CN107749468A - A kind of preparation method and application of carbon nano-fiber with multilevel hierarchy, metal phase molybdenum disulfide and sulphur composite - Google Patents
A kind of preparation method and application of carbon nano-fiber with multilevel hierarchy, metal phase molybdenum disulfide and sulphur composite Download PDFInfo
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Abstract
The preparation method and application of a kind of carbon nano-fiber with multilevel hierarchy, metal phase molybdenum disulfide and sulphur composite, belongs to technical field of energy material.Methods described is as follows：1st, ammonium molybdate, L cysteines and sodium borohydride are dissolved in mixed solution, are put into carbon nano-fiber, are transferred in ptfe autoclave, hydro-thermal reaction, naturally cooled to room temperature, be dried overnight in baking oven；2nd, weigh 200 400mg sulphur powders to be dissolved into 5mL carbon disulfide, the material that step 1 is obtained is impregnated into sulphur solution, is taken out, and vacuum drying, heating and calcining, that is, obtains the carbon nano-fiber, metal phase molybdenum disulfide and sulphur composite with multilevel hierarchy.It is an advantage of the invention that：It is advantageously implemented the efficient utilization of sulphur and obtains the lithium-sulfur cell of stable circulation.Carbon nano-fiber and metal phase molybdenum disulfide composite with multilevel hierarchy can be prepared by simple one step hydro thermal method, and simple and easy, composition is controllable.
Description
Technical field
The invention belongs to technical field of energy material, and in particular to a kind of carbon nano-fiber with multilevel hierarchy, metal
The preparation method and application of phase molybdenum disulfide 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 material specific capacities such as lithium, LiMn2O4, lithium ion battery can not meet the needs of present.Seek a kind of more Fabrication of High Specific Capacitance
The secondary cell of amount 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.Multilevel structure material is used in electro-catalysis and energy field simultaneously
Way is extensive, but tradition constructs multilevel hierarchy method cumbersome tediously long, big energy-consuming mostly, is unfavorable for preparing on a large scale, preparation has
The polar material of multilevel hierarchy can effectively lift the performance of lithium-sulfur cell.
The content of the invention
The invention aims to solve shuttle effect problem serious existing for current lithium-sulfur cell, there is provided one kind tool
There is the preparation method and application of the carbon nano-fiber of multilevel hierarchy, metal phase molybdenum disulfide and sulphur composite.
To achieve the above object, the technical scheme that the present invention takes is as follows：
The preparation method of a kind of carbon nano-fiber with multilevel hierarchy, metal phase molybdenum disulfide and sulphur composite, the side
Method step is as follows：
Step 1：182 mg ammonium molybdates, 304 mg Cys and 113 ~ 452 mg sodium borohydrides are dissolved in into 70mL to mix
In solution, ultrasonic dissolution 30min, it is put into carbon nano-fiber and continues ultrasonic 30min, then will be put into the mixing of carbon nano-fiber
Solution is transferred in ptfe autoclave, hydro-thermal 24h at a temperature of 180 DEG C, naturally cools to room temperature, takes out carbon Nanowire
Dimension, is washed with water and ethanol, is dried overnight in 70 DEG C of baking ovens, that is, obtain the carbon nano-fiber and metal with multilevel hierarchy successively
Phase molybdenum disulfide composite；
Step 2：Weigh 200-400mg sulphur powders to be dissolved into 5mL carbon disulfide, there is multilevel hierarchy by prepared by step 1
Carbon nano-fiber and metal phase molybdenum disulfide composite are impregnated into sulphur solution, make the load capacity of sulphur in 1.5-3.0mg cm-2）, take out after 5min, be dried in vacuo at a temperature of 40 DEG C, then the heating and calcining 12h at a temperature of 155 DEG C, that is, obtain that there is multistage
Carbon nano-fiber, metal phase molybdenum disulfide and the sulphur composite of structure.
The carbon nano-fiber with multilevel hierarchy, metal phase molybdenum disulfide and the sulphur that a kind of above method is prepared are compound
Application of the material in lithium-sulphur cell positive electrode.
It is of the invention to be relative to the beneficial effect of prior art：
（1）Metal phase molybdenum disulfide has good more lithium sulfide adsorption capacities, can lift the stability of lithium-sulfur cell.
（2）Metal phase molybdenum disulfide has good electric conductivity in itself, and absorption and conversion reaction can be simultaneously in metal phases
Molybdenum disulfide surface occurs.
（3）Carbon nano-fiber avoids cumbersome and binding agent the use of electrode material preparation technology as collector.
（4）Preparing raw material cost is low, and manufacture craft is simple, preparation process clean environment firendly, is advantageous to the reality of lithium-sulfur cell
Using.
（5）Molybdenum disulfide with multilevel hierarchy is with the strong suction-operated to polysulfide, and electric conductivity itself is strong, absorption
Binding agent can be reduced with conversion as collector in metal phase molybdenum disulfide surface conversion, next carbon nano-fiber simultaneously
Use, so as to improve electrode material monolithic conductive, be advantageously implemented sulphur efficient utilization and obtain stable circulation lithium
Sulphur battery.Carbon nano-fiber and metal phase molybdenum disulfide composite with multilevel hierarchy can pass through simple step hydro-thermal
Prepared by method, simple and easy, composition is controllable.
（6）Carbon nano-fiber with multilevel hierarchy, metal phase molybdenum disulfide and sulphur composite are because 5 points with more than
Advantage, show outstanding cyclical stability.
Brief description of the drawings
Fig. 1 is the SEM figures of carbon nano-fiber and metal phase molybdenum disulfide with multilevel hierarchy.
Fig. 2 is charging and discharging curve figure of the button cell of assembling under 0.2C.
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 multilevel hierarchy, metal phase
The preparation method of molybdenum disulfide and sulphur composite, methods described step are as follows：
Step 1：182 mg ammonium molybdates, 304 mg Cys and 113 ~ 452mg sodium borohydrides are dissolved in into 70mL to mix
In solution, ultrasonic dissolution 30min, it is put into carbon nano-fiber and continues ultrasonic 30min, then will be put into the mixing of carbon nano-fiber
Solution is transferred in ptfe autoclave, hydro-thermal 24h at a temperature of 180 DEG C, naturally cools to room temperature, takes out carbon Nanowire
Dimension, is washed with water and ethanol, is dried overnight in 70 DEG C of baking ovens, that is, obtain the carbon nano-fiber and metal with multilevel hierarchy successively
Phase molybdenum disulfide composite；
Step 2：Weigh 200-400mg sulphur powders to be dissolved into 5mL carbon disulfide, there is multilevel hierarchy by prepared by step 1
Carbon nano-fiber and metal phase molybdenum disulfide composite are impregnated into sulphur solution, make the load capacity of sulphur in 1.5-3.0mg cm-2）, take out after 5min, be dried in vacuo at a temperature of 40 DEG C, then the heating and calcining 12h at a temperature of 155 DEG C, that is, obtain that there is multistage
Carbon nano-fiber, metal phase molybdenum disulfide and the sulphur composite of structure.
Embodiment two：A kind of carbon nano-fiber with multilevel hierarchy, metal described in embodiment one
The preparation method of phase molybdenum disulfide and sulphur composite, in step 1, described mixed solution is by DMF and water according to 1.5:1
Volume ratio forms.
Embodiment three：A kind of carbon nano-fiber with multilevel hierarchy, metal described in embodiment one
The preparation method of phase molybdenum disulfide and sulphur composite, in step 1, described carbon nano-fiber and metal phase molybdenum disulfide are answered
The pattern of condensation material is the smooth nanometer sheet multilevel hierarchy in surface.
Embodiment four：Any embodiment methods described is prepared into a kind of embodiment one to three
To the carbon nano-fiber with multilevel hierarchy, metal phase molybdenum disulfide and sulphur composite in lithium-sulphur cell positive electrode should
With.
Embodiment five：The carbon nano-fiber with multilevel hierarchy, metal phase two described in embodiment four
The application of molybdenum sulfide and sulphur composite in lithium-sulphur cell positive electrode, concrete application are as follows：By carbon nano-fiber, the sulphur of metal phase two
Change molybdenum and sulphur composite directly as lithium sulfur battery anode material.
Embodiment 1：
（1）Take 182 mg ammonium molybdates, 304 mg Cys and 113 mg sodium borohydride are dissolved into 70mL mixed solvents
In（Volume ratio is DMF:H2O=1.5:1）, ultrasonic dissolution 30 minutes, it is put into a diameter of 1cm carbon nano-fiber continuation ultrasonic 30
Minute, transfer the solution into 100mL ptfe autoclaves, 180 DEG C of hydro-thermals 24 hours, room temperature is naturally cooled to, by carbon
Nanofiber is taken out, and washing ethanol is washed, and is dried overnight in 70 DEG C of baking ovens, is obtained carbon nano-fiber and metal phase molybdenum disulfide is answered
Condensation material；
（2）Weigh 200mg sulphur powders to be dissolved into 5mL carbon disulfide, by the mesoporous carbon nano-fiber of preparation and metal phase curing
Molybdenum 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, there is carbon nano-fiber, metal phase molybdenum disulfide and sulphur composite by obtaining.
Embodiment 2：
（1）Take 182 mg ammonium molybdates, 304 mg Cys and 226 mg sodium borohydride are dissolved into 70mL mixed solvents
In（Volume ratio is DMF:H2O=1.5:1）, ultrasonic dissolution 30 minutes, it is put into a diameter of 1cm carbon nano-fiber continuation ultrasonic 30
Minute, transfer the solution into 100mL ptfe autoclaves, 180 DEG C of hydro-thermals 24 hours, room temperature is naturally cooled to, by carbon
Nanofiber is taken out, and washing ethanol is washed, and is dried overnight in 70 DEG C of baking ovens, is obtained carbon nano-fiber and metal phase molybdenum disulfide is answered
Condensation material；
（2）Weigh 200mg sulphur powders to be dissolved into 5mL carbon disulfide, by the mesoporous carbon nano-fiber of preparation and metal phase curing
Molybdenum 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, there is carbon nano-fiber, metal phase molybdenum disulfide and sulphur composite by obtaining.
Embodiment 3：
（1）Take 182 mg ammonium molybdates, 304 mg Cys and 339 mg sodium borohydride are dissolved into 70mL mixed solvents
In（Volume ratio is DMF:H2O=1.5:1）, ultrasonic dissolution 30 minutes, it is put into a diameter of 1cm carbon nano-fiber continuation ultrasonic 30
Minute, transfer the solution into 100mL ptfe autoclaves, 180 DEG C of hydro-thermals 24 hours, room temperature is naturally cooled to, by carbon
Nanofiber is taken out, and washing ethanol is washed, and is dried overnight in 70 DEG C of baking ovens, is obtained carbon nano-fiber and metal phase molybdenum disulfide is answered
Condensation material；
（2）Weigh 200mg sulphur powders to be dissolved into 5mL carbon disulfide, by the mesoporous carbon nano-fiber of preparation and metal phase curing
Molybdenum 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, there is carbon nano-fiber, metal phase molybdenum disulfide and sulphur composite by obtaining.
Embodiment 4：
（1）Take 182 mg ammonium molybdates, 304 mg Cys and 452 mg sodium borohydride are dissolved into 70mL mixed solvents
In（Volume ratio is DMF:H2O=1.5:1）, ultrasonic dissolution 30 minutes, it is put into a diameter of 1cm carbon nano-fiber continuation ultrasonic 30
Minute, transfer the solution into 100mL ptfe autoclaves, 180 DEG C of hydro-thermals 24 hours, room temperature is naturally cooled to, by carbon
Nanofiber is taken out, and washing ethanol is washed, and is dried overnight in 70 DEG C of baking ovens, is obtained carbon nano-fiber and metal phase molybdenum disulfide is answered
Condensation material；
（2）Weigh 200mg sulphur powders to be dissolved into 5mL carbon disulfide, by the mesoporous carbon nano-fiber of preparation and metal phase curing
Molybdenum 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, there is carbon nano-fiber, metal phase molybdenum disulfide and sulphur composite by obtaining.
Embodiment 5：
（1）Take 182 mg ammonium molybdates, 304 mg Cys and 113 mg sodium borohydride are dissolved into 70mL mixed solvents
In（Volume ratio is DMF:H2O=1.5:1）, ultrasonic dissolution 30 minutes, it is put into a diameter of 1cm carbon nano-fiber continuation ultrasonic 30
Minute, transfer the solution into 100mL ptfe autoclaves, 180 DEG C of hydro-thermals 24 hours, room temperature is naturally cooled to, by carbon
Nanofiber is taken out, and washing ethanol is washed, and is dried overnight in 70 DEG C of baking ovens, is obtained carbon nano-fiber and metal phase molybdenum disulfide is answered
Condensation material；
（2）Weigh 300mg sulphur powders to be dissolved into 5mL carbon disulfide, by the mesoporous carbon nano-fiber of preparation and metal phase curing
Molybdenum 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, there is carbon nano-fiber, metal phase molybdenum disulfide and sulphur composite by obtaining.
Embodiment 6：
（1）Take 182 mg ammonium molybdates, 304 mg Cys and 113 mg sodium borohydride are dissolved into 70mL mixed solvents
In（Volume ratio is DMF:H2O=1.5:1）, ultrasonic dissolution 30 minutes, it is put into a diameter of 1cm carbon nano-fiber continuation ultrasonic 30
Minute, transfer the solution into 100mL ptfe autoclaves, 180 DEG C of hydro-thermals 24 hours, room temperature is naturally cooled to, by carbon
Nanofiber is taken out, and washing ethanol is washed, and is dried overnight in 70 DEG C of baking ovens, is obtained carbon nano-fiber and metal phase molybdenum disulfide is answered
Condensation material；
（2）Weigh 400mg sulphur powders to be dissolved into 5mL carbon disulfide, by the mesoporous carbon nano-fiber of preparation and metal phase curing
Molybdenum 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, there is carbon nano-fiber, metal phase molybdenum disulfide and sulphur composite by obtaining.
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 the SEM figures of carbon nano-fiber and metal phase molybdenum disulfide with multilevel hierarchy, in it can be seen from the figure that carbon
Nanofiber and metal phase molybdenum disulfide are the flaky materials for having meso-hole structure, have abundant surface to be contacted with sulphur.
Fig. 2 is charging and discharging curve of the button cell of assembling under 0.2C, and capacity is up to 1000mAh/g, circulation 100 first
After circle, capacity is retained in 800 mAh/g.
Claims (5)
1. the preparation method of a kind of carbon nano-fiber with multilevel hierarchy, metal phase molybdenum disulfide and sulphur composite, it is special
Sign is：Methods described step is as follows：
Step 1：182 mg ammonium molybdates, 304 mg Cys and 113 ~ 452 mg sodium borohydrides are dissolved in into 70mL to mix
In solution, ultrasonic dissolution 30min, it is put into carbon nano-fiber and continues ultrasonic 30min, then will be put into the mixing of carbon nano-fiber
Solution is transferred in ptfe autoclave, hydro-thermal 24h at a temperature of 180 DEG C, naturally cools to room temperature, takes out carbon Nanowire
Dimension, is washed with water and ethanol, is dried overnight in 70 DEG C of baking ovens, that is, obtain the carbon nano-fiber and metal with multilevel hierarchy successively
Phase molybdenum disulfide composite；
Step 2：Weigh 200-400mg sulphur powders to be dissolved into 5mL carbon disulfide, there is multilevel hierarchy by prepared by step 1
Carbon nano-fiber and metal phase molybdenum disulfide composite are impregnated into sulphur solution, make the load capacity of sulphur in 1.5-3.0mg cm-2）, take out after 5min, be dried in vacuo at a temperature of 40 DEG C, then the heating and calcining 12h at a temperature of 155 DEG C, that is, obtain that there is multistage
Carbon nano-fiber, metal phase molybdenum disulfide and the sulphur composite of structure.
2. a kind of carbon nano-fiber with multilevel hierarchy according to claim 1, metal phase molybdenum disulfide and sulphur are compound
The preparation method of material, it is characterised in that：In step 1, described mixed solution is by DMF and water according to 1.5:1 volume ratio group
Into.
3. a kind of carbon nano-fiber with multilevel hierarchy according to claim 1, metal phase molybdenum disulfide and sulphur are compound
The preparation method of material, it is characterised in that：In step 1, described carbon nano-fiber and metal phase molybdenum disulfide composite
Pattern is the smooth nanometer sheet multilevel hierarchy in surface.
4. the carbon Nanowire with multilevel hierarchy that a kind of method in claim 1 ~ 3 described in any claim is prepared
Dimension, the application of metal phase molybdenum disulfide and sulphur composite in lithium-sulphur cell positive electrode.
5. the carbon nano-fiber according to claim 4 with multilevel hierarchy, metal phase molybdenum disulfide and sulphur composite
Application in lithium-sulphur cell positive electrode, it is characterised in that：Concrete application is as follows：By carbon nano-fiber, metal phase molybdenum disulfide and
Sulphur composite is directly as lithium sulfur battery anode material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108550813A (en) * | 2018-04-16 | 2018-09-18 | 清华大学深圳研究生院 | A kind of lithium sulfur battery anode material and preparation method, lithium-sulfur cell |
| CN109647442A (en) * | 2018-12-25 | 2019-04-19 | 中国石油天然气股份有限公司 | Completely vulcanized hydrofining catalyst, preparation method thereof and distillate oil hydrofining method |
| CN111293293A (en) * | 2020-02-19 | 2020-06-16 | 中国科学技术大学 | Molybdenum disulfide nanotube/sulfur composite cathode material with increased interlayer spacing and preparation method and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102201567A (en) * | 2011-04-18 | 2011-09-28 | 武汉工程大学 | Preparation method for anode of lithium-sulfur battery |
| CN102683659A (en) * | 2012-05-31 | 2012-09-19 | 中国科学院物理研究所 | Lithium-sulphur battery anode material and preparation method thereof |
| CN104056642A (en) * | 2014-05-19 | 2014-09-24 | 浙江理工大学 | Preparation method of molybdenum disulfide/carbon nano-fiber hybrid material |
| CN104201392A (en) * | 2014-08-20 | 2014-12-10 | 中南大学 | Preparation method of lithium-sulphur battery electrode |
| CN105293581A (en) * | 2015-10-25 | 2016-02-03 | 复旦大学 | Molybdenum sulfide/graphene/carbon nanoball composite material and preparing method thereof |
| CN105529448A (en) * | 2016-01-22 | 2016-04-27 | 西北工业大学 | Preparation method for flexible lithium ion battery cathode material |
| CN106311282A (en) * | 2016-08-09 | 2017-01-11 | 河南工程学院 | Preparing method of porous monocrystal IT MoS2 nanosheet and application thereof |
| CN106904580A (en) * | 2017-03-09 | 2017-06-30 | 哈尔滨工业大学 | Using the method for the two-dimensional nano piece of hydro-thermal method synthesis 1T phase degree of disorder coordinated regulations |
-
2017
- 2017-09-26 CN CN201710884097.0A patent/CN107749468A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102201567A (en) * | 2011-04-18 | 2011-09-28 | 武汉工程大学 | Preparation method for anode of lithium-sulfur battery |
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