CN107768620A - A kind of carbon nano-fiber with heterojunction structure, stannic disulfide, the preparation method and application of tin ash and sulphur composite - Google Patents
A kind of carbon nano-fiber with heterojunction structure, stannic disulfide, the preparation method and application of tin ash and sulphur composite Download PDFInfo
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Abstract
A kind of carbon nano-fiber with heterojunction structure, stannic disulfide, the preparation method and application of tin ash and sulphur composite, belong to technical field of energy material.Methods described is as follows：1st, butter of tin, thioacetamide, carbon nano-fiber are dissolved in poly- propyl alcohol, carry out hydro-thermal reaction, that is, obtain the carbon nano-fiber, stannic disulfide and tin dioxide composite material with heterojunction structure；2nd, the composite for obtaining step 1 is impregnated into sulphur solution, is taken out after 5min, vacuum drying, high-temperature calcination, obtains having the carbon nano-fiber of heterojunction structure, stannic disulfide, tin ash and sulphur composite.It is an advantage of the invention that：Existing special interfacial effect can be effectively increased electrode surface electronics and ion transport speed to composite in itself, be advantageously implemented the efficient utilization of sulphur and obtain the lithium-sulfur cell of stable circulation.Composite can be prepared directly using one step hydro thermal method, and simple and easy, composition is controllable.
Description
Technical field
The invention belongs to technical field of energy material, more particularly to a kind of carbon nano-fiber with heterojunction structure, two
The preparation method and application of artificial gold, tin ash and sulphur composite.
Background technology
It is more urgent to the demand of high-specific energy battery with the development of portable electronic industry, it is limited to traditional cobalt acid
The restriction of the specific capacity of the materials such as lithium, LiMn2O4, lithium ion battery can not meet the needs of present.Seek a kind of higher ratio
The secondary cell of capacity is imperative.Lithium-sulfur cell was paid attention to by researcher in the last few years, because its specific capacity is high
（1675mAh/g）, the advantages that cost is low, elemental sulfur source is wide, nontoxic, get a good chance of the secondary electricity as high-energy-density of future generation
Pond body system.
But the commercial applications that still there are many difficulties to govern lithium-sulfur cell at present, such as：（1）Elemental sulfur is not
Conduction, influence the chemical property of whole battery；（2）Discharge potential is than relatively low, only 2.1V；（3）Discharge the more sulphur of intermediate product
Change lithium and be soluble in ethers electrolyte（Shuttle effect）, cause sulphur to move to negative terminal surface by electrolyte, reduce battery life；
（4）Elemental sulfur discharge process volumetric expansion is serious, from elemental lithium as negative material, potential safety hazard be present.In problem above
The problem of dissolving of more lithium sulfides is the maximum to be solved at present.
The method for generally solving shuttle effect is compound from a kind of carbon material and elemental sulfur, among elemental sulfur and electric discharge
Product is wrapped in the duct of carbon material.But recent studies suggest that, carbon material belongs to nonpolar molecule, between more lithium sulfides
The effect of chemisorbed can not be formed, causes the DeGrain for suppressing shuttle effect.Based on such a viewpoint, researcher selects again
The surface texture of element doping modified carbonaceous components is taken, but the avtive spot adulterated is limited.Recently, polar molecule is as lithium sulphur electricity
The research of pond positive electrode turns into the focus for suppressing shuttle effect.But how the emphasis of researcher's concern mainly suppresses to wear
Shuttle effect, and few people go consider catalysis lithium-sulfur cell discharge process extent of reaction problem, if accelerate more lithium sulfides to
The transfer process of lithium sulfide, it can also suppress the dissolving of more lithium sulfides indirectly, so as to lift the cycle performance of lithium-sulfur cell.
The content of the invention
The invention aims to solve the problems, such as more lithium sulfide shuttle effects present in lithium-sulfur cell, there is provided a kind of
The preparation method and application of carbon nano-fiber, stannic disulfide, tin ash and sulphur composite with heterojunction structure.
To achieve the above object, the technical scheme that the present invention takes is as follows：
A kind of carbon nano-fiber with heterojunction structure, stannic disulfide, the preparation method of tin ash and sulphur composite, institute
It is as follows to state method and step：
Step 1：16 mg thioacetamides are taken, 32-80 mg butters of tin are dissolved into 10mL isopropanols, are added a diameter of
1cm carbon nano-fiber, in 180 DEG C of hydro-thermal reactions 24 hours, room temperature is naturally cooled to, is dried overnight at a temperature of 70 DEG C, i.e.,
Obtain the carbon nano-fiber, stannic disulfide and tin dioxide composite material with heterojunction structure；
Step 2：Take 200 ~ 400mg sulphur powders to be dissolved in 5mL carbon disulfide, obtain sulphur solution, step 1 is had into hetero-junctions
Carbon nano-fiber, stannic disulfide and the tin dioxide composite material of structure are impregnated into sulphur solution, make the load capacity of sulphur in 1.5-
3.0mg cm-2In, take out after 5min, be dried in vacuo at a temperature of 40 DEG C, in 155 DEG C of temperature lower calcination 12h, obtain having heterogeneous
Carbon nano-fiber, stannic disulfide, tin ash and the sulphur composite of junction structure.
Carbon nano-fiber, stannic disulfide, tin ash and the sulphur composite that a kind of above method is prepared are in lithium sulphur
Application in anode.
Compared with prior art, the present invention has the advantages that：
（1）Stannic disulfide and tin dioxide composite material have good more lithium sulfide adsorption capacities, can lift lithium-sulfur cell
Stability.
（2）Stannic disulfide and tin dioxide composite material have good catalytic activity, can promote more lithium sulfides to sulphur
Change the transformation of lithium, be catalyzed lithium-sulfur cell discharge process, reduce the dissolving of more lithium sulfides.
（3）Stannic disulfide and tin dioxide composite material with heterojunction structure, can be effectively increased electrode material table
The electronic and ionic transfer rate in face, so as to promote the transformation of lithium-sulfur cell redox reaction.
（4）Carbon nano-fiber avoids cumbersome and binding agent the use of electrode material preparation technology as collector,
So as to improve electrode material monolithic conductive.Preparing raw material cost is low, and manufacture craft is simple, preparation process clean environment firendly, favorably
In the practical application of lithium-sulfur cell.
（5）Existing special interfacial effect can be with itself for the stannic disulfide and tin dioxide composite material of heterojunction structure
Electrode surface electronics and ion transport speed are effectively increased, the efficient utilization of sulphur is advantageously implemented and obtains the lithium of stable circulation
Sulphur battery.Carbon nano-fiber, stannic disulfide and tin dioxide composite material with heterojunction structure can directly utilize a step
Prepared by hydro-thermal method, simple and easy, composition is controllable.
Brief description of the drawings
Fig. 1 is that the SEM of the carbon nano-fiber with heterojunction structure, stannic disulfide and tin dioxide composite material schemes.
Fig. 2 is charging and discharging curve figure of the button cell of assembling under different multiplying.
Fig. 3 is the button cell curve map that charge and discharge cycles 200 are enclosed in the case where current density is 0.5C and 1C multiplying powers of assembling.
Embodiment
Technical scheme is further described with reference to the accompanying drawings and examples, but is not limited thereto,
It is every technical solution of the present invention to be modified or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention,
It all should cover in protection scope of the present invention.
Embodiment one：What present embodiment was recorded is a kind of carbon nano-fiber with heterojunction structure, two sulphur
Change the preparation method of tin, tin ash and sulphur composite, methods described step is as follows：
Step 1：16 mg thioacetamides are taken, 32-80 mg butters of tin are dissolved into 10mL isopropanols, are added a diameter of
1cm carbon nano-fiber, in 180 DEG C of hydro-thermal reactions 24 hours, room temperature is naturally cooled to, is dried overnight at a temperature of 70 DEG C, i.e.,
Obtain the carbon nano-fiber, stannic disulfide and tin dioxide composite material with heterojunction structure；
Step 2：Take 200 ~ 400mg sulphur powders to be dissolved in 5mL carbon disulfide, obtain sulphur solution, step 1 is had into hetero-junctions
Carbon nano-fiber, stannic disulfide and the tin dioxide composite material of structure are impregnated into sulphur solution, make the load capacity of sulphur in 1.5-
3.0mg cm-2In, take out after 5min, be dried in vacuo at a temperature of 40 DEG C, in 155 DEG C of temperature lower calcination 12h, obtain having heterogeneous
Carbon nano-fiber, stannic disulfide, tin ash and the sulphur composite of junction structure.
Embodiment two：A kind of carbon nano-fiber with heterojunction structure described in embodiment one, two
The preparation method of artificial gold, tin ash and sulphur composite, the pattern of the carbon nano-fiber, stannic disulfide and tin ash
It is the nano-chip arrays structure with rough surface.
Embodiment three：Carbon nano-fiber that the methods described of embodiment one or two is prepared, curing
The application of tin, tin ash and sulphur composite in lithium-sulphur cell positive electrode.
Embodiment four：Carbon nano-fiber, stannic disulfide, tin ash and sulphur described in embodiment three are answered
Application of the condensation material in lithium-sulphur cell positive electrode, it is characterised in that：Concrete application is as follows：By carbon nano-fiber, stannic disulfide, two
Tin oxide and sulphur composite, without using binding agent, it is cumbersome to avoid electrode material directly as lithium sulfur battery anode material
Preparation technology.
Embodiment 1：
（1）16 mg thioacetamides are taken, 80 mg butters of tin are dissolved into 10mL isopropanols, ultrasonic dissolution 30 minutes, are put into
A diameter of 1cm carbon nano-fiber continues ultrasound 30 minutes, transfers the solution into 100mL ptfe autoclaves, 180 DEG C
Hydro-thermal 24 hours, naturally cools to room temperature, carbon nano-fiber is taken out, and washing ethanol is washed, and is dried overnight, is obtained in 70 DEG C of baking ovens
Tin dioxide composite material is closed to carbon nano-fiber, stannic disulfide；
（2）Weigh 200mg sulphur powders to be dissolved into 5mL carbon disulfide, by the carbon nano-fiber, stannic disulfide and titanium dioxide of preparation
Tin composite material is immersed in the solution of sulphur and taken out after about 5 minutes, is dried in vacuo at a temperature of 40 DEG C, separately at 155 DEG C
At a temperature of heating and calcining 12 hours, carbon nano-fiber, stannic disulfide, tin ash and sulphur with heterojunction structure will be obtained and answered
Condensation material.
Embodiment 2：
（1）16 mg thioacetamides are taken, 64 mg butters of tin are dissolved into 10mL isopropanols, ultrasonic dissolution 30 minutes, are put into
A diameter of 1cm carbon nano-fiber continues ultrasound 30 minutes, transfers the solution into 100mL ptfe autoclaves, 180 DEG C
Hydro-thermal 24 hours, naturally cools to room temperature, carbon nano-fiber is taken out, and washing ethanol is washed, and is dried overnight, is obtained in 70 DEG C of baking ovens
To carbon nano-fiber, stannic disulfide and tin dioxide composite material；
（2）Weigh 200mg sulphur powders to be dissolved into 5mL carbon disulfide, by the carbon nano-fiber, stannic disulfide and titanium dioxide of preparation
Tin composite material is immersed in the solution of sulphur and taken out after about 5 minutes, is dried in vacuo at a temperature of 40 DEG C, separately at 155 DEG C
At a temperature of heating and calcining 12 hours, carbon nano-fiber, stannic disulfide, tin ash and sulphur with heterojunction structure will be obtained and answered
Condensation material.
Embodiment 3：
（1）16 mg thioacetamides are taken, 48 mg butters of tin are dissolved into 10mL isopropanols, ultrasonic dissolution 30 minutes, are put into
A diameter of 1cm carbon nano-fiber continues ultrasound 30 minutes, transfers the solution into 100mL ptfe autoclaves, 180 DEG C
Hydro-thermal 24 hours, naturally cools to room temperature, carbon nano-fiber is taken out, and washing ethanol is washed, and is dried overnight, is obtained in 70 DEG C of baking ovens
To carbon nano-fiber, stannic disulfide and tin dioxide composite material；
（2）Weigh 200mg sulphur powders to be dissolved into 5mL carbon disulfide, by the carbon nano-fiber, stannic disulfide and titanium dioxide of preparation
Tin composite material is immersed in the solution of sulphur and taken out after about 5 minutes, is dried in vacuo at a temperature of 40 DEG C, separately at 155 DEG C
Heating and calcining 12 hours, carbon nano-fiber, stannic disulfide, tin ash and sulphur composite wood with heterojunction structure will be obtained
Material.
Embodiment 4：
（1）16 mg thioacetamides are taken, 32 mg butters of tin are dissolved into 10mL isopropanols, ultrasonic dissolution 30 minutes, are put into
A diameter of 1cm carbon nano-fiber continues ultrasound 30 minutes, transfers the solution into 100mL ptfe autoclaves, 180 DEG C
Hydro-thermal 24 hours, naturally cools to room temperature, carbon nano-fiber is taken out, and washing ethanol is washed, and is dried overnight, is obtained in 70 DEG C of baking ovens
To carbon nano-fiber, stannic disulfide and tin dioxide composite material；
（2）Weigh 200mg sulphur powders to be dissolved into 5mL carbon disulfide, by the carbon nano-fiber, stannic disulfide and titanium dioxide of preparation
Tin composite material is immersed in the solution of sulphur and taken out after about 5 minutes, is dried in vacuo at a temperature of 40 DEG C, separately at 155 DEG C
Heating and calcining 12 hours, carbon nano-fiber, stannic disulfide, tin ash and sulphur composite wood with heterojunction structure will be obtained
Material.
Embodiment 5：
（1）16 mg thioacetamides are taken, 32 mg butters of tin are dissolved into 10mL isopropanols, ultrasonic dissolution 30 minutes, are put into
A diameter of 1cm carbon nano-fiber continues ultrasound 30 minutes, transfers the solution into 100mL ptfe autoclaves, 180 DEG C
Hydro-thermal 24 hours, naturally cools to room temperature, carbon nano-fiber is taken out, and washing ethanol is washed, and is dried overnight, is obtained in 70 DEG C of baking ovens
To carbon nano-fiber, stannic disulfide and tin dioxide composite material；
（2）Weigh 300mg sulphur powders to be dissolved into 5mL carbon disulfide, by the carbon nano-fiber, stannic disulfide and titanium dioxide of preparation
Tin composite material is immersed in the solution of sulphur and taken out after about 5 minutes, is dried in vacuo at a temperature of 40 DEG C, separately at 155 DEG C
Heating and calcining 12 hours, carbon nano-fiber, stannic disulfide, tin ash and sulphur composite wood with heterojunction structure will be obtained
Material.
Embodiment 6：
（1）16 mg thioacetamides are taken, 32 mg butters of tin are dissolved into 10mL isopropanols, ultrasonic dissolution 30 minutes, are put into
A diameter of 1cm carbon nano-fiber continues ultrasound 30 minutes, transfers the solution into 100mL ptfe autoclaves, 180 DEG C
Hydro-thermal 24 hours, naturally cools to room temperature, carbon nano-fiber is taken out, and washing ethanol is washed, and is dried overnight, is obtained in 70 DEG C of baking ovens
To carbon nano-fiber, stannic disulfide and tin dioxide composite material；
（2）Weigh 400mg sulphur powders to be dissolved into 5mL carbon disulfide, by the carbon nano-fiber, stannic disulfide and titanium dioxide of preparation
Tin composite material is immersed in the solution of sulphur and taken out after about 5 minutes, is dried in vacuo at a temperature of 40 DEG C, separately at 155 DEG C
Heating and calcining 12 hours, carbon nano-fiber, stannic disulfide, tin ash and sulphur composite wood with heterojunction structure will be obtained
Material.
Embodiment 7：
The preparation and performance test of electrode：Due to, directly as collector, avoiding conventional electrode materials using carbon nano-fiber
The complicated processes of preparation and the use of binding agent, can be directly as lithium sulfur battery anode material.Lithium metal uses as negative pole
The model barrier films of Celgard 2400,1mol/L LiTFSI are dissolved in DOL/DME (volume ratios 1:1) it is electrolysed in solvent
Liquid, 1mol/L LiNO3Additive is done, button cell is assembled into glove box.Carried out using Neware ponds test system
Constant current charge-discharge test, charging/discharging voltage scope are 1.7 ~ 2.8 V.
Fig. 1 is that the SEM of the carbon nano-fiber with heterojunction structure, stannic disulfide and tin ash schemes, can be with figure
It is the laminated structure for having rough surface to find out carbon nano-fiber, stannic disulfide and tin ash, has abundant surface to be connect with sulphur
Touch.
Fig. 2 is charging and discharging curve of the button cell under different multiplying of assembling, and capacity is up to first under 0.2C
1558mAh/g, still there is 800 mAh/g capacity under 2C.
Fig. 3 is the button cell curve that charge and discharge cycles 200 are enclosed in the case where current density is 0.5C and 1C multiplying powers of assembling,
Discharge capacity is 1300mAh/g to 0.5C first, and discharge capacity is 1000mAh/g to 1C first, and after the circle of circulation 200, capacity does not almost have
There is decay.
Claims (4)
1. a kind of carbon nano-fiber with heterojunction structure, stannic disulfide, the preparation method of tin ash and sulphur composite,
It is characterized in that：Methods described step is as follows：
Step 1：16 mg thioacetamides are taken, 32-80 mg butters of tin are dissolved into 10mL isopropanols, are added a diameter of
1cm carbon nano-fiber, in 180 DEG C of hydro-thermal reactions 24 hours, room temperature is naturally cooled to, is dried overnight at a temperature of 70 DEG C, i.e.,
Obtain the carbon nano-fiber, stannic disulfide and tin dioxide composite material with heterojunction structure；
Step 2：Take 200 ~ 400mg sulphur powders to be dissolved in 5mL carbon disulfide, obtain sulphur solution, step 1 is had into hetero-junctions
Carbon nano-fiber, stannic disulfide and the tin dioxide composite material of structure are impregnated into sulphur solution, make the load capacity of sulphur in 1.5-
3.0mg cm-2In, take out after 5min, be dried in vacuo at a temperature of 40 DEG C, in 155 DEG C of temperature lower calcination 12h, obtain having heterogeneous
Carbon nano-fiber, stannic disulfide, tin ash and the sulphur composite of junction structure.
2. a kind of carbon nano-fiber with heterojunction structure, stannic disulfide, tin ash and sulphur according to claim 1
The preparation method of composite, it is characterised in that：The pattern of the carbon nano-fiber, stannic disulfide and tin ash is that have slightly
The nano-chip arrays structure on rough surface.
3. carbon nano-fiber, stannic disulfide, tin ash and the sulphur that a kind of methods described of claim 1 or 2 is prepared are compound
Application of the material in lithium-sulphur cell positive electrode.
4. carbon nano-fiber according to claim 3, stannic disulfide, tin ash and sulphur composite in lithium-sulfur cell just
Application in extremely, it is characterised in that：Concrete application is as follows：By carbon nano-fiber, stannic disulfide, tin ash and sulphur composite
Directly as lithium sulfur battery anode material.
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| CN114665074A (en) * | 2022-03-21 | 2022-06-24 | 西安航空学院 | Sn simple substance modified biological carbon/sulfur composite material and preparation method and application thereof |
| CN114725343A (en) * | 2022-04-19 | 2022-07-08 | 西安航空学院 | Nitrogen and sulfur co-doped biochar/SnO2SnS/S composite material, preparation method and application |
| CN115347173A (en) * | 2022-08-30 | 2022-11-15 | 陕西科技大学 | Three-dimensional bridged double-carbon-limited-domain tin oxide-based negative electrode material and preparation method and application thereof |
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