CN110190271A - It is a kind of using carbon cloth as lithium sulfur battery anode material of substrate and preparation method thereof - Google Patents
It is a kind of using carbon cloth as lithium sulfur battery anode material of substrate and preparation method thereof Download PDFInfo
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- CN110190271A CN110190271A CN201910589074.6A CN201910589074A CN110190271A CN 110190271 A CN110190271 A CN 110190271A CN 201910589074 A CN201910589074 A CN 201910589074A CN 110190271 A CN110190271 A CN 110190271A
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Abstract
The present invention relates to a kind of using carbon cloth as lithium sulfur battery anode material of substrate and preparation method thereof, the technical issues of which solve conductivities existing for existing lithium sulfur battery anode material poor, cathode material structure destructible and positive active material continuous loss, it includes carbon cloth, active material, binder and conductive agent, growth has molybdenum disulfide nano sheet on carbon cloth, active material, binder and conductive agent are coated on the carbon cloth, and invention also provides preparation methods.It invention can be widely used in the preparation field of lithium sulfur battery anode material.
Description
Technical field
The present invention relates to a kind of electrode materials and preparation method thereof, specifically, being related to a kind of using carbon cloth as the lithium of substrate
Sulphur cell positive electrode material and preparation method thereof.
Background technique
Lithium-sulfur cell refers to that using lithium as cathode, the compound of elemental sulfur or sulphur is the high-energy secondary cell body of anode
System.The Mechanism of electrochemical behaviors of anhydrous of lithium-sulfur cell is different from the removal lithium embedded mechanism of conventional lithium ion battery, and multistep oxygen occurs for active material sulphur
Change reduction reaction, by the fracture of sulphur-sulfide linkage and generates mutually converting between realization chemical energy and electric energy.The reason of lithium-sulfur cell
2600 Wh/kg are up to by energy density, 10 times higher than conventional lithium ion battery or more, and active material sulphur has high theory
Specific capacity (1675mAh/g), feature low in cost and environmental-friendly, being widely regarded as next-generation energy storage device most has prospect
One of system.But this new energy storage system is still faced with many technical problems at present, how to guarantee lithium-sulfur cell system
Electrochemical reaction steadily carry out, obtain efficient and stable energy, it is still necessary to researchers to make further effort.
The particular problem that lithium-sulfur cell faces specifically includes that the conductivity of active material sulphur and lithium sulfide is very poor；Sulphur simple substance
Huge volume expansion (80%) can be generated in charge and discharge process, be easy to damage the structure of positive electrode；Charge and discharge
The polysulfide formed in the process is highly soluble in ether solvent, leads to the combined material continuous damage of positive electrode active material so as to cause shuttle effect
It loses.
Above-mentioned problem is easy to cause the actual specific capacity of lithium-sulfur cell low, and cyclical stability is poor, to restrict it
Using.
Summary of the invention
The present invention is exactly that conductivity existing for existing lithium sulfur battery anode material is poor, cathode material structure is fragile in order to solve
The technical issues of bad and positive active material continuous loss, provide that a kind of conductivity is good, cathode material structure is stable, electrochemistry
Performance is good using carbon cloth as lithium sulfur battery anode material of substrate and preparation method thereof.
For this purpose, the present invention provides a kind of using carbon cloth as the lithium sulfur battery anode material of substrate, the lithium-sulphur cell positive electrode material
Material includes carbon cloth, active material, binder and conductive agent, and growth has molybdenum disulfide nano sheet, the active matter on the carbon cloth
Matter, binder and conductive agent are coated on the carbon cloth.
Preferably, the active material is sublimed sulfur；The binder is polyacrylic acid；The conductive agent be Super P,
One of single wall CNTs, multi wall CNTs or Nano titanium nitride.
It preferably, is in terms of 100% by the material gross mass, the mass fraction of the molybdenum disulfide is 15~30%, institute
The mass fraction for stating sublimed sulfur is 7.5~20%, and the mass fraction of the polyacrylic acid is 2~3%, the quality of the conductive agent
Score is 2~5%, remaining is carbon cloth.
Preferably, the carbon cloth specification be 1~32K, the plain weave or twill carbon cloth of T300, T700, surface density be 70~
200g/m2。
Present invention simultaneously provides a kind of using carbon cloth as the preparation method of the lithium sulfur battery anode material of substrate comprising as follows
Carbon cloth: (1) being first placed in dehydrated alcohol and deionized water by step, and ultrasonic treatment falls carbon cloth surfaces impurity, then is shifted
It is dry into vacuum drying oven；(2) in deionized water by the dissolution of molybdenum source, sulphur source and reducing agent, ultrasonic treatment keeps Dispersion of Solute Matter equal
It is even；Then carbon cloth obtained in above-mentioned solution and the step (1) is transferred in autoclave and carries out hydro-thermal reaction, to height
After pressing reaction kettle cooling, takes out carbon cloth and be transferred in vacuum oven with dehydrated alcohol and deionized water washing by soaking, it is dry
Obtain molybdenum disulfide/carbon cloth material；(3) active material, binder and conductive agent are dissolved in organic solvent dimethyl sulfoxide
In, stir evenly, and heat up, until solute is evenly dispersed, by above-mentioned solution be coated in the molybdenum disulfide in the step (2)/
On carbon cloth；It is then placed into drying in vacuum drying oven, obtains the lithium sulfur battery anode material that carbon cloth is substrate.
Preferably, molybdenum source is sodium molybdate or ammonium molybdate in the step (2), and sulphur source is thiocarbamide, and reducing agent is anhydrous oxalic acid
Or DEXTROSE ANHYDROUS.
Preferably, the molar ratio of molybdenum source, sulphur source and reducing agent is respectively 1:(3~5 in the step (2)): (0~1).
Preferably, in the step (2), hydrothermal temperature is 180~240 DEG C, and the reaction time is 12~32h.
Preferably, in the step (2), the time of the ultrasonic treatment is 10~30min.
Preferably, in the step (3), the ratio of active material, binder and conductive agent is (6~7): (1~2): 2；
In the heating step, temperature is 140~160 DEG C.
In the present invention, carbon cloth has high conductivity and big specific surface area, and molybdenum disulfide is semiconductor, therefore,
Molybdenum disulfide nano sheet is grown on carbon cloth can guarantee higher conductivity.The electrode prepared in the present invention is raw on carbon cloth
Long molybdenum disulfide nano sheet is substrate, after the heating mixing of active material sulphur, binder, conductive agent and organic solvent, coating
In carbon cloth substrate.Since carbon cloth has higher conductivity than traditional aluminium foil, electronics is more advantageous in electrochemical reaction process
Transmission.Active material sulphur and conductive agent pass through binder physical absorption on carbon cloth, and the compact reactor of molybdenum disulfide nano sheet
Product can effective buffers active substance volume expansion, meanwhile, molybdenum disulfide can effectively inhibit the shuttle effect of more lithium sulfides, two sulphur
Changing molybdenum has anchoring effect to polysulfide, and the active site of generation not only can effectively inhibit the shuttle effect of more lithium sulfides,
The utilization rate of active material sulphur can also be improved, the chemical property of lithium-sulfur cell can be effectively promoted.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of untreated carbon cloth.
Fig. 2 is the stereoscan photograph that carbon cloth surfaces prepared by the present invention grow molybdenum disulfide nano sheet.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies content described in example and is merely to illustrate the present invention, without this hair described in claims should will not be limited
It is bright.
Embodiment 1
Step (1): by 1K, T300,140g/m2Plain weave carbon cloth be first placed in dehydrated alcohol and the solvent of deionized water
Ultrasonic treatment falls carbon cloth surfaces impurity, then is transferred into vacuum drying oven dry；
Step (2): in deionized water with the ratio dissolution of 1:4.2:0 by sodium molybdate, thiocarbamide and anhydrous oxalic acid, at ultrasound
Reason 30min keeps Dispersion of Solute Matter uniform；Then carbon cloth obtained in above-mentioned solution and step (1) is transferred in autoclave
22h is reacted at 200 DEG C, after autoclave is cooling, carbon cloth is taken out and uses dehydrated alcohol and deionized water washing by soaking respectively
For several times, it is transferred in vacuum oven and is dried to obtain molybdenum disulfide/carbon cloth material；
Step (3): active material sublimed sulfur, binder polyacrylic acid and conductive agent Super P is molten with the ratio of 6:2:2
In organic solvent dimethyl sulfoxide, stir evenly and be warming up to 150 DEG C until solute it is evenly dispersed, by above-mentioned solution be added dropwise exist
On molybdenum disulfide/carbon cloth in step (2)；It is then placed into vacuum drying oven and is dried to obtain molybdenum disulfide/carbon cloth-sulphur anode material
Material.
For the battery that 1 final product of embodiment is assembled under 0.2C current density, first circle discharge capacity is 978.1mAh/g,
436.4mAh/g is maintained at by the charge and discharge cycles capacity of 200 circles, and coulombic efficiency is close to 100%.
Embodiment 2
Step (1): by 3K, T700,120g/m2Plain weave carbon cloth be first placed in dehydrated alcohol and the solvent of deionized water
Ultrasonic treatment falls carbon cloth surfaces impurity, then is transferred into vacuum drying oven dry；
Step (2): in deionized water with the ratio dissolution of 1:4.5:1 by sodium molybdate, thiocarbamide and anhydrous oxalic acid, at ultrasound
Reason 30min keeps Dispersion of Solute Matter uniform；Then carbon cloth obtained in above-mentioned solution and step (1) is transferred in autoclave
It is reacted at 200 DEG C for 24 hours, after autoclave is cooling, takes out carbon cloth and use dehydrated alcohol and deionized water washing by soaking respectively
For several times, it is transferred in vacuum oven and is dried to obtain molybdenum disulfide/carbon cloth material；
Step (3): by active material sublimed sulfur, binder polyacrylic acid and conductive agent Super P with the ratio of 6:2:2
Be dissolved in organic solvent dimethyl sulfoxide, stir evenly and be warming up to 155 DEG C until solute it is evenly dispersed, above-mentioned solution is added dropwise
On molybdenum disulfide/carbon cloth in step (2)；It is then placed into vacuum drying oven and is dried to obtain molybdenum disulfide/carbon cloth-sulphur anode
Material.
For the battery that 2 final product of embodiment is assembled under 0.2C current density, first circle discharge capacity is 1120.4mAh/g,
658.5mAh/g is maintained at by the charge and discharge cycles capacity of 200 circles, and coulombic efficiency is close to 100%.
Embodiment 3
Step (1): by 12K, T300,140g/m2Twill carbon cloth carbon cloth be first placed on dehydrated alcohol and deionized water
Ultrasonic treatment falls carbon cloth surfaces impurity in solvent, then is transferred into vacuum drying oven dry；
Step (2): in deionized water with the ratio dissolution of 1:3:0 by ammonium molybdate, thiocarbamide and DEXTROSE ANHYDROUS, at ultrasound
Reason 20min keeps Dispersion of Solute Matter uniform；Then carbon cloth obtained in above-mentioned solution and step (1) is transferred in autoclave
32h is reacted at 180 DEG C, after autoclave is cooling, carbon cloth is taken out and uses dehydrated alcohol and deionized water washing by soaking respectively
For several times, it is transferred to drying in vacuum oven, obtains molybdenum disulfide/carbon cloth material；
Step (3): by active material sublimed sulfur, binder polyacrylic acid and conductive agent single wall CNTs with the ratio of 6:2:2
Be dissolved in organic solvent dimethyl sulfoxide, stir evenly and be warming up to 160 DEG C until solute it is evenly dispersed, above-mentioned solution is added dropwise
On molybdenum disulfide/carbon cloth in step (2)；It is then placed into vacuum drying oven and is dried to obtain molybdenum disulfide/carbon cloth-sulphur anode
Material.
For the battery that 3 final product of embodiment is assembled under 0.2C current density, first circle discharge capacity is 432.5mAh/g,
402.3mAh/g, coulombic efficiency 96.38% are maintained at by the charge and discharge cycles capacity of 200 circles.
Embodiment 4
Step (1): by 32K, T700,70g/m2Plain weave carbon cloth carbon cloth be first placed on the molten of dehydrated alcohol and deionized water
Ultrasonic treatment falls carbon cloth surfaces impurity in agent, then is transferred into vacuum drying oven dry；
Step (2): in deionized water with the ratio dissolution of 1:5:0.5 by sodium molybdate, thiocarbamide and DEXTROSE ANHYDROUS, ultrasound
Processing 10min keeps Dispersion of Solute Matter uniform；Carbon cloth obtained in above-mentioned solution and step (1) is then transferred to autoclave
In react 12h at 240 DEG C, after autoclave is cooling, takes out carbon cloth and washed respectively with dehydrated alcohol and deionized water immersion
It washs for several times, is transferred in vacuum oven and is dried to obtain molybdenum disulfide/carbon cloth material；
Step (3): by active material sublimed sulfur, binder polyacrylic acid and conductive agent multi wall CNTs with the ratio of 7:1:2
Be dissolved in organic solvent dimethyl sulfoxide, stir evenly and be warming up to 140 DEG C until solute it is evenly dispersed, above-mentioned solution is added dropwise
On molybdenum disulfide/carbon cloth in step (2)；It is then placed into vacuum drying oven and is dried to obtain molybdenum disulfide/carbon cloth-sulphur anode
Material.
For the battery that 4 final product of embodiment is assembled under 0.2C current density, first circle discharge capacity is 501.8mAh/g,
469.1mAh/g, coulombic efficiency 97.63% are maintained at by the charge and discharge cycles capacity of 200 circles.
Embodiment 5
Step (1): by 1K, T300,200g/m2Twill carbon cloth carbon cloth be first placed on the molten of dehydrated alcohol and deionized water
Ultrasonic treatment falls carbon cloth surfaces impurity in agent, then is transferred into vacuum drying oven dry；
Step (2): in deionized water with the ratio dissolution of 1:3:1 by sodium molybdate, sulphur source and anhydrous oxalic acid, ultrasonic treatment
15min keeps Dispersion of Solute Matter uniform；Then carbon cloth obtained in above-mentioned solution and step (1) is transferred in autoclave
20h is reacted at 220 DEG C, after autoclave is cooling, carbon cloth is taken out and uses dehydrated alcohol and deionized water washing by soaking number respectively
It is secondary, it is transferred to drying in vacuum oven, obtains molybdenum disulfide/carbon cloth material；
Step (3): by active material sublimed sulfur, binder polyacrylic acid and conductive agent Nano titanium nitride with the ratio of 6:2:2
Example be dissolved in organic solvent dimethyl sulfoxide, stir evenly and be warming up to 155 DEG C until solute it is evenly dispersed, above-mentioned solution is dripped
It is added on molybdenum disulfide/carbon cloth in step (2)；It is then placed into vacuum drying oven and is being dried to obtain molybdenum disulfide/carbon cloth-sulphur
Positive electrode.
For the battery that 5 final product of embodiment is assembled under 0.2C current density, first circle discharge capacity is 957.4mAh/g,
846.1mAh/g is maintained at by the charge and discharge cycles capacity of 200 circles, and coulombic efficiency is close to 100%.
Embodiment 6
Step (1): by 1K, T300,120g/m2Twill carbon cloth carbon cloth be first placed on the molten of dehydrated alcohol and deionized water
Ultrasonic treatment falls carbon cloth surfaces impurity in agent, then is transferred into vacuum drying oven dry；
Step (2): in deionized water with the ratio dissolution of 1:3.5:1 by ammonium molybdate, sulphur source and DEXTROSE ANHYDROUS, ultrasound
Processing 15min keeps Dispersion of Solute Matter uniform；Carbon cloth obtained in above-mentioned solution and step (1) is then transferred to autoclave
In react 20h at 220 DEG C, after autoclave is cooling, takes out carbon cloth and washed respectively with dehydrated alcohol and deionized water immersion
It washs for several times, is transferred to drying in vacuum oven, obtains molybdenum disulfide/carbon cloth material；
Step (3): by active material sublimed sulfur, binder polyacrylic acid and conductive agent Nano titanium nitride with the ratio of 7:1:2
Example be dissolved in organic solvent dimethyl sulfoxide, stir evenly and be warming up to 140 DEG C until solute it is evenly dispersed, above-mentioned solution is dripped
It is added on molybdenum disulfide/carbon cloth in step (2)；It is then placed into vacuum drying oven and is being dried to obtain molybdenum disulfide/carbon cloth-sulphur
Positive electrode.
For the battery that 6 final product of embodiment is assembled under 0.2C current density, first circle discharge capacity is 876.5mAh/g, warp
The charge and discharge cycles capacity for crossing 200 circles is maintained at 816.3mAh/g, coulombic efficiency 98.9%.
Claims (10)
1. a kind of using carbon cloth as the lithium sulfur battery anode material of substrate, characterized in that the lithium sulfur battery anode material includes carbon
Cloth, active material, binder and conductive agent, growth has molybdenum disulfide nano sheet, the active material, binder on the carbon cloth
It is coated on the carbon cloth with conductive agent.
2. according to claim 1 using carbon cloth as the lithium sulfur battery anode material of substrate, which is characterized in that the active matter
Matter is sublimed sulfur；The binder is polyacrylic acid；The conductive agent is Super P, single wall CNTs, multi wall CNTs or nanometer nitrogen
Change one of titanium.
3. according to claim 2 using carbon cloth as the lithium sulfur battery anode material of substrate, which is characterized in that with the material
Gross mass is 100% meter, and the mass fraction of the molybdenum disulfide is 15~30%, the mass fraction of the sublimed sulfur is 7.5~
20%, the mass fraction of the polyacrylic acid is 2~3%, and the mass fraction of the conductive agent is 2~5%, remaining is carbon cloth.
4. according to claim 1 using carbon cloth as the lithium sulfur battery anode material of substrate, which is characterized in that the carbon cloth rule
Lattice are 1~32K, and the plain weave or twill carbon cloth of T300, T700, surface density is 70~200g/m2。
5. as described in Claims 1 to 4 is any using carbon cloth as the preparation method of the lithium sulfur battery anode material of substrate, feature
It is to include the following steps:
(1) carbon cloth is first placed in dehydrated alcohol and deionized water, ultrasonic treatment falls carbon cloth surfaces impurity, then is transferred into
It is dry in vacuum drying oven；
(2) in deionized water by the dissolution of molybdenum source, sulphur source and reducing agent, ultrasonic treatment keeps Dispersion of Solute Matter uniform；It then will be above-mentioned
Carbon cloth obtained in solution and the step (1), which is transferred in autoclave, carries out hydro-thermal reaction, cooling to autoclave
Afterwards, take out carbon cloth be transferred in vacuum oven with dehydrated alcohol and deionized water washing by soaking, be dried to obtain molybdenum disulfide/
Carbon cloth material；
(3) active material, binder and conductive agent are dissolved in organic solvent dimethyl sulfoxide, are stirred evenly, and heated up,
Until solute is evenly dispersed, above-mentioned solution is coated on molybdenum disulfide/carbon cloth in the step (2)；It is then placed into true
It is dry in empty baking oven, obtain the lithium sulfur battery anode material that carbon cloth is substrate.
6. according to right want 5 described in using carbon cloth as the preparation method of the lithium sulfur battery anode material of substrate, which is characterized in that institute
Stating molybdenum source in step (2) is sodium molybdate or ammonium molybdate, and sulphur source is thiocarbamide, and reducing agent is anhydrous oxalic acid or DEXTROSE ANHYDROUS.
7. according to right want 5 described in using carbon cloth as the preparation method of the lithium sulfur battery anode material of substrate, which is characterized in that institute
The molar ratio for stating molybdenum source, sulphur source and reducing agent in step (2) is respectively 1:(3~5): (0~1).
8. according to right want 5 described in using carbon cloth as the preparation method of the lithium sulfur battery anode material of substrate, which is characterized in that institute
It states in step (2), hydrothermal temperature is 180~240 DEG C, and the reaction time is 12~32h.
9. according to right want 5 described in using carbon cloth as the preparation method of the lithium sulfur battery anode material of substrate, which is characterized in that institute
It states in step (2), the time of the ultrasonic treatment is 10~30min.
10. according to right want 5 described in using carbon cloth as the preparation method of the lithium sulfur battery anode material of substrate, which is characterized in that
In the step (3), the ratio of active material, binder and conductive agent is (6~7): (1~2): 2；In the heating step,
Temperature is 140~160 DEG C.
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| CN110550660A (en) * | 2019-09-04 | 2019-12-10 | 江苏理工学院 | preparation method of tungsten disulfide/MXene composite material |
| CN111211329A (en) * | 2020-01-15 | 2020-05-29 | 重庆工商大学 | Water candle cattail-shaped MoS2Carbon nanofiber composite material and preparation method and application thereof |
| CN111370673A (en) * | 2020-03-23 | 2020-07-03 | 合肥工业大学 | Self-supporting lithium-sulfur battery cathode material with hierarchical structure and preparation method thereof |
| CN111403709A (en) * | 2020-03-26 | 2020-07-10 | 上海理工大学 | Flexible integrated three-dimensional carbon-based metal lithium negative electrode material, preparation method and application thereof |
| CN112436151A (en) * | 2020-11-13 | 2021-03-02 | 昆明理工大学 | Preparation method of lithium-sulfur battery current collector |
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