CN109216704A - A kind of preparation method applied to the modified interlayer of anode in lithium-sulfur cell - Google Patents
A kind of preparation method applied to the modified interlayer of anode in lithium-sulfur cell Download PDFInfo
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- CN109216704A CN109216704A CN201811062619.XA CN201811062619A CN109216704A CN 109216704 A CN109216704 A CN 109216704A CN 201811062619 A CN201811062619 A CN 201811062619A CN 109216704 A CN109216704 A CN 109216704A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/665—Composites
- H01M4/667—Composites in the form of layers, e.g. coatings
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- 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 present invention relates to a kind of preparation methods applied to the modified interlayer of anode in lithium-sulfur cell, this method prepares continuous nano-ZnO tunica fibrosa using method of electrostatic spinning, then by carrying out the modified interlayer of anode that carbonization treatment obtains to electrostatic spinning ZnO film, the modification interlayer that this method obtains improves polysulfide shuttle effect in lithium-sulfur cell of the existing technology, active material utilization in positive electrode is low, the defect for causing lithium-sulfur cell performance bad.
Description
Technical field
The invention belongs to lithium battery preparation technical fields, more particularly, to a kind of anode applied in lithium-sulfur cell
The preparation method of modified interlayer.
Background technique
An urgent demand with the world today to new energy, more and more clean energy resourcies are used in electric power and power is set
In standby.Lithium ion battery, as light, high specific energy, it is environmental-friendly, can be recycled the advantages that, become numerous energy storage devices
It is preferred.Positive electrode of the elemental sulfur as lithium-sulfur cell, theoretical capacity reach 1675 mAh/g, and theoretical energy density can reach
2600 Wh/kg have critical role in the development of later lithium battery.But due in elemental sulfur and its charge and discharge process
Between product electric conductivity it is poor, there is the problems such as shuttle effect in polysulfide, lead to the utilization rate one of positive electrode during the reaction
It directly remains at low levels, affects its practical application.
In order to be dedicated to solving the disadvantages mentioned above of lithium-sulfur cell, in recent years, researcher is in the side such as anode, cathode, electrolyte
Many effort have been done in face, and emphasis solves the conductivity of positive electrode, reduces " shuttle effect " in reaction process, to lithium metal
The several aspects of the protection of cathode.In addition to the rapid development of sulphur anode and cathode of lithium, the research of modified interlayer material is also closed extensively
Note.Modified interlayer is placed among anode and diaphragm, can play it is physical or chemically fix wearing for polysulfide
The effect of shuttle, which improves the utilization rates of positive active material, so that the overall performance of lithium-sulfur cell be made all to get a promotion.
Such as: Sheng-Heng Chung et al. (Sheng-Heng C, Arumugam M. High-Performance Li-S
Batteries with an Ultra-lightweight MWCNT-Coated Separator[J]. Journal of
Physical Chemistry Letters, 2014,5 (11): 1978.) using MWCNT(multi-walled carbon nanotube) come modify every
Film makes diaphragm have bi-functional, and by it using in lithium-sulfur cell, performance is promoted well.It traces it to its cause and mainly contains
The diaphragm of multi-walled carbon nanotube: having strong electric conductivity, as collector, is conducive to the transmission of electronics and ion, improves activity
The utilization rate of substance；As the barrier layer of polysulfide, the shuttle of physical blocking and absorption polysulfide；Porous barrier layer
Be conducive to shuttling for electrolyte, improve the efficiency of transmission of ion, so as to cause the utilization of superpower circulation and active material.
(Shaibani M, Akbari A, Sheath P, the et al. Suppressed Polysulfide such as Shaibani
Crossover in Li–S Batteries through a High-Flux Graphene Oxide Membrane
Supported on a Sulfur Cathode [J] Acs Nano, 2016,10 (8)) using the oxidation stone of high crimp
The GO of the discotic mesogenic sulphur positive electrode surface for being applied directly to coat in advance is prepared orderly row by cutting method by black alkene (GO)
The GO film of column coats positive interlayer.The result shows that discharge capacity is respectively 1063mAh/g (sulfur-bearing to coated anode for the first time
Mass fraction 70%) and 1182mAh/g (sulfur mass fraction 80%), electrode capacity is 835mAh/g after recycling 100 times.
CN104393349A discloses a kind of lithium-sulfur cell protective layer and preparation method thereof, is coated and is connect on diaphragm by the method
The mixing of the modified graphene and adhesive of the various functional groups of branch, thus effectively to prevent polysulfide wearing in the electrolytic solution
The corrosion of shuttle and polysulfide to cathode of lithium can make discharging product more uniformly be deposited on electrode surface, improve lithium-sulfur cell
Specific capacity and cycle life.
Document above and patent effectively improve the conductivity of elemental sulfur, improve the reactivity of elemental sulfur, are promoted
To the protection of cathode and the circulation of battery and safety, but not from the effect and lithium metal of the basic shuttle for solving polysulfide
The problem of dendrite dusting, and preparation process is more complicated, production 78 is at high cost, influences its extensive use in lithium-sulfur cell.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods applied to the modified interlayer of anode in lithium-sulfur cell.
The present invention prepares continuous nano-ZnO tunica fibrosa using method of electrostatic spinning, then by electrostatic spinning ZnO film into
The modified interlayer of the anode that row carbonization treatment obtains, the modification interlayer that this method obtains improve in lithium-sulfur cell of the existing technology
Polysulfide shuttle effect, the active material utilization in positive electrode is low, the defect for causing lithium-sulfur cell performance bad.
Technical scheme is as follows:
The present invention provides a kind of preparation methods applied to the modified interlayer of anode in lithium-sulfur cell, include the following steps:
Step 1: electrostatic spinning precursor liquid is prepared
Be that zinc acetate solution is added in 10% ~ 30% poly-vinyl alcohol solution to mass fraction under magnetic agitation state, then 50 ~
Water-bath flows back several 2 ~ 10 hours at 80 DEG C；
Step 2: nano-ZnO tunica fibrosa is prepared
The mixed solution that step 1 obtains is added in syringe and carries out electrostatic spinning, control operating voltage is 10 ~ 20kV, is adjusted
Receiver and spinning syringe needle distance are 5 ~ 20cm, and the rate of outflow of mixed solution is 0.2 ~ 0.8ml/h, and the spinning time is 4 ~ 8h,
Nano-ZnO tunica fibrosa is obtained,
Step 3: nano-ZnO fiber is prepared
The nano-ZnO tunica fibrosa that step 2 is spun is calcined after (50 ~ 80 DEG C) of vacuum oven dry 8h at 600 ~ 800 DEG C
5h is then down to room temperature naturally, obtains ZnO nano fiber.
Step 4: the preparation of positive interlayer
The preparation of interlayer: nano-ZnO fibrous material, conductive agent and binder Kynoar (PVDF) that step 3 obtains are existed
The lower mixing of argon atmosphere protection, instills N-methyl pyrrolidinone solvent, is made into slurry, and coated in diaphragm matrix, dries and cut
It cuts out and is modified interlayer to get to the anode applied to lithium-sulfur cell；
Wherein, the material proportion is nano-ZnO fibrous material: conductive agent: binder=7~8.5:0.5~2:1, described
Conductive agent be acetylene black or Super P；The coating thickness of diaphragm matrix spreading mass is 0.01~0.1mm.
In above-mentioned steps one, polyvinyl alcohol and zinc acetate mass ratio are 0.5 ~ 3:1.
The material of the diaphragm is specially microporous polypropylene membrane (PP(Celgard-2400) diaphragm)
The preparation method of the above-mentioned functional ZnO interlayer for lithium-sulfur cell, wherein involved raw material pass through it is commercially available
It obtains, equipment used and technique are known to those skilled in the art.
Compared with prior art, the invention has the advantages that and the utility model has the advantages that
The present invention prepares ZnO nano tunica fibrosa with reticular structure pattern very rich, after calcining by electrostatic spinning
ZnO nano fiber preferably maintain one-dimensional nano structure, the large specific surface area of this nanofiber, hole are compared with horn of plenty.
ZnO prevents the shuttle effect of polysulfide with the characteristic of itself absorption polysulfide.In addition, ZnO also has good heat steady
Qualitative and mechanical property improves absorption characteristic in the electrolytic solution and influences the diffusion of polysulfide, and then improves lithium sulphur
The chemical property of battery.
Detailed description of the invention
Fig. 1 is the X-ray diffraction (XRD) figure of the modified interlayer of ZnO fiber anode obtained by embodiment 1；
Fig. 2 is scanning electron microscope (SEM) figure of the modified interlayer of ZnO fiber anode obtained by embodiment 1；
Fig. 3 is circulation volume figure of the modified interlayer of ZnO fiber anode obtained by embodiment 1 at 0.1 C.
Specific embodiment
Further illustrate the present invention below in conjunction with specific embodiments and the drawings, but embodiment the present invention is not done it is any
The restriction of form.Unless stated otherwise, the reagent and equipment that the present invention uses are used for the art conventional reagent and equipment
Reagent and material are commercially available.
Embodiment 1:
The first step, the preparation of electrostatic spinning precursor liquid:
Under magnetic agitation state, in 20g 10%(mass percent) zinc acetate solution (1.5g is slowly added dropwise in poly-vinyl alcohol solution
(CH3COO)2Zn·H2O and 2g H2O).Then water-bath reflux 5h is spare at 60 DEG C.
Second step, the preparation of ZnO nano tunica fibrosa:
Mixed solution is added in syringe, control operating voltage is 10kV, and adjusting receiver and spinning syringe needle distance is 10cm,
The rate of outflow of solution is 0.5ml/h, obtains ZnO nano tunica fibrosa after spinning 6h.
Third step, the preparation of ZnO nano fiber:
The tunica fibrosa spun is after (70 DEG C) of vacuum oven dry 8h, in 700 DEG C of calcining 5h.It is then down to room temperature naturally, obtains
To ZnO nano fiber.
4th step, the preparation of positive interlayer:
Nano ZnO material obtained and conductive agent and binder are placed in mortar according to the ratio that mass ratio is 8: 1: 1 and ground,
It then instills N-methyl pyrrolidinone solvent and is mixed into slurry, slurry is uniformly scratched in microporous polypropylene membrane (PP(Celgard-
2400) diaphragm) on, dry 2h, cuts out to obtain interlayer at 60 DEG C, and it is anode, metal lithium sheet as cathode using sulphur, electrolyte is added,
Assembly obtains lithium-sulfur cell in the glove box full of argon gas, obtains button CR2032 half-cell, and wherein conductive agent is acetylene black,
Binder is PVDF.
Fig. 1 is the X-ray diffraction (XRD) figure of interlayer material made from the present embodiment, diffraction maximum and JCPDS:36-1451 card
Piece is consistent, and diffraction maximum is very sharp, and the crystallinity of ZnO is fine.This explanation is burnt under the electrostatic spinning process of this experiment by sky
The ZnO substance arrived is very pure.Fig. 2 be after electrostatic spinning it is empty fire ZnO scanning electron microscope (SEM) figure, as can be seen from Figure 2
ZnO growth in situ on fiber, fiber width is larger, and network structure is intricate, and microscopic appearance is good, therefore as battery
The phenomenon that modified interlayer of anode can largely reduce polysulfide " shuttle " in charge and discharge process, to improve battery
Chemical property.
Fig. 3 is that embodiment 1 is obtained using nano-ZnO fiber as the constant current punching at 0.1 C of the lithium-sulfur cell of interlayer
Electric discharge figure, there are two platforms near 2.4 V and 2.0 V as can be seen from Figure 3, this is two reduction common in lithium-sulfur cell
Peak.From the figure we can see that maximum discharge capacity is close to 1500 mAh/g, due to nanofibrous structures large specific surface area,
Hole improves absorption characteristic in the electrolytic solution and influences the diffusion of polysulfide compared with horn of plenty, and then improves lithium sulphur electricity
The chemical property in pond.
Embodiment 2:
The first step, the preparation of electrostatic spinning precursor liquid:
Under magnetic agitation state, in 20g 30%(mass percent) zinc acetate solution (3g is slowly added dropwise in poly-vinyl alcohol solution
(CH3COO)2ZnH2O and 1g H2O).Then water-bath reflux 5h is spare at 80 DEG C.
Second step, the preparation of ZnO nano tunica fibrosa:
Mixed solution is added in syringe, control operating voltage is 10kV, and adjusting receiver and spinning syringe needle distance is 10cm,
The rate of outflow of solution is 0.5ml/h, obtains ZnO nano tunica fibrosa after spinning 4h.
Third step, the preparation of ZnO nano fiber:
The fiber spun is after (70 DEG C) of vacuum oven dry 8h, in 700 DEG C of calcining 5h.It is then down to room temperature naturally, obtains
ZnO nano fiber.
4th step, the preparation of positive interlayer:
Nano ZnO material obtained and conductive agent and binder are placed in mortar according to the ratio that mass ratio is 8: 1: 1 and ground
Afterwards, it instills N-methyl pyrrolidinone solvent and is mixed into slurry, slurry is uniformly scratched in microporous polypropylene membrane (PP(Celgard-
2400) diaphragm) on, dry 2h, cuts out to obtain interlayer at 60 DEG C, and it is anode, metal lithium sheet as cathode using sulphur, electrolyte is added,
Assembly obtains lithium-sulfur cell in the glove box full of argon gas, obtains button CR2032 half-cell.
Embodiment 3:
The first step, the preparation of electrostatic spinning precursor liquid:
Under magnetic agitation state, in 20g 10%(mass percent) zinc acetate solution (1.5g is slowly added dropwise in poly-vinyl alcohol solution
(CH3COO)2ZnH2O and 2g H2O).Then water-bath reflux 5h is spare at 60 DEG C.
Second step, the preparation of ZnO nano tunica fibrosa:
Mixed solution is added in syringe, control operating voltage is 20kV, and adjusting receiver and spinning syringe needle distance is 20cm,
The rate of outflow of solution be 0.8ml/h, the spinning time be 4 ~ 8h to get arrive ZnO nano tunica fibrosa.
Third step, the preparation of ZnO nano fiber:
The tunica fibrosa spun is after (70 DEG C) of vacuum oven dry 8h, in 700 DEG C of calcining 5h.It is then down to room temperature naturally, obtains
To ZnO nano fiber.
4th step, the preparation of positive interlayer:
Nano ZnO material obtained and conductive agent and binder are placed in mortar according to the ratio that mass ratio is 8: 1: 1 and ground
Afterwards, N-methyl pyrrolidinone solvent is instilled, slurry is mixed into, slurry is uniformly scratched in microporous polypropylene membrane (PP(Celgard-
2400) diaphragm) on, dry 2h, cuts out to obtain interlayer at 60 DEG C, and it is anode, metal lithium sheet as cathode using sulphur, electrolyte is added,
Assembly obtains lithium-sulfur cell in the glove box full of argon gas, obtains button CR2032 half-cell.
Embodiment 4:
The first step, the preparation of electrostatic spinning precursor liquid:
Under magnetic agitation state, in 20g 10%(mass percent) zinc acetate solution (1.5g is slowly added dropwise in poly-vinyl alcohol solution
(CH3COO)2ZnH2O and 2g H2O).Then water-bath reflux 5h is spare at 60 DEG C.
Second step, the preparation of ZnO nano tunica fibrosa:
Mixed solution is added in syringe, control operating voltage is 10kV, and adjusting receiver and spinning syringe needle distance is 10cm,
The rate of outflow of solution be 0.5ml/h, spinning 8h to get arrive ZnO nano tunica fibrosa.
Third step, the preparation of ZnO nano fiber:
The fiber spun is after (70 DEG C) of vacuum oven dry 8h, in 400 DEG C of calcining 5h.It is then down to room temperature naturally, obtains
ZnO nano fiber.
4th step, the preparation of positive interlayer:
Nano ZnO material obtained and conductive agent and binder are placed in mortar according to the ratio that mass ratio is 8: 1: 1 and ground
Afterwards, it instills N-methyl pyrrolidinone solvent and is mixed into slurry, slurry is uniformly scratched in microporous polypropylene membrane (PP(Celgard-
2400) diaphragm) on, dry 2h, cuts out to obtain interlayer at 60 DEG C, and it is anode, metal lithium sheet as cathode using sulphur, electrolyte is added,
Assembly obtains lithium-sulfur cell in the glove box full of argon gas, obtains button CR2032 half-cell.
Unaccomplished matter of the present invention is well-known technique.
Claims (9)
1. a kind of preparation method applied to the modified interlayer of anode in lithium-sulfur cell, which is characterized in that include the following steps, walk
Rapid one: preparing electrostatic spinning precursor liquid；Step 2: method of electrostatic spinning prepares nano-ZnO tunica fibrosa；Step 3: carbonization nano-ZnO
Fiber film preparation nano-ZnO fiber；Step 4: positive interlayer is prepared by coating diaphragm.
2. the preparation method according to claim 1 applied to the modified interlayer of anode in lithium-sulfur cell, which is characterized in that
The method that the step 1 prepares electrostatic spinning precursor liquid are as follows: be 10% ~ 30% polyethylene to mass fraction under magnetic agitation state
Zinc acetate solution is added in alcoholic solution, then water-bath flows back several 2 ~ 10 hours at 50 ~ 80 DEG C.
3. the preparation method according to claim 2 applied to the modified interlayer of anode in lithium-sulfur cell, which is characterized in that
The polyvinyl alcohol and zinc acetate mass ratio is 0.5 ~ 3:1.
4. the preparation method according to claim 1 applied to the modified interlayer of anode in lithium-sulfur cell, which is characterized in that
The method that the step 2 method of electrostatic spinning prepares nano-ZnO tunica fibrosa are as follows: the mixed solution for obtaining the step 1 is added
Electrostatic spinning is carried out in syringe, control operating voltage is 10 ~ 20kV, and adjusting receiver and spinning syringe needle distance is 5 ~ 20cm,
The rate of outflow of mixed solution be 0.2 ~ 0.8ml/h, the spinning time be 4 ~ 8h to get arrive nano-ZnO tunica fibrosa.
5. the preparation method according to claim 1 applied to the modified interlayer of anode in lithium-sulfur cell, which is characterized in that
The method of the step 3 carbonization nano-ZnO fiber film preparation nano-ZnO fiber are as follows: the nano-ZnO for spinning the step 2
Tunica fibrosa, in 600 ~ 800 DEG C of calcining 5h, is then down to room temperature naturally, is obtained in a vacuum drying oven at 50 ~ 80 DEG C after dry 8h
ZnO nano fiber.
6. the preparation method according to claim 1 applied to the modified interlayer of anode in lithium-sulfur cell, which is characterized in that
The method that the step 4 prepares positive interlayer by coating diaphragm are as follows: the nano-ZnO fibrous material that obtains the step 3,
Conductive agent and binder Kynoar mix under argon atmosphere protection, instill N-methyl pyrrolidinone solvent, are made into slurry,
And interlayer is modified to get to the anode applied to lithium-sulfur cell coated in diaphragm matrix, drying to cut out.
7. the preparation method according to claim 6 applied to the modified interlayer of anode in lithium-sulfur cell, which is characterized in that
The conductive agent is acetylene black or Super P.
8. the preparation method according to claim 6 applied to the modified interlayer of anode in lithium-sulfur cell, which is characterized in that
The coating thickness of the diaphragm matrix spreading mass is 0.01~0.1mm.
9. the preparation method according to claim 6 applied to the modified interlayer of anode in lithium-sulfur cell, which is characterized in that
The nano-ZnO fibrous material: conductive agent: the mass ratio of binder is 7~8.5:0.5~2:1.
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Application publication date: 20190115 |