichloride antimony ethanol solution and the volume ratio of sodium hydroxide solution in the step (1) are 2:1.
The addition of the organic high molecular polymer in the step (2) is 50~5000g/mol Sb2O3。
Roasting heating rate in the step (2) is 5-20 DEG C per minute；Inert atmosphere is argon gas.
Organic high molecular polymer in the step (2) for the one kind in polyethylene glycol, p-phenylenediamine, polyvinyl alcohol or
It is several.
The invention provides a kind of application of antimony-carbon composite, the composite is applied to lithium ion battery and sodium
Ion battery cathode material.
The present invention provide technical scheme be：Composite is mixed by by antimony oxide predecessor and solid polyethylene glycol
Uniformly, suitable quantity of water is added to be tuned into rheology state, then roasting obtains lithium ion and anode material of lithium-ion battery under an inert atmosphere
Antimony-carbon composite.So-called rheology state refers to a kind of existence of the material with rheological property.In rheology state
It can not only include solid particle but also the material comprising liquid on physical composition that material is general, can flow or slowly flow
It is dynamic, a kind of complex system of even macroscopic；There is complicated composition or structure in chemistry；Solid is both shown on mechanics
Property shows the property of liquid again.
Beneficial effect
(1) present invention pre-reaction material is well mixed, obtain target product after an one-step baking in inert atmosphere；Side
Method is rheology phase local reduction way；Primary raw material major part abundance used, it is cheap；It is a kind of economical, clean, high
The green synthesis method of effect；
(2) present invention process is simple, and technological parameter is relatively easy to control, reproducible, has a good application prospect.
(3) polyethylene glycol of one of raw material is not only carbon source, and the carbon obtained by its decomposition in situ improves the electric conductivity of material,
And used as a kind of reducing agent in-situ reducing antimony oxide, the hydrogen that its decomposition in situ is produced and the generation that carbon is product antimony are carried
Strong reduction atmosphere is supplied；
(4) antimony-carbon composite prepared by the present invention has excellent as lithium ion and anode material of lithium-ion battery
Chemical property, carbon closely coats the porous spherical structure that metallic antimony forms uniqueness, and this structure is favorably improved antimony-carbon and is combined
The tap density of material simultaneously reduces Volume Changes of the electrode in charge and discharge process and the structure that causes collapses etc. to battery performance
Influence.
Brief description of the drawings
Fig. 1 is the XRD spectrum and the XRD spectrum of antimony-carbon composite of antimony oxide predecessor in embodiment 1；
Fig. 2 is that the SEM of antimony oxide predecessor in embodiment 1 schemes (a, b are different amplification) and by after calcining
The SEM figures (c, d are different amplification) of the antimony/carbon composite for obtaining；
Fig. 3 be embodiment 1 in antimony/carbon composite as lithium ion battery negative material in 0.1mVs-lObtained when sweeping speed
The cyclic voltammogram for obtaining；
Fig. 4 be embodiment 1 in antimony-carbon composite as lithium ion battery negative material current density be 100mA
g-1When, the charge/discharge capacity voltage curve of first five circle circulation.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
(1) trichloride antimony is first dissolved in absolute ethyl alcohol, and after magnetic agitation 3min so that solution is in colourless uniform
Liquid, concentration is 0.05mol/L.
(2) 1mol/L sodium hydroxide solutions and continuing magnetic force stirring 1h will be added dropwise in solution obtained above, be obtained
Mixed solution.
(3) the homogeneous mixed solution of above-mentioned formation is poured onto in the polytetrafluoroethyllining lining of 60mL, by liner reactor
It is sealed in stainless steel autoclave, is put into baking oven and is heated to 120 DEG C, then keeps constant temperature 24h.
(4) after question response case naturally cools to ambient temperature, open liner reactor and be poured off supernatant liquor, to remaining white
A small amount of distilled water is added in color sediment, is centrifuged after stirring, then respectively washed 1-2 times successively with distilled water, absolute ethyl alcohol, centrifugation is completed
The product (i.e. antimony oxide predecessor) for obtaining is placed in vacuum drying chamber afterwards, 12h is dried under the conditions of 50 DEG C and is collected standby
With.
(5) by antimony oxide predecessor and polyethylene glycol, (addition is 100g/mol Sb2O3) well mixed, add water
Rheology state is tuned into, then roasting obtains antimony-carbon composite under an inert atmosphere；Wherein, sintering temperature is 300 DEG C, during roasting
Between be 2h, heating rate be 5 DEG C per minute, inert atmosphere is argon gas.
Embodiment 2
(1) trichloride antimony is first dissolved in absolute ethyl alcohol, and after magnetic agitation 3min so that solution is in colourless uniform
Liquid, concentration is 0.05mol/L.
(2) 1mol/L sodium hydroxide solutions and continuing magnetic force stirring 1h will be added dropwise in solution obtained above, be obtained
Mixed solution.
(3) the homogeneous mixed solution of above-mentioned formation is poured onto in the polytetrafluoroethyllining lining of 60mL, by liner reactor
It is sealed in stainless steel autoclave, is put into baking oven and is heated to 120 DEG C, then keeps constant temperature 24h.
(4) after question response case naturally cools to ambient temperature, open liner reactor and be poured off supernatant liquor, to remaining white
A small amount of distilled water is added in color sediment, is centrifuged after stirring, then respectively washed 1-2 times successively with distilled water, absolute ethyl alcohol, centrifugation is completed
The product (i.e. antimony oxide predecessor) for obtaining is placed in vacuum drying chamber afterwards, 12h is dried under the conditions of 50 DEG C and is collected standby
With.
(5) by antimony oxide predecessor and polyethylene glycol, (addition is 200g/mol Sb2O3) well mixed, add water
Rheology state is tuned into, then roasting obtains antimony-carbon composite under an inert atmosphere；Wherein, sintering temperature is 400 DEG C, during roasting
Between be 8h, heating rate be 10 DEG C per minute, inert atmosphere is argon gas.
Embodiment 3
(1) trichloride antimony is first dissolved in absolute ethyl alcohol, and after magnetic agitation 3min so that solution is in colourless uniform
Liquid, concentration is 0.05mol/L.
(2) 1mol/L sodium hydroxide solutions and continuing magnetic force stirring 1h will be added dropwise in solution obtained above, be obtained
Mixed solution.
(3) the homogeneous mixed solution of above-mentioned formation is poured onto in the polytetrafluoroethyllining lining of 60mL, by liner reactor
It is sealed in stainless steel autoclave, is put into baking oven and is heated to 120 DEG C, then keeps constant temperature 24h.
(4) after question response case naturally cools to ambient temperature, open liner reactor and be poured off supernatant liquor, to remaining white
A small amount of distilled water is added in color sediment, is centrifuged after stirring, then respectively washed 1-2 times successively with distilled water, absolute ethyl alcohol, centrifugation is completed
The product (i.e. antimony oxide predecessor) for obtaining is placed in vacuum drying chamber afterwards, 12h is dried under the conditions of 50 DEG C and is collected standby
With.
(5) by antimony oxide predecessor and polyethylene glycol, (addition is 300g/mol Sb2O3) well mixed, add water
Rheology state is tuned into, then roasting obtains antimony-carbon composite under an inert atmosphere；Wherein, sintering temperature is 600 DEG C, during roasting
Between be 10h, heating rate be 20 DEG C per minute, inert atmosphere is argon gas.
The institute of embodiment 1 is characterized using X-ray diffractometer (XRD), SEM (SEM), electrochemical workstation
The pattern of the antimony/carbon composite for preparing and the chemical property of structure and the electrode material as lithium ion, its result
It is as follows：
(1) XRD test results show：The XRD spectrum of antimony oxide predecessor, diffraction maximum can correspond to orthorhombic phase
Antimony oxide.The XRD spectrum of antimony-carbon composite, all of diffraction maximum can be demarcated as the antimony of hexagonal phase.(Fig. 1)
(2) SEM test results show：Result display antimony oxide predecessor has the spherical morphology of micro nano structure.
The SEM of high power shows that a micron ball, by many secondary nanometer bar constructions, there is substantial amounts of hole between rod and rod.By after roasting
Antimony-the carbon composite for obtaining keeps original pattern substantially.(Fig. 2)
(3) Electrochemical results show：Spherical antimony-the carbon composite of multi-pore micron is used as lithium ion battery negative material
Material, in 0.1mVs-lThe cyclic voltammogram (Fig. 3) obtained during speed is swept, a pair of electrochemical reduction oxidation peaks are occurred in that, this pair of peaks point
Not Dui Yingyu the electrochemical lithium metaplasia of antimony go lithiumation process into lithium antimony alloy and lithium antimony alloy.It is 100mA g in current density-1
When, charge-discharge test shows the cycle performance of its stabilization having, and discharge capacity can be stablized in 600mAh g-1More than.(Fig. 4)
Claims (10)
1. a kind of antimony-carbon composite, it is characterised in that：By antimony oxide Sb2O3Predecessor and organic high molecular polymer
Rheology state mixture is prepared by in-situ reducing and carbon coating in situ.
2. a kind of antimony-carbon composite according to claim 1, it is characterised in that：The antimony oxide predecessor is
Multi-pore micron spherical structure.
3. a kind of preparation method of antimony-carbon composite, including：
(1) by trichloride antimony SbCl3It is dissolved in absolute ethyl alcohol and obtains trichloride antimony ethanol solution, adds sodium hydroxide solution to stir
Mix and obtain mixed solution；Then mixed solution is put into reactor and reacts 1-30h in 120-150 DEG C, be centrifuged, wash, dry,
Obtain final product antimony oxide predecessor；
(2) antimony oxide predecessor and organic high molecular polymer are well mixed, add water to be tuned into rheology state, then lazy
Property atmosphere under roasting obtain antimony-carbon composite；Wherein, sintering temperature is 300-600 DEG C, and roasting time is 30min-20h.
4. the preparation method of a kind of antimony-carbon composite according to claim 3, it is characterised in that：In the step (1)
Trichloride antimony ethanol solution concentration be 0.05-0.08molL-1。
5. the preparation method of a kind of antimony-carbon composite according to claim 3, it is characterised in that：In the step (1)
Sodium hydroxide solution concentration be 1molL-1。
6. the preparation method of a kind of antimony-carbon composite according to claim 3, it is characterised in that：In the step (1)
The volume ratio of trichloride antimony ethanol solution and sodium hydroxide solution be 2:1.
7. the preparation method of a kind of antimony-carbon composite according to claim 3, it is characterised in that：In the step (2)
Organic high molecular polymer addition be 50~5000g/mol Sb2O3。
8. the preparation method of a kind of antimony-carbon composite according to claim 3, it is characterised in that：In the step (2)
Roasting heating rate be 5-20 DEG C per minute；Inert atmosphere is argon gas.
9. the preparation method of a kind of antimony-carbon composite according to claim 3, it is characterised in that：In the step (2)
Organic high molecular polymer be one or more in polyethylene glycol, p-phenylenediamine, polyvinyl alcohol.
10. a kind of application of antimony-carbon composite as claimed in claim 1, it is characterised in that：The composite is applied to
Lithium ion battery and anode material of lithium-ion battery.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108878820A (en) * | 2018-06-19 | 2018-11-23 | 上海师范大学 | A kind of sodium-ion battery antimony carbon negative pole material and its preparation, application method |
| CN108899504A (en) * | 2018-06-29 | 2018-11-27 | 东华大学 | A kind of antimony-carbon nanotube-carbon composite, preparation method and application |
| CN109494368A (en) * | 2018-12-04 | 2019-03-19 | 中北大学 | A kind of preparation method and applications of carbonaceous nanocomposite |
| CN112886014A (en) * | 2021-01-29 | 2021-06-01 | 南方科技大学 | Hollow core-shell type antimony-carbon composite negative electrode material, preparation method thereof and secondary battery |
| CN113059174A (en) * | 2021-04-30 | 2021-07-02 | 信阳师范学院 | Preparation method of two-dimensional metal antimony nanosheet |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108878820A (en) * | 2018-06-19 | 2018-11-23 | 上海师范大学 | A kind of sodium-ion battery antimony carbon negative pole material and its preparation, application method |
| CN108899504A (en) * | 2018-06-29 | 2018-11-27 | 东华大学 | A kind of antimony-carbon nanotube-carbon composite, preparation method and application |
| CN108899504B (en) * | 2018-06-29 | 2021-03-16 | 东华大学 | Antimony-carbon nanotube-carbon composite material, preparation method and application |
| CN109494368A (en) * | 2018-12-04 | 2019-03-19 | 中北大学 | A kind of preparation method and applications of carbonaceous nanocomposite |
| CN112886014A (en) * | 2021-01-29 | 2021-06-01 | 南方科技大学 | Hollow core-shell type antimony-carbon composite negative electrode material, preparation method thereof and secondary battery |
| WO2022160671A1 (en) * | 2021-01-29 | 2022-08-04 | 南方科技大学 | Hollow core-shell type antimony-carbon composite negative electrode material, preparation method therefor and secondary battery |
| CN113059174A (en) * | 2021-04-30 | 2021-07-02 | 信阳师范学院 | Preparation method of two-dimensional metal antimony nanosheet |
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Application publication date: 20170623 |