CN204424370U - A kind of preparation facilities for sulfur electrode material - Google Patents
A kind of preparation facilities for sulfur electrode material Download PDFInfo
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- CN204424370U CN204424370U CN201520031972.7U CN201520031972U CN204424370U CN 204424370 U CN204424370 U CN 204424370U CN 201520031972 U CN201520031972 U CN 201520031972U CN 204424370 U CN204424370 U CN 204424370U
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- stainless steel
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- electrode material
- preparation facilities
- sulfur electrode
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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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The utility model relates to the preparation facilities for sulfur electrode material.Sulfur electrode material preparation facilities comprises blender, storage sulphur device, heating system and vacuum system; Storage sulphur device and blender body is contour, the trapezoid steel pipe that porous stainless steel is wide bottom being, top is narrow; Hole is symmetrically distributed in stainless steel pipe surface, and aperture is 1 ~ 20 micron, and hole count is 2 ~ 10/ square centimeters; Composite material prepared by this device, has good specific capacity and excellent cycle performance: have good application prospect in field of batteries.
Description
Technical field
The present invention relates to a kind of process units of electrode material, be specifically related to a kind of preparation facilities for sulfur electrode material.
Background technology
Elemental sulfur has cheap, rich reserves, than can high, the advantage such as environmental pollution is little, therefore lithium-sulfur cell be considered to very promising battery of new generation.The critical bottleneck of lithium-sulfur cell is to develop high performance sulphur positive electrode. but the non-constant of sulphur conductivity, be unfavorable for the high rate capability of battery; Sulphur sulphur generation volumetric expansion and contraction in charge and discharge process can make the structure of electrode material change, and depart from metal collector, cause capacity rapid decay in cyclic process, utilization efficiency low.Current attainable lithium-sulfur cell actual specific capacity is far below theoretical specific capacity.Surface modification is the common method of the conductivity improving sulphur.Lot of documents and patent adopt porous conductive material with carbon element to support sulphur simple substance, show the high rate performance of high specific capacity, good cycle performance and excellence.Guo JC(Guo JC，Xu Y H，Wang CS.Nano Letters，2011，11：4288-4294.)。GengXY (Geng XY, Rao M, Li XP.J.Solid State Electrochem., 2013,17:987-992.) prepared sulphur/carbon nano tube compound material, first discharge specific capacity is 900mAh/g, and 100 times recycle ratio capacity keeps 700mAh/g.Direct precipitation method is adopted to prepare sulphur/multi-wall carbon nano-tube composite material; When current density is 0.02C, first discharge specific capacity is 1229mAh/g, and after 50 circulations, capacity remains on more than 800mAh/g.In order to improve the chemical property of sulphur/carbon composite further, Wang (Wang C, Wan W, Chen JT, Zhou HH.J Mater.Chem.A, 2013,1:1716-1723) prepare the MWCNTs/S/PPy composite material with double-nucleocapsid structure; 200mA/g, first discharge specific capacity is 1517mAh/g; 1500mA/g, 200 circulations, specific capacity 560mAh/g.Amphipathic nature polyalcohol is adopted to carry out surface treatment to hollow Nano carbon fiber; Modified sulphur/nano-fiber composite material 0.2C specific discharge capacity is 1180mAh/g, and 0.5C300 time capability retention is 80%.
Undeniable, novel structure, the material with carbon element that hole dimension is little effectively limits the granular size of sulphur simple substance, simultaneously the conductivity such as material with carbon element and polymer good material improves the conductance of elemental sulfur. but carbon and polymer add the energy density that membership reduces whole battery, only have sulfur content in carbon sulphur combination electrode material just to have using value more than 70wt%.And the high rate performance of sulphur/carbon composite does not improve.
Summary of the invention
The object of the invention is the preparation facilities and the production method that provide a kind of sulfur electrode material, overcomes the defect of existing technology of preparing, improves high rate performance and the cycle life of sulfur electrode material.For achieving the above object, technical scheme of the present invention is, the sulfur electrode material preparation facilities provided comprises blender, storage sulphur device, heating system and vacuum system; Blender comprises upper cover, mounting flange and blender body; Heating system comprises heating plate, transducer and controller; Vacuum system comprises vacuum pump and alloy membrane; Heating plate, together with sensor stack, is arranged at blender case surface and coated thermal insulation layer; Controller is arranged at bottom blender; Vacuum pump connects blender upper cover by alloy membrane, stainless steel tube; Blender top cap connects the left and right sides, alloy membrane place and arranges stainless steel pipes, and stainless steel tube connects recirculated water; Storage sulphur device is porous stainless steel handstand plane hollow steel plate, and porous stainless steel quantity is 2 ~ 30, and porous stainless steel is fixed on plane hollow steel plate by movable bolt; Storage sulphur device and blender body is contour, the trapezoid steel pipe that porous stainless steel is wide bottom being, top is narrow; Hole is symmetrically distributed in stainless steel pipe surface, and aperture is 1 ~ 20 micron, and hole count is 2 ~ 10/ square centimeters;
Described sulfur electrode material is that elemental sulfur is scattered in porous oxide electrode material; The particle of porous oxide electrode material is between 10 ~ 500nm; Porous oxide electrode material is the one of hollow vanadic oxide nano-powder, Hollow Nickel cobalt manganese oxidate for lithium nano-powder, hollow LiMn2O4 nano-powder, Hollow Nickel cobalt oxidate for lithium nano-powder; The mass fraction that sulphur simple substance accounts for sulfur electrode material is 20 ~ 70%;
The conducting polymer of coated 1 ~ 20% mass fraction of described sulfur electrode material surface: conducting polymer is the one of polypyrrole, polyaniline, polythiophene, polyacrylonitrile;
Described sulfur electrode material preparation facilities and production method: it comprises the following steps:
1) porous electrode material and sulphur simple substance is weighed by a certain percentage; Sulphur simple substance puts into storage sulphur device stainless steel tube, and is fixed on storage sulphur device plane hollow steel plate and blender body bottom portion by movable bolt; Porous electrode material is positioned in blender body; With flange motionless mixer upper cover and body;
2) start vacuum pump and heating-system-controller, controlling mixer temperature is 200 ~ 500 DEG C, constant temperature time 2 ~ 20h;
3) step (2) product is mixed with the polybenzazole precursor liquid solution of certain mass ratio, stirs 2 ~ 5h, add initator polymerization, leave standstill, suction filtration, oven dry, obtain sulfur electrode material.
Sulfur electrode material preparation facilities provided by the invention, compared with other sulphur method for preparing anode material, tool has the following advantages:
1) present invention process is simple, easy to operate, is conducive to suitability for industrialized production.
2) sulfur electrode material preparation facilities adopts sulphur diffusion of vapor to enter porous electrode material hole; Design porous, trapezoidal storage sulphur device stainless steel pipes, be conducive to sulphur steam rapid diffusion; Storage sulphur device stainless steel tube thermal conductivity is good, is conducive to the heat trnasfer strengthening porous electrode material;
3) sulfur electrode material preparation facilities design vacuum system, reduces the sublimation temperature of sulphur steam, improves the diffusion rate of sulphur steam; Alloy membrane be set and stainless steel condenser pipe is set near diffusion barrier, preventing sulphur steam from leaking.
Accompanying drawing illustrates:
Fig. 1 is the schematic diagram of sulfur electrode material preparation facilities of the present invention.
In figure, 1-blender body, 2-heating system, 3-stores up sulphur device, 4-aperture, 5-set bolt, 6-mounting flange, 7-blender upper cover, 8-recirculated water stainless steel tube, 9-diffusion barrier, 10-vacuum system
Embodiment
For summary of the invention of the present invention, Characteristic can be understood further, hereby lift following examples, and coordinate accompanying drawing to be described in detail as follows:
Refer to accompanying drawing 1
Embodiment 1
A kind of sulfur electrode material preparation facilities comprises blender, storage sulphur device, heating system and vacuum system; Blender comprises upper cover, mounting flange and blender body; Heating system comprises heating plate, transducer and controller; Vacuum system comprises vacuum pump and alloy membrane; Heating plate, together with sensor stack, is arranged at blender case surface and coated thermal insulation layer; Controller is arranged at bottom blender; Vacuum pump connects blender upper cover by alloy membrane, stainless steel tube; Blender top cap connects the left and right sides, alloy membrane place and arranges stainless steel pipes, and stainless steel tube connects recirculated water; Storage sulphur device is porous stainless steel handstand plane hollow steel plate, and porous stainless steel quantity is 2 ~ 30, and porous stainless steel is fixed on plane hollow steel plate by movable bolt; Storage sulphur device and blender body contour, porous stainless steel is that bottom is wide, trapezoid steel pipe that top is narrow; Hole is symmetrically distributed in stainless steel pipe surface, and aperture is 1 ~ 20 micron, and hole count is 2 ~ 10/ square centimeters;
A kind of sulfur electrode material comprises following system:
1) hollow vanadic oxide nano-powder (particle size, 200nm), mass fraction 55%; Sulphur simple substance, mass fraction 30%; Polyaniline, mass fraction 15%;
2) Hollow Nickel cobalt manganese oxidate for lithium nano-powder (LiCo
1/3ni
1/3mn
1/3o
2, particle size 100nm), mass fraction 40%; Sulphur simple substance, mass fraction 45%; Polypropylene, mass fraction 15%;
3) hollow LiMn2O4 nano-powder (particle size, 80nm), mass fraction 50%; Sulphur simple substance, mass fraction 35%; Polypyrrole, mass fraction 15%;
A kind of sulfur electrode material preparation facilities and production method: it comprises the following steps:
1) porous electrode material and sulphur simple substance is weighed by a certain percentage; Sulphur simple substance puts into storage sulphur device stainless steel tube, and is fixed on storage sulphur device plane hollow steel plate and blender body bottom portion by movable bolt; Porous electrode material is positioned in blender body; With flange motionless mixer upper cover and body;
2) start vacuum pump and heating-system-controller, controlling mixer temperature is 400 DEG C, constant temperature time 10h;
3) step (2) product is mixed with the polybenzazole precursor liquid solution of certain mass ratio, stirs 5h, add initator polymerization, leave standstill, suction filtration, oven dry, obtain sulfur electrode material.
The preparation and property test of sulfur electrode; Sulfur electrode material, acetylene black and PVDF among NMPs to be mixed in mass ratio at 80: 10: 5, be coated on aluminium foil is electrode film, metal lithium sheet is to electrode, CELGARD 2400 is barrier film, the LiPF6/EC+DMCWEI of 1mol/L is electrolyte, be assembled into button cell being full of in Ar glove box, adopt Land battery test system to carry out constant current charge-discharge test.The 0.1C of system 1,2 and 3 sulfur electrode first discharge capacity is greater than 700mAh/g, and after 1C discharge capacity is greater than 300mAh/g.100 circulation, capability retention is greater than 70%.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (2)
1. the preparation facilities for sulfur electrode material; It is characterized in that: described sulfur electrode material preparation facilities comprises blender, storage sulphur device, heating system and vacuum system; Blender comprises upper cover, mounting flange and blender body; Heating system comprises heating plate, transducer and controller; Vacuum system comprises vacuum pump and alloy membrane; Heating plate, together with sensor stack, is arranged at blender case surface and coated thermal insulation layer; Controller is arranged at bottom blender; Vacuum pump connects blender upper cover by alloy membrane, stainless steel tube; Blender top cap connects the left and right sides, alloy membrane place and arranges stainless steel pipes, and stainless steel tube connects recirculated water; Storage sulphur device is porous stainless steel handstand plane hollow steel plate, and porous stainless steel quantity is 2 ~ 30, and porous stainless steel is fixed on plane hollow steel plate by movable bolt.
2. sulfur electrode material preparation facilities according to claim 1: it is characterized in that: described storage sulphur device and blender body contour, porous stainless steel is that bottom is wide, trapezoid steel pipe that top is narrow; Hole is symmetrically distributed in stainless steel pipe surface, and aperture is 1 ~ 20 micron, and hole count is 2 ~ 10/ square centimeters.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201520031972.7U CN204424370U (en) | 2015-01-16 | 2015-01-16 | A kind of preparation facilities for sulfur electrode material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104538602A (en) * | 2015-01-16 | 2015-04-22 | 中国计量学院 | Preparation device and production method for sulfur electrode material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104538602A (en) * | 2015-01-16 | 2015-04-22 | 中国计量学院 | Preparation device and production method for sulfur electrode material |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150624 Termination date: 20170116 |