CN108987719A - A kind of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material and preparation method thereof - Google Patents
A kind of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material and preparation method thereof Download PDFInfo
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- CN108987719A CN108987719A CN201810840964.5A CN201810840964A CN108987719A CN 108987719 A CN108987719 A CN 108987719A CN 201810840964 A CN201810840964 A CN 201810840964A CN 108987719 A CN108987719 A CN 108987719A
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- H—ELECTRICITY
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Abstract
The present invention provides a kind of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode materials and preparation method thereof, are related to field of batteries, which includes: that (1) prepares three-dimensional sulfur doping porous carbon.(2) sulfur doping porous carbon is mixed and is dissolved with mass ratio 1:0.2~5 with the chloride of tin, assisting ultrasonic 0.5-2h, the mixed solution is transferred in reaction kettle, solvent-thermal method keeps the temperature 1~10h at 150~220 DEG C, obtains the combination electrode material of stannic oxide mass ratio 5%-60%.The performances such as specific capacitance, power density, energy density, high rate performance, the cyclical stability of the three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material prepared by this method are greatly improved and improve, compared to existing electrode material, this method is simple to operation, it can be used as new energy electric motor vehicle battery pack electrode material, promote the development of new-energy automobile.
Description
Technical field
The present invention relates to field of batteries, in particular to a kind of three-dimensional sulfur doping porous carbon/stannic oxide compound electric
Pole material and preparation method thereof.
Background technique
Lithium ion battery has high operating voltage, energy density height, self discharge speed as a kind of novel rechargable power supplies
The advantages that rate is low, safety non-pollution, is widely used on the portable electronic devices such as mobile phone, laptop.Mesh
Before, commercial lithium ion battery negative material is mainly graphite/carbon material, electric conductivity with higher, but its theoretical specific capacity
It is lower, high rate performance is poor, constrain its application in next-generation lithium ion battery.Metal oxide theory with higher
Specific capacity, but its poorly conductive are easy to reunite during the reaction, cause cyclical stability poor, capacity retention ratio is low.
In consideration of it, the present invention is specifically proposed.
Summary of the invention
The purpose of the present invention is to provide a kind of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material and its preparations
Method, the specific capacity of the electrode composite material is big, good rate capability, energy density are big, and energy-storage property is outstanding, can be used for new energy
Automobile batteries packet electrode material, promotes the development of new-energy automobile.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
In a first aspect, the present invention provides a kind of preparation side of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material
Method comprising:
Sulfur doping porous carbon is mixed and dissolved with mass ratio 1:0.2~5 with stannous chloride, using solvent-thermal method in 150
1~10h is kept the temperature at~220 DEG C.
Further, in preferred embodiments of the present invention, above-mentioned using during solvent-thermal method, heating rate is 1~5
℃/min。
Further, in preferred embodiments of the present invention, the sulphur atom amount of mixing in above-mentioned sulfur doping porous carbon is 1~
30%.
Further, in preferred embodiments of the present invention, above-mentioned sulfur doping porous carbon is by by carbon source and sulfate
Mixing, 0.5~3h of heat preservation carbonization is prepared at 450~800 DEG C under an inert gas.
Further, in preferred embodiments of the present invention, the mass ratio of above-mentioned carbon source and sulfate is 1:0.5~6.
Further, in preferred embodiments of the present invention, above-mentioned carbon source is selected from slurry oil, pitch, sucrose, glucose, fibre
At least one of dimension element and starch.Further, in preferred embodiments of the present invention, above-mentioned sulphur source is selected from magnesium sulfate, sulphur
At least one of sour sodium, aluminum sulfate, sodium bisulfate, calcium sulfate and zinc sulfate.Further, in preferred embodiments of the present invention
In, the above-mentioned heating rate prepared during sulfur doping porous carbon is 2~10 DEG C/min.
Further, in preferred embodiments of the present invention, heat preservation carbonization after, further include to gained be carbonized ability product into
The step of row pickling, washing.
Second aspect, it is multiple that the present invention provides three-dimensional sulfur doping porous carbon/stannic oxide made from a kind of above-mentioned preparation method
Composite electrode material, the degree of sulphur atom are 1~30%, and lithium ion memory capacity is 1000-3000mAh/g, and energy is close
Degree is 150-350wh/kg.Compared with prior art, beneficial effects of the present invention for example,
The preparation method of this three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material provided by the invention, with sulphur
Doped carbon is carrier, and transition metal tin is introduced between carbon nanometer layer and in duct by solvent-thermal method, keeps it uniform with carbon carrier
And closely combine, sulfur doping carbon/stannic oxide nanometer complex is obtained, can be used as electrode material use.By to preparation side
Each response parameter in method optimizes, and realizes the Effective Regulation to stannic oxide pattern, size and dispersibility, thus favorably
In the synergistic effect for further playing sulfur doping carbon and stannic oxide.
For inventor the study found that compared to the carbon not mixed, sulphur atom adulterates the chemical ring that can significantly affect carbon structure
Border, including surface polarity and electronic state enhance chemical property to promote carbon-based electrochemical process, improve lithium ion
Memory capacity.
Compared to existing electrode material, the three-dimensional sulfur doping porous carbon/stannic oxide prepared by this method is compound
The performances such as specific capacitance, power density, energy density, high rate performance, the cyclical stability of electrode material be greatly improved with
It improves.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described.
Fig. 1 is three sulfur doping porous carbon transmission electron microscope pictures that embodiment 1 provides.
Fig. 2 is three-dimensional sulfur doping porous carbon/stannic oxide transmission electron microscope picture that embodiment 2 provides.
Fig. 3 is three-dimensional sulfur doping porous carbon/stannic oxide transmission electron microscope picture that embodiment 3 provides.
Fig. 4 is three sulfur doping porous carbon/tin dioxide composite material x-ray photoelectron spectroscopies that embodiment 3 provides
Figure.
Fig. 5 is three-dimensional sulfur doping porous carbon/stannic oxide transmission electron microscope picture that embodiment 4 provides.
Fig. 6 is the high rate performance figure for three-dimensional sulfur doping porous carbon/stannic oxide that embodiment 4 provides.
Fig. 7 is sulfur doping porous carbon/stannic oxide combination electrode material charging and discharging curve figure that embodiment 4 provides.
Fig. 8 is 4 sulfur doping porous carbon of embodiment/stannic oxide combination electrode material power density-energy density curve
Figure.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
Present embodiment provides a kind of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material, preparation method packet
It includes:
Sulfur doping porous carbon is mixed and dissolved with mass ratio 1:0.2~5 with stannous chloride, using solvent-thermal method in 150
1~10h is kept the temperature at~220 DEG C.
Further, during using solvent-thermal method, heating rate is 1~5 DEG C/min, or be 1.5~2.5
DEG C/min, or be 1.8~2.2 DEG C/min.
Wherein, the sulphur atom amount of mixing is 0.1~30% in sulfur doping porous carbon, be perhaps 3~22% or be 5~
20%, it is perhaps 7~18% to be perhaps 9~16% or be 11~14%.
The sulfur doping porous carbon the preparation method is as follows:
Carbon source is mixed with sulfate, 0.5~3h of heat preservation carbonization is prepared at 450~800 DEG C under an inert gas
It arrives.
By this method, controllable to prepare sulfur doping carbon, realize the doping vario-property of carbon material, and then effectively adjust its electricity
Sub- hole widens energy gap and it is induced to generate more topological defects, so that sulfur doping carbon has more on lower voltage platform
Excellent chemical property.
In the method, carbon source is slurry oil, pitch, sucrose, glucose, cellulose and starch；Sulfate as template,
Including but not limited to magnesium sulfate, sodium sulphate, aluminum sulfate, sodium bisulfate, calcium sulfate and zinc sulfate, more preferably, template is
Magnesium sulfate.
Preferably, the mass ratio of carbon source and sulfate is 1:0.5~6, or is 1:0.7~5；It or is 1:0.8
~4；It or is 1:0.9~3；It or is 1:1.1.
It is more preferred, the preparation method of sulfur doping porous carbon further include: pickling, washing are carried out to gained carbonization ability product
The step of, to remove template agent removing, obtain clean sulfur doping porous carbon.It is further preferable that carrying out pickling using citric acid soln.
More preferably, heating rate during preparing sulfur doping porous carbon is 2~10 DEG C/min, or is 3
~8 DEG C/min, or be 5~7 DEG C/min.Using temperature programming, strict control temperature program, the substrate that makes to be carbonized is in heating process
In be slowly carbonized, be conducive to further promoted sulfur doping carbon performance.
Feature and performance of the invention are described in further detail with reference to embodiments:
Embodiment 1
The present embodiment provides a kind of three-dimensional sulfur doping porous carbon materials, preparation method includes:
Slurry oil and magnesium sulfate are mixed to uniformly with mass ratio 1:3, which are transferred in horizontal pipe furnace,
It is passed through argon gas and does protective atmosphere, be warming up to 700 with the heating rate of 5 DEG C/min, keep the temperature 1h to get three-dimensional sulfur doping porous carbon
Material, transmission electron microscope photo are as shown in Figure 1.The method does not need template presoma, and a method obtains three containing porous structure
Sulfur doping porous carbon materials are tieed up, method is simple.
Embodiment 2
The present embodiment provides a kind of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material, preparation method includes:
The sulfur doping porous carbon that embodiment is prepared is mixed with stannous chloride with mass ratio 1:1 and is dissolved into water,
This solution is transferred in autoclave, autoclave is put into baking oven and makes baking oven with the heating rate of 1 DEG C/min
It is warming up at 150 DEG C, keeps the temperature 10h.
It is to be cooled to after room temperature, washing, drying obtain three-dimensional sulfur doping porous carbon/tin dioxide composite material.This method
The partial size 3-5nm of obtained three-dimensional sulfur doping porous carbon/tin dioxide composite material, load capacity 45% are evenly distributed, thoroughly
It is as shown in Figure 2 to penetrate electron microscope.
Embodiment 3
The present embodiment provides a kind of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material, preparation method includes:
A. sucrose is mixed with magnesium sulfate, is heated up at 450 DEG C with the heating rate of 2 DEG C/min under an inert gas, heat preservation
Be carbonized 0.5h, after being washed with citric acid soln, is washed with water, obtains sulfur doping porous carbon.
B. sulfur doping porous carbon is mixed with stannous chloride with mass ratio 1:5 and is dissolved into water, this solution is transferred to
In autoclave, autoclave is put into baking oven and is warming up to baking oven at 220 DEG C with the heating rate of 5 DEG C/min,
Keep the temperature 1h.
C. to be cooled to after room temperature, washing, drying obtain three-dimensional sulfur doping porous carbon/tin dioxide composite material.
Transmission electron microscope picture such as Fig. 3 of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material provided in this embodiment
It is shown, it is clear that tin dioxide nano-particle is uniformly dispersed in the surface and duct of sulfur doping porous carbon by the figure
It is interior.Stannic oxide load capacity mass percent 85%.Fig. 4 is corresponding x-ray photoelectron spectroscopy figure, as we can see from the figure S
Content be 8.1%, Sn atomic ratio content be 15.4%.Prove that S is bonded in carbon material in the form of chemical combination key, SnO2At
Function be combined in the duct of porous carbon and surface.
Embodiment 4
The present embodiment provides a kind of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material, preparation method includes:
A. sucrose is mixed with magnesium sulfate, is heated up at 600 DEG C with the heating rate of 2 DEG C/min under an inert gas, heat preservation
Be carbonized 2h, after being washed with citric acid soln, is washed with water, obtains sulfur doping porous carbon.
B. sulfur doping porous carbon is mixed with stannous chloride with mass ratio 1:2 and is dissolved into water, this solution is transferred to
In autoclave, autoclave is put into baking oven and is warming up to baking oven at 200 DEG C with the heating rate of 2 DEG C/min,
Keep the temperature 5h.
C. to be cooled to after room temperature, washing, drying obtain three-dimensional sulfur doping porous carbon/tin dioxide composite material.
Transmission electron microscope picture such as Fig. 5 of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material provided in this embodiment
It is shown, it is clear that tin dioxide nano-particle is uniformly dispersed in the surface and duct of sulfur doping porous carbon by the figure
It is interior.Stannic oxide load capacity mass percent 65%.
There is high lithium storage content, Fig. 6 by sulfur doping porous carbon/stannic oxide combination electrode material prepared by this method
For high rate performance figure.When current density is 200mA/g, sulfur doping porous carbon/stannic oxide combination electrode material capacity is
1490mAh/g, when current density is 1600mA/g, capacity remains to remain 800mAh/g.When current density is 200mA/g
The lithium storage content of sulfur doping porous carbon is 1305mAh/g, and when current density is 1600mA/g, capacity remains to remain 580mAh/
g.It will be appreciated from fig. 6 that sulfur doping porous carbon/stannic oxide combination electrode material has higher lithium storage content, there is excellent electricity
Chemical property.
Sulfur doping porous carbon/stannic oxide combination electrode material charging and discharging curve figure is as shown in Fig. 7, as seen from the figure,
The material has preferable cycle performance.
Sulfur doping porous carbon/stannic oxide combination electrode material power density-energy density curve graph such as Fig. 8 institute
Show, as seen from the figure, in current density 0.2C, energy density can reach 341Wh/Kg, and sulfur doping porous carbon/stannic oxide is compound
Electrode material has higher energy density and power density.It can be applied on New-energy electric vehicle, be new energy power
The development of battery is opened up a path.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from of the invention
Many other change and modification can be made in the case where spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of preparation method of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material, characterized in that it comprises:
Sulfur doping porous carbon is mixed and dissolved with mass ratio 1:0.2~5 with stannous chloride, using solvent-thermal method in 150~220
1~10h is kept the temperature at DEG C.
2. the preparation method of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material according to claim 1, special
Sign is, during using the solvent-thermal method, heating rate is 1~5 DEG C/min.
3. the preparation method of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material according to claim 1, special
Sign is that the sulphur atom amount of mixing in the sulfur doping porous carbon is 1~30%.
4. the preparation method of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material according to claim 3, special
Sign is that the sulfur doping porous carbon is kept the temperature at 450~800 DEG C under an inert gas by mixing carbon source with sulphur source
0.5~3h of carbonization is prepared.
5. the preparation method of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material according to claim 4, special
Sign is that the mass ratio of the carbon source and the sulphur source is 1:0.5~6.
6. the preparation method of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material according to claim 4, special
Sign is that the carbon source is selected from least one of slurry oil, pitch, sucrose, glucose, cellulose and starch.
7. the preparation method of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material according to claim 4, special
Sign is that the sulphur source is selected from least one of magnesium sulfate, sodium sulphate, aluminum sulfate, sodium bisulfate, calcium sulfate and zinc sulfate.
8. the preparation method of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material according to claim 4, special
Sign is that heating rate during preparing the sulfur doping porous carbon is 2~10 DEG C/min.
9. the preparation method of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material according to claim 4, special
Sign is, after heat preservation carbonization, further includes the steps that carrying out gained carbonized product pickling, washing.
10. a kind of three-dimensional sulfur doping porous carbon/stannic oxide as made from preparation method according to any one of claims 1 to 9
Combination electrode material, which is characterized in that the degree of sulphur atom is 1~30%, and lithium ion memory capacity is 1000-
3000mAh/g, energy density 150-350wh/kg.
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