CN106784699A - A kind of method for preparing the composite for adhering to tin oxide nano particles on honeycomb carbon - Google Patents
A kind of method for preparing the composite for adhering to tin oxide nano particles on honeycomb carbon Download PDFInfo
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- CN106784699A CN106784699A CN201611221274.9A CN201611221274A CN106784699A CN 106784699 A CN106784699 A CN 106784699A CN 201611221274 A CN201611221274 A CN 201611221274A CN 106784699 A CN106784699 A CN 106784699A
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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
- H01M4/366—Composites as layered products
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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 method for preparing the composite for adhering to tin oxide nano particles on honeycomb carbon;Magneton stirring is lower to prepare SnCl4·5H2O solution;Take honeycomb carbon and add SnCl4·5H2O solution, and carry out ultrasonically treated;The presoma mixed liquor that will be obtained is transferred to heating response in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner;It is washed out, dried process is made annealing treatment in argon gas atmosphere, obtains adhering on honeycomb carbon the composite of tin oxide nano particles.The material is by SnO2Nano-particle and honeycomb carbon are constituted, wherein SnO2Particle growth improves the electric conductivity of material and carries SnO in the aperture of honeycomb carbon2Volumetric expansion in electrochemical reaction process;Effectively improve SnO2As the chemical property of anode material of lithium-ion battery.
Description
Technical field
The invention belongs to inorganic nano material synthesis field.In particular it relates to by change experiment in reaction condition come
The method for preparing the composite for adhering to tin oxide nano particles on honeycomb carbon.
Background technology
With the extensive application of lithium ion battery, the demand to lithium is greatly increased, but lithium resource is limited, and distribution
Uneven (being mainly distributed on America area), this causes that Development of Novel energy-storage battery turns into Strategic Demand.Sodium ion and lithium ion
Physicochemical properties it is similar, and sodium resource reserve is abundant, and widely distributed, cheap, it is huge that this causes that sodium-ion battery has
Big potential turns into the strategy alternatives product of lithium ion battery and causes the concern of numerous researchers.
Because negative material most widely used in lithium ion battery does not possess storage sodium property, therefore to sodium-ion battery
The research of negative material is particularly significant.Wherein, SnO2Negative material and its composite are because have suitable operating voltage to put down
Platform, theoretical specific capacity high, low cost, it is pollution-free the advantages of cause extensive research.But due to transition metal oxide certainly
Body has poor electric conductivity so that SnO2It is infeasible directly as anode material of lithium-ion battery., Guoxiu in 2013
Wang etc. reports SnO first2@MWCNT composites can be used as anode material of lithium-ion battery.By with multi-walled carbon nano-tubes
It is combined, is substantially increased the electric conductivity of material, and is made SnO2It is provided with good storage sodium property.But, due to closing
The reason for aurification is reacted, SnO2There is huge volumetric expansion (about 400%) in it there is electrochemical reaction process so that living
Property material occur efflorescence and to come off, cause battery performance to decline.SnO2With the compound electricity that can effectively improve battery of carbon material
Chemical property, but for now, do not there is SnO2With the report of honeycomb carbon composite.We are closed by new preparation method
Adhere to the composite of tin oxide nano particles on into new honeycomb carbon, the material effectively improves SnO2As sodium
The chemical property of ion battery cathode material.
The content of the invention
The present invention has been synthesized using the method that hydro-thermal method and annealing are combined and adhere to stannic oxide nanometer on honeycomb carbon
The composite of particle, wherein SnO2On nano-particle and honeycomb carbon are combined closely, the presence of honeycomb carbon effectively carries SnO2
Volumetric expansion and increased the electric conductivity of material, substantially increase the chemical property of material.
The present invention is provided a kind of method being combined using hydro-thermal method and annealing and adhere to dioxy on honeycomb carbon to synthesize
The method for changing the composite of tin nanoparticles.Experiment is also synthesized by changing pre-reaction material concentration and adhere to two on honeycomb carbon
The composite of tin oxide nanoparticles.
Technical scheme is as follows:
A kind of method for preparing the composite for adhering to tin oxide nano particles on honeycomb carbon;Comprise the following steps that:
1) the lower SnCl for preparing 0.25-1.00mol/L of magnetons stirring4·5H2O solution;
2) takes honeycomb carbon and adds step 1) SnCl that obtains4·5H2O solution so that the concentration of honeycomb carbon is 5-7.5g/L,
And carry out ultrasonically treated;
3) is by step 2) the presoma mixed liquor that obtains is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner, and use
After stainless steel cauldron sealing, 170-190 DEG C is heated to, is incubated 12-36h;
4) after reactions terminate, normal temperature is cooled at room temperature, takes out reactant, washed using deionized water and ethanol respectively,
Treatment is dried, desciccate is obtained.
5) is by step 4) desciccate that obtains made annealing treatment in argon gas atmosphere, obtains adhering to two on honeycomb carbon
The composite of tin oxide nanoparticles.
The step 2) in the aperture prioritizing selection aperture size of honeycomb carbon be less than 5 μm.
The step 4) preferably drying condition be to dry 8-12h at 60-80 DEG C.
The step 4) wash preferred 3-5 times with deionized water and ethanol.
The step 5) annealing condition is preferably:In argon gas atmosphere, heating rate is 5-10 DEG C/min, in 600-
120-200min is incubated at 650 DEG C, room temperature is then naturally cooled to.
It is described to be with magneton stirring optimum condition:1-20r/s.
Adhere to dioxy on the method synthesis honeycomb carbon being combined the invention provides a kind of use hydro-thermal method and annealing
The method for changing the composite of tin nanoparticles.Specifically, by ultrasonic mixing honeycomb carbon and Sn4+Salt, in Hydrothermal Synthesiss process
In, the pore structure of honeycomb carbon is SnO2Nucleation provides active position, SnO2Nucleating growth is carried out at the honeycomb carbon pores footpath, from
And effectively improve the electric conductivity of material and carry SnO well2Volumetric expansion.
Effect of the invention is:The method being combined by hydro-thermal method and annealing, have been synthesized and adhere to two on honeycomb carbon
The composite of tin oxide nanoparticles.The material is by SnO2Nano-particle and honeycomb carbon are constituted, wherein SnO2Particle growth
In the aperture of honeycomb carbon, improve the electric conductivity of material and carry SnO2Volumetric expansion in electrochemical reaction process;
Effectively improve SnO2As the chemical property of anode material of lithium-ion battery.
Brief description of the drawings
Fig. 1 is the X-ray diffraction of the composite for adhering to tin oxide nano particles on honeycomb carbon prepared by embodiment 1
Figure, as seen from the figure, the X-ray diffractogram and SnO of products therefrom2The peak position of standard PDF cards (41-1445) fits like a glove, and says
The bright SnO for having synthesized pure phase2。
Adhere to the SEM figures of the composite of tin oxide nano particles, such as Fig. 2 on honeycomb carbon prepared by Fig. 2 embodiments 2
Shown in (a), the uniform pore diameter of honeycomb carbon in order, as shown in Fig. 2 (b), the aperture size of honeycomb carbon at 1-5 μm, such as Fig. 2 (c) institutes
Show, product is by honeycomb carbon and SnO2Nano particle is constituted, shown in such as Fig. 2 (d), SnO2Nanoparticle size be distributed in 10-20nm it
Between.SnO2Nano particle is grown on honeycomb carbon securely, and this can improve the electric conductivity of material and carry SnO2In discharge and recharge
Volumetric expansion in journey, so as to improve the chemical property of material.
Fig. 3 is to adhere to the composite of tin oxide nano particles on honeycomb carbon prepared by embodiment 3 as negative pole group
The electrochemical cycle stability performance map tested after battery is dressed up, as can be seen from Fig., battery is carried out under 50mA/g current densities
After constant current charge-discharge 10 is enclosed (first lap activation is disregarded), the specific capacity of battery does not almost decay, and the storehouse of discharge and recharge weekly
Human relations efficiency is close to 100%.Adhere to the composite of tin oxide nano particles as sodium-ion battery on this explanation honeycomb carbon
Negative material has good chemical property.
Specific embodiment
The method of the embodiment of the present invention, is described by preferred embodiment, and person skilled substantially can be not
Depart from and methods and techniques described herein route is modified or reconfigured in present invention, spirit and scope, come real
Now final technology of preparing.In particular, all similar replacements and change for a person skilled in the art
It is it will be apparent that they are considered as being included in spirit of the invention, scope and content.
1) prepares the SnCl of 0.25-1.00mol/L4·5H2O solution, during with magneton stirring (1-20r/s), obtain
To SnCl4·5H2O solution;
2) takes aperture size and is added to step 1 less than 5 μm of honeycomb carbon) SnCl that obtains4·5H2In O solution so that honeybee
The concentration of nest carbon is 5-7.5g/L, and is carried out ultrasonically treated;
3) be transferred to above-mentioned presoma mixed liquor in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner by, and anti-using stainless steel
After answering kettle to seal, 170-190 DEG C is heated to, is incubated 12-36h;
4) after reactions terminate, normal temperature is cooled at room temperature, takes out reactant, washed using deionized water and ethanol respectively
3-5 times, treatment is dried, obtains desciccate.
5) is by step 4) desciccate that obtains made annealing treatment;In argon gas atmosphere, heating rate be 5-10 DEG C/
Min, is incubated 120-200min at 600-650 DEG C, then naturally cools to room temperature, obtains adhering to titanium dioxide sijna on honeycomb carbon
The composite of rice grain.
Embodiment 1:
1) is by the SnCl of 0.025mol4·5H2O is added in 100mL deionized waters, and magneton is uniformly mixed;
2) takes 0.4g aperture sizes and is added to step 1 less than 5 μm of honeycomb carbon) the 80mL SnCl that obtain4·5H2O solution
In, and carry out ultrasonically treated;
3) takes the precursor solution that appropriate step 2 obtains and is transferred to the polytetrafluoroethylene (PTFE) hydrothermal reaction kettle that capacity is 100mL
In liner, stainless steel cauldron sealing is heated using baking oven, is heated to 170 DEG C, is incubated 36h;
4) after reactions terminate, normal temperature is cooled at room temperature, takes out reactant, wash 3 using deionized water and ethanol respectively
Secondary, 60 DEG C dry 12h, obtain desciccate;
5) step 4 is obtained desciccate and is made annealing treatment under an argon atmosphere by, and heating rate is set to 5 DEG C/min,
Room temperature is naturally cooled to after being incubated 200min at 600 DEG C, obtains adhering on honeycomb carbon the composite of tin oxide nano particles.
As shown in Figure 1, the X-ray diffractogram and SnO of products therefrom2The peak position of standard PDF cards (41-1445) is kissed completely
Close, illustrate to have synthesized the SnO of pure phase2.This method for showing to be combined by hydro-thermal method and annealing successfully synthesizes honeycomb
Adhere to the composite of tin oxide nano particles on carbon.
Embodiment 2:
1) is by the SnCl of 0.05mol4·5H2O is added in 100mL deionized waters, and magneton is uniformly mixed;
2) takes 0.5g aperture sizes and is added to step 1 less than 5 μm of honeycomb carbon) the 80mL SnCl that obtain4·5H2O solution
In, and carry out ultrasonically treated;
3) takes the precursor solution that appropriate step 2 obtains and is transferred to the polytetrafluoroethylene (PTFE) hydrothermal reaction kettle that capacity is 100mL
In liner, stainless steel cauldron sealing is heated using baking oven, is heated to 180 DEG C, is incubated 24h;
4) after reactions terminate, normal temperature is cooled at room temperature, takes out reactant, wash 4 using deionized water and ethanol respectively
Secondary, 70 DEG C dry 10h, obtain desciccate;
5) step 4 is obtained desciccate and is made annealing treatment under an argon atmosphere by, and heating rate is set to 8 DEG C/min,
Room temperature is naturally cooled to after being incubated 160min at 625 DEG C, obtains adhering on honeycomb carbon the composite of tin oxide nano particles.
As shown in Fig. 2 (a), in order, such as shown in Fig. 2 (b), the aperture size of honeycomb carbon is in 1-5 μ for the uniform pore diameter of honeycomb carbon
Shown in m, such as Fig. 2 (c), product is by honeycomb carbon and SnO2Nano particle is constituted, shown in such as Fig. 2 (d), SnO2Nanoparticle size point
Cloth is between 10-20nm.Honeycomb carbon and SnO2The successful combination of nano particle, will greatly improve the electric conductivity of material, honeycomb carbon
Hole can also effectively carry SnO2Volumetric expansion, so as to substantially improve SnO2As the electricity of anode material of lithium-ion battery
Chemical property.
Embodiment 3:
1) is by the SnCl of 0.1mol4·5H2O is added in 100mL deionized waters, and magneton is uniformly mixed;
2) takes 0.6g aperture sizes and is added to step 1 less than 5 μm of honeycomb carbon) the 80mL SnCl that obtain4·5H2O solution
In, and carry out ultrasonically treated;
3) takes the precursor solution that appropriate step 2 obtains and is transferred to the polytetrafluoroethylene (PTFE) hydrothermal reaction kettle that capacity is 100mL
In liner, stainless steel cauldron sealing is heated using baking oven, is heated to 190 DEG C, is incubated 12h;
4) after reactions terminate, normal temperature is cooled at room temperature, takes out reactant, wash 5 using deionized water and ethanol respectively
Secondary, 80 DEG C dry 8h, obtain desciccate;
5) step 4 is obtained desciccate and is made annealing treatment under an argon atmosphere by, and heating rate is set to 10 DEG C/min,
Room temperature is naturally cooled to after being incubated 120min at 650 DEG C, obtains adhering on honeycomb carbon the composite wood of tin oxide nano particles
Material.
As shown in figure 3, the composite for adhering to tin oxide nano particles on honeycomb carbon has good chemical property,
Its first week specific discharge capacity can be up to 559.5mAh g-1, after circulating 10 weeks, its specific capacity remains to stabilization in 110.4mAh g-1, illustrate that the presence of honeycomb carbon effectively improves SnO2As the chemical property of anode material of lithium-ion battery.
To sum up the accompanying drawing of embodiment can clearly be found out, by the present invention in that the side being combined with hydro-thermal method and annealing
Adhere to the composite of tin oxide nano particles on method synthesis honeycomb carbon, the material is by SnO2Nano-particle and honeycomb carbon group
Into wherein SnO2Nano-particle is equably grown in the hole of honeycomb carbon, and honeycomb carbon improves the electric conductivity of material and effectively holds
SnO is carried2Volumetric expansion in electrochemical reaction process.When the material is as sodium-ion battery negative pole, with preferable electricity
Chemical stability.
Claims (6)
1. it is a kind of prepare on honeycomb carbon adhere to tin oxide nano particles composite method;It is characterized in that specific steps are such as
Under:
1) the lower SnCl for preparing 0.25-1.00mol/L of magnetons stirring4·5H2O solution;
2) takes honeycomb carbon and adds step 1) SnCl that obtains4·5H2O solution so that the concentration of honeycomb carbon is 5-7.5g/L, is gone forward side by side
Row is ultrasonically treated;
3) is by step 2) the presoma mixed liquor that obtains is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner, and using stainless
After the sealing of steel reactor, 170-190 DEG C is heated to, is incubated 12-36h;
4) after reactions terminate, normal temperature is cooled at room temperature, takes out reactant, washed using deionized water and ethanol respectively, carry out
Dried process, obtains desciccate.
5) is by step 4) desciccate that obtains made annealing treatment in argon gas atmosphere, obtains SnO2/ honeycomb carbon composite.
2. the method for claim 1, it is characterized in that the step 2) in the aperture size of honeycomb carbon be less than 5 μm.
3. the method for claim 1, it is characterized in that the step 4) drying condition is to dry 8-12h at 60-80 DEG C.
4. the method for claim 1, it is characterized in that the step 4) washed 3-5 times with deionized water and ethanol.
5. the method for claim 1, it is characterized in that the step 5) annealing condition is:In argon gas atmosphere, rise
Warm speed is 5-10 DEG C/min, and 120-200min is incubated at 600-650 DEG C, then naturally cools to room temperature.
6. the method for claim 1, it is characterized in that described be with magneton stirring optimum condition:1-20r/s.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107516732A (en) * | 2017-08-08 | 2017-12-26 | 南陵县生产力促进中心 | A kind of SnO&MoS as Anode of lithium cell2The preparation method of composite |
CN108493403A (en) * | 2018-05-17 | 2018-09-04 | 中山大学 | A kind of synthetic method of self-supporting sodium-ion battery cathode |
CN114068895A (en) * | 2021-10-28 | 2022-02-18 | 华南理工大学 | Lignin-based graphene porous carbon nanosheet tin dioxide composite material and preparation and application thereof |
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CN104157876A (en) * | 2014-08-14 | 2014-11-19 | 上海交通大学 | Preparation method of porous carbon-tin nanocomposite material for lithium battery cathode |
CN106058184A (en) * | 2016-07-08 | 2016-10-26 | 天津大学 | Method for preparing tin dioxide/porous carbon sphere composite material |
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CN104157876A (en) * | 2014-08-14 | 2014-11-19 | 上海交通大学 | Preparation method of porous carbon-tin nanocomposite material for lithium battery cathode |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107516732A (en) * | 2017-08-08 | 2017-12-26 | 南陵县生产力促进中心 | A kind of SnO&MoS as Anode of lithium cell2The preparation method of composite |
CN107516732B (en) * | 2017-08-08 | 2020-08-11 | 南陵县生产力促进中心 | Preparation method of SnO & MoS2 composite material used as lithium battery anode |
CN108493403A (en) * | 2018-05-17 | 2018-09-04 | 中山大学 | A kind of synthetic method of self-supporting sodium-ion battery cathode |
CN108493403B (en) * | 2018-05-17 | 2020-10-27 | 中山大学 | Synthesis method of self-supporting sodium ion battery cathode |
CN114068895A (en) * | 2021-10-28 | 2022-02-18 | 华南理工大学 | Lignin-based graphene porous carbon nanosheet tin dioxide composite material and preparation and application thereof |
CN114068895B (en) * | 2021-10-28 | 2023-01-06 | 华南理工大学 | Lignin-based graphene porous carbon nanosheet tin dioxide composite material and preparation and application thereof |
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