CN109192542A - Supercapacitor stannic disulfide/graphite phase carbon nitride composite material and preparation method - Google Patents
Supercapacitor stannic disulfide/graphite phase carbon nitride composite material and preparation method Download PDFInfo
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- CN109192542A CN109192542A CN201811152202.2A CN201811152202A CN109192542A CN 109192542 A CN109192542 A CN 109192542A CN 201811152202 A CN201811152202 A CN 201811152202A CN 109192542 A CN109192542 A CN 109192542A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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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
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- Y02E60/13—Energy storage using capacitors
Abstract
The present invention relates to supercapacitor stannic disulfide/graphite phase carbon nitride composite material and preparation methods, melamine are calcined in Muffle furnace, blocky g-C is made3N4；(2) by blocky g-C3N4SnCl is distributed under ultrasonic treatment4·5H2In the ethanol solution of O；(3) thioacetamide is added in step (2) mixed solution obtained and is stirred at room temperature to transparent；(4) clear solution is sealed and is heated；(5) it after being cooled to room temperature, collects products therefrom and washs for several times；(6) step (5) material obtained is dried, obtains supercapacitor SnS2/g‑C3N4Composite material.Compared with prior art, the SnS that the present invention is prepared2/g‑C3N4Composite material has good capacitive property and cyclical stability, is the ideal electrode material of supercapacitor.
Description
Technical field
The present invention relates to belonging to electrode material for super capacitor technical field, more particularly, to a kind of supercapacitor with two
Artificial gold/graphite phase carbon nitride composite material and preparation method.
Background technique
The advantages that supercapacitor is due to its high power density, excellent cyclical stability, low cost and fast charging and discharging,
It is considered as a kind of equipment of great potential of next-generation energy storage.Pass through exploitation new electrode materials, electrolyte and device
The energy and power density of supercapacitor can be improved.Usual electrode material be influence performance of the supercapacitor it is important because
Element, two chalcogenide of transition metal (TMDCs) is as a kind of promising two-dimentional layered material, due to ion between overlapping layer
Be effectively embedded into the capacitive property that supercapacitor can be enhanced.Stannic disulfide (SnS2) it is important in TMDCs family partly to lead
One of body attracts wide attention in terms of energy storage and conversion.Although SnS2With very high theoretical capacity, but its is low
Intrinsic conductivity and large volume fluctuation result in SnS2Storge quality in practical applications is poor.By SnS2It is multiple with carbon-based material
Conjunction can overcome disadvantage mentioned above, and composite material obtained has large specific surface area, activated centre is more, diffusion path is short etc.
The chemical property of supercapacitor can be improved in advantage.
Graphite-phase C3N4(g-C3N4) be the graphene similar structures being made of carbon and nitrogen-atoms, due to its high-specific surface area,
Environment friendly and low cost have been widely used in photoelectron, photocatalysis, the energy-storage systems such as supercapacitor.Due to two dimension
The aspect ratio of material can show biggish specific surface area, which can provide excellent charge storage performance.Meanwhile with biography
The carbon material of system is compared, g-C3N4In nitrogen can improve the electron donor characteristic of material, improve the wetability of material in electrolyte,
Further increase capacitive property.
Currently, SnS2With g-C3N4Compound composite material obtained is only applied in photocatalysis field, and the present invention utilizes
Synergistic effect after the two is compound improves electric conductivity, to further increase chemical property, is applied to super capacitor
Device field.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of supercapacitors to use
Stannic disulfide/graphite phase carbon nitride composite material preparation method.
The purpose of the present invention can be achieved through the following technical solutions:
Supercapacitor stannic disulfide/graphite phase carbon nitride composite material preparation method, comprising the following steps:
(1) melamine is calcined in Muffle furnace and blocky g-C is made3N4；
(2) by blocky g-C3N4SnCl is distributed under ultrasonic treatment4·5H2In the ethanol solution of O；
(3) thioacetamide is added in step (2) mixed solution obtained and is stirred at room temperature to transparent；
(4) clear solution is sealed and is heated；
(5) it after being cooled to room temperature, collects products therefrom and washs for several times；
(6) step (5) material obtained is dried, obtains supercapacitor SnS2The nitridation of/graphite-phase
Carbon composite.
In step (1) when calcining, it is warming up to 540-560 DEG C with 3-6 DEG C per minute of rate, then keeps the temperature 3-5 hours.
Bulk g-C in step (2)3N4With SnCl4·5H2The mass ratio of O is 30-300:350.
The ultrasonic disperse time is 30-90min, ultrasonic power 120W in step (2).
The thioacetyl and bulk g-C that step (3) is added3N4Mass ratio be 325:30-300.
The temperature of control heating is 160-200 DEG C in step (4), time 8-12h.
Step (5) is washed using ethyl alcohol and deionized water.
The material of acquisition is dried in vacuo 6-8h at 60 DEG C by step (6).
The present invention also provides a kind of supercapacitor stannic disulfide/g-C that above-mentioned preparation method is prepared3N4It is multiple
Condensation material, wherein g-C3N4It can not only play and avoid SnS2The effect of accumulation, nitrogenous carbon material can also further improve compound
The electric conductivity of material, electrode composite material obtained have good capacitive property and cyclical stability, are supercapacitors
Ideal electrode material.
Compared with prior art, the invention has the following advantages:
(1) SnS that the present invention is prepared using hydrothermal synthesis method2/g-C3N4Composite process is simple, does not need complexity and sets
It is standby and low in cost.
(2) hydrothermal synthesis method that the present invention uses only is needed in relatively low reaction temperature and is obtained in the time
Stable two-dimentional flower-like structure, the SnS of the structure2/g-C3N4Composite material has excellent capacitive property.Be higher than when temperature or
SnS when lower than the temperature and time2/g-C3N4Composite material is in two-dimensional slice stratiform, can not form flower-like structure.
(3) SnS prepared by the present invention2/g-C3N4Composite material has the capacitive character of good electrochemical stability and enhancing
Can, it is the ideal electrode material of supercapacitor.
Detailed description of the invention
Fig. 1 is SnS prepared by embodiment 22/g-C3N4The characterization photo of composite material；
Fig. 2 is SnS prepared by embodiment 22/g-C3N4The nyquist diagram of the electrochemical impedance spectroscopy of composite material.
Fig. 3 is SnS prepared by embodiment 22/g-C3N4Cyclic voltammogram of the composite material under different scanning rates.
Fig. 4 is SnS prepared by embodiment 22/g-C3N4Constant current charge-discharge curve of the composite material under different current densities
Figure.
Fig. 5 is SnS prepared by embodiment 22/g-C3N4The stable circulation performance curve graph of composite material.
In Fig. 1, a SnS2/g-C3N4The scanning electron microscope SEM image of composite material, b are transmission electron microscope
TEM figure, c and d are high resolution transmission electron microscope HR-TEM figure, and e is corresponding selective electron diffraction SAED figure, and f is carbon,
The respective element mapping graph of nitrogen, tin and sulphur.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1
Melamine calcines preparation g-C in Muffle furnace3N4, calcination procedure is as follows: calcination procedure is as follows: with 5 DEG C per minute
Rate be warming up to 560 DEG C after, keep the temperature 3 hours.Then, by the resulting bulk g-C of 30mg3N4Dispersed under ultrasonic treatment at 1 hour
Contain 350mg SnCl to 30ml4·5H2In the ethanol solution of O.Later, 325mg thioacetamide (TAA) is added to above-mentioned
In solution and it is stirred at room temperature 4 hours.Finally, obtained clear solution to be moved to the autoclave of 50ml teflon lined
In, it seals and is heated 12 hours at 160 DEG C.After being cooled to room temperature, collects products therefrom and washed using ethyl alcohol and deionized water
Three times to remove impurity.Obtained material is further dried 6 hours under 60 DEG C of vacuum, obtains supercapacitor SnS2/g-C3N4
(SSCN-1) composite material.Electrochemical property test is carried out to it, the charge transfer resistance (Rct) of the composite material is 0.76,
And there is lower equivalent series impedance and excellent diffusion.Cyclic voltammetry curve is in class rectangle, when sweep speed is from 2
Increase to 100mV s-1When, the shape of curve is left undistorted, and shows that the composite material has good high rate performance.By filling
Discharge curve can be calculated, when current density is 0.5A g-1When, which goes out 411F g-1Specific capacitance value, tool
There is excellent chemical property.
Embodiment 2
Melamine calcines preparation g-C in Muffle furnace3N4, calcination procedure is as follows: calcination procedure is as follows: with 4 DEG C per minute
Rate be warming up to 550 DEG C after, keep the temperature 4 hours.Then, by the resulting bulk g-C of 50mg3N4Dispersed under ultrasonic treatment at 1 hour
Contain 350mg SnCl to 30ml4·5H2In the ethanol solution of O.Later, 325mg thioacetamide (TAA) is added to above-mentioned
In solution and it is stirred at room temperature 4 hours.Finally, obtained clear solution to be moved to the autoclave of 50ml teflon lined
In, it seals and is heated 12 hours at 160 DEG C.After being cooled to room temperature, collects products therefrom and washed using ethyl alcohol and deionized water
Three times to remove impurity.Obtained material is further dried 6 hours under 60 DEG C of vacuum, obtains supercapacitor SnS2/g-C3N4
(SSCN-2) composite material.Electrochemical property test is carried out to it, the charge transfer resistance (Rct) of the composite material is 0.68,
And there is lower equivalent series impedance and excellent diffusion.Cyclic voltammetry curve is in class rectangle, when sweep speed is from 2
Increase to 100mV s-1When, the shape of curve is left undistorted, and shows that the composite material has good high rate performance.By filling
Discharge curve can be calculated, when current density is 0.5A g-1When, which goes out 552F g-1Specific capacitance value, tool
There is excellent chemical property.
Embodiment 3
Melamine calcines preparation g-C in Muffle furnace3N4, calcination procedure is as follows: calcination procedure is as follows: with 5 DEG C per minute
Rate be warming up to 540 DEG C after, keep the temperature 5 hours.Then, by the resulting bulk g-C of 100mg3N4Divided under ultrasonic treatment at 1 hour
It is scattered to 30ml and contains 350mg SnCl4·5H2In the ethanol solution of O.Later, 325mg thioacetamide (TAA) is added to
It states in solution and is stirred at room temperature 4 hours.Finally, obtained clear solution to be moved to the high pressure of 50ml teflon lined
In kettle, seals and heated 12 hours at 160 DEG C.After being cooled to room temperature, collects products therefrom and washed using ethyl alcohol and deionization
It washs three times to remove impurity.Obtained material is further dried 6 hours under 60 DEG C of vacuum, obtains supercapacitor SnS2/g-
C3N4(SSCN-3) composite material.Electrochemical property test is carried out to it, the charge transfer resistance (Rct) of the composite material is
0.69, and there is lower equivalent series impedance and excellent diffusion.Cyclic voltammetry curve is in class rectangle, when scanning speed
Rate increases to 100mV s from 2-1When, the shape of curve is left undistorted, and shows that the composite material has good high rate performance.
It can be calculated by charging and discharging curve, when current density is 0.5A g-1When, which goes out 417F g-1Specific capacitance
Value has excellent chemical property.
Embodiment 4
Melamine calcines preparation g-C in Muffle furnace3N4, calcination procedure is as follows: calcination procedure is as follows: with 6 DEG C per minute
Rate be warming up to 550 DEG C after, keep the temperature 4 hours.Then, by the resulting bulk g-C of 300mg3N4Divided under ultrasonic treatment at 1 hour
It is scattered to 30ml and contains 350mg SnCl4·5H2In the ethanol solution of O.Later, 325mg thioacetamide (TAA) is added to
It states in solution and is stirred at room temperature 4 hours.Finally, obtained clear solution to be moved to the high pressure of 50ml teflon lined
In kettle, seals and heated 12 hours at 160 DEG C.After being cooled to room temperature, collects products therefrom and washed using ethyl alcohol and deionization
It washs three times to remove impurity.Obtained material is further dried 6 hours under 60 DEG C of vacuum, obtains supercapacitor SnS2/g-
C3N4(SSCN-4) composite material.Electrochemical property test is carried out to it, the charge transfer resistance (Rct) of the composite material is
0.70, and there is lower equivalent series impedance and excellent diffusion.Cyclic voltammetry curve is in class rectangle, when scanning speed
Rate increases to 100mV s from 2-1When, the shape of curve is left undistorted, and shows that the composite material has good high rate performance.
It can be calculated by charging and discharging curve, when current density is 0.5A g-1When, which goes out 329F g-1Specific capacitance
Value has excellent chemical property.
Embodiment 5
Supercapacitor stannic disulfide/graphite phase carbon nitride composite material preparation method, comprising the following steps:
(1) melamine is calcined in Muffle furnace and blocky g-C is made3N4, with 3 DEG C of rate per minute heating when calcining
To 540 DEG C, then 5 hours are kept the temperature；
(2) by blocky g-C3N4SnCl is distributed under ultrasonic treatment4·5H2In the ethanol solution of O, blocky g-C3N4With
SnCl4·5H2The mass ratio of O is 30:350, and the ultrasonic disperse time is 30min, and the power of the Vltrasonic device used is 120W；
(3) thioacetamide is added in step (2) mixed solution obtained and is stirred at room temperature to transparent, added
The thioacetyl and bulk g-C entered3N4Mass ratio be 325:30；
(4) clear solution is sealed, the temperature for controlling heating is 160 DEG C, heats 12h；
(5) it after being cooled to room temperature, collects products therefrom and is washed for several times using ethyl alcohol and deionized water；
(6) step (5) material obtained is dried in vacuo 6h at 60 DEG C, obtains supercapacitor SnS2/g-C3N4
Composite material, in above-mentioned material, g-C3N4It can not only play and avoid SnS2The effect of accumulation, nitrogenous carbon material can also be into one
Step improves the electric conductivity of composite material, and it is super that electrode composite material obtained, which has good capacitive property and cyclical stability,
The ideal electrode material of grade capacitor.
Embodiment 6
Supercapacitor stannic disulfide/graphite phase carbon nitride composite material preparation method, comprising the following steps:
(1) melamine is calcined in Muffle furnace and blocky g-C is made3N4, with 6 DEG C of rate per minute heating when calcining
To 560 DEG C, then 3 hours are kept the temperature；
(2) by blocky g-C3N4SnCl is distributed under ultrasonic treatment4·5H2In the ethanol solution of O, blocky g-C3N4With
SnCl4·5H2The mass ratio of O is 300:350, and the ultrasonic disperse time is 90min, and the power of the Vltrasonic device used is 120W；
(3) thioacetamide is added in step (2) mixed solution obtained and is stirred at room temperature to transparent, added
The thioacetyl and bulk g-C entered3N4Mass ratio be 325:300；
(4) clear solution is sealed, the temperature for controlling heating is 200 DEG C, heats 8h；
(5) it after being cooled to room temperature, collects products therefrom and is washed for several times using ethyl alcohol and deionized water；
(6) step (5) material obtained is dried in vacuo 8h at 60 DEG C, obtains supercapacitor SnS2/g-C3N4
Composite material.
In Fig. 1, a SnS2/g-C3N4The scanning electron microscope SEM image of composite material, it can be observed that flower-like structure
SnS2For random orientation, there is fine and close but non-uniform size distribution.Shown in the transmission electron microscope TEM figure of b, preparation
SnS2/g-C3N4Composite material good dispersion and without significantly building up, shows SnS2Energy and g-C3N4Surface combines.SnS2/g-C3N4It is multiple
The high resolution transmission electron microscope HR-TEM of condensation material schemes as shown in c-d, it can be seen that between the lattice of three lattice fringes
Away from matching with JCPDS card number 23-0677.Corresponding selective electron diffraction SAED figure (figure e) shows SnS2(100) and g-
C3N4(002) exist while plane, further demonstrate SnS2/g-C3N4The formation of composite material.The phase of carbon, nitrogen, tin and sulphur
Answer element mapping as shown byf, which demonstrate SnS2And g-C3N4Be uniformly distributed.The result shows that the SnS of preparation2/g-C3N4It is compound
Material has stable microstructure, facilitates carrier separation and electron-transport efficiency.
Fig. 2 is SnS2/g-C3N4The electrochemical impedance spectroscopy that composite material measures in the frequency range of 10mHz-100000Hz
(EIS) nyquist diagram.The material has lesser equivalent series resistance (Rs) and charge transfer resistance (Rct) value, and bent
Line is that almost vertical line, that is, Warburg value is smaller, shows the ideal capacitance behavior of diffusion controlling mechanism.
Fig. 3 is SnS2/g-C3N4Composite material is in 2-100mV s-1Sweep speed under cyclic voltammogram.- 0.3 to-
In the voltage window of 0.80V, CV curve shows typical quasi- rectangular shape.When sweep speed increases to 100mV s-1 from 2
When, the shape of CV curve is left undistorted, and shows SnS2/g-C3N4Composite material can quick electric potential scanning in aqueous electrolyte
And there is good high rate performance.
Fig. 4 is SnS2/g-C3N4Composite material is in 0.5-10A g-1Current density under constant current charge-discharge curve graph.It is logical
GCD survey calculation is crossed in 0.5A g-1Current density under, specific capacitance value be 552F g-1.It is observed that current density increases
When the charge and discharge time reduce, this is because the effective interaction between electrolyte ion and electrode reduces, lead to lower ratio
Capacitor, this shows that energy storage mechanism may be electrochemistry diffusion.
Fig. 5 is SnS2/g-C3N4Composite material is in 10A g-1Current density under the cycle performance curve that measures.15000
SnS after secondary charge-discharge test2/g-C3N4Show lesser capacitor consumption, capacitor retention rate is 95.8%, shows it with good
Good cyclical stability.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (9)
1. supercapacitor stannic disulfide/graphite phase carbon nitride composite material preparation method, which is characterized in that this method packet
Include following steps:
(1) melamine is calcined in Muffle furnace and blocky g-C is made3N4；
(2) by blocky g-C3N4SnCl is distributed under ultrasonic treatment4·5H2In the ethanol solution of O；
(3) thioacetamide is added in step (2) mixed solution obtained and is stirred at room temperature to transparent；
(4) clear solution is sealed and is heated；
(5) it after being cooled to room temperature, collects products therefrom and washs for several times；
(6) step (5) material obtained is dried, obtains supercapacitor SnS2/g-C3N4Composite material.
2. supercapacitor according to claim 1 stannic disulfide/graphite phase carbon nitride composite material preparation method,
It is characterized in that, being warming up to 540-560 DEG C when calcining in step (1) with 3-6 DEG C per minute of rate, it is small then to keep the temperature 3-5
When.
3. supercapacitor according to claim 1 stannic disulfide/graphite phase carbon nitride composite material preparation method,
It is characterized in that, bulk g-C in step (2)3N4With SnCl4·5H2The mass ratio of O is 30-300:350.
4. the supercapacitor according to claim 1 preparation method of stannic disulfide graphite phase carbon nitride composite material,
It is characterized in that, the ultrasonic disperse time is 30-90min, ultrasonic power 120W in step (2).
5. supercapacitor according to claim 1 stannic disulfide/graphite phase carbon nitride composite material preparation method,
It is characterized in that, thioacetyl and bulk g-C that step (3) is added3N4Mass ratio be 325:30-300.
6. supercapacitor according to claim 1 stannic disulfide/graphite phase carbon nitride composite material preparation method,
It is characterized in that, the temperature of control heating is 160-200 DEG C in step (4), time 8-12h.
7. supercapacitor according to claim 1 stannic disulfide/graphite phase carbon nitride composite material preparation method,
It is characterized in that, step (5) is washed using ethyl alcohol and deionized water.
8. supercapacitor according to claim 1 stannic disulfide/graphite phase carbon nitride composite material preparation method,
It is characterized in that, the material of acquisition is dried in vacuo 6-8h at 60 DEG C by step (6).
9. the supercapacitor being prepared method according to claim 1 stannic disulfide graphite phase carbon nitride composite wood
Material.
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| CN110828191A (en) * | 2019-09-27 | 2020-02-21 | 西安交通大学 | Carbon nitride/graphene/nickel disulfide supercapacitor material with porous layered structure and preparation method thereof |
| CN114243010A (en) * | 2021-12-21 | 2022-03-25 | 黑龙江省能源环境研究院 | Catalytic slurry oil based composite material and preparation method thereof |
| CN114243010B (en) * | 2021-12-21 | 2024-05-10 | 黑龙江省能源环境研究院 | Catalytic slurry oil based composite material and preparation method thereof |
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