CN109461915A - A kind of preparation method of the positive electrode of lithium-sulfur cell - Google Patents
A kind of preparation method of the positive electrode of lithium-sulfur cell Download PDFInfo
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- CN109461915A CN109461915A CN201811273170.1A CN201811273170A CN109461915A CN 109461915 A CN109461915 A CN 109461915A CN 201811273170 A CN201811273170 A CN 201811273170A CN 109461915 A CN109461915 A CN 109461915A
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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
- H01M4/362—Composites
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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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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
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- 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 of the positive electrode of lithium-sulfur cell, specifically, ZIF-67 nano material is prepared first, ZIF-67 GO/CNTS composite material is prepared using spray drying technology with GO/CNTS mixed solution in it again, and sulphur will be mixed as a kind of positive electrode of lithium-sulfur cell after composite material carbonization.Wherein, the preparation process of ZIF-67 is simple, and yield is higher, and product morphology is good, and spray drying can increase the synergistic effect of graphene and carbon nanotube, increases the electric conductivity of sample, and it is easy to reunite not allow its balling-up.It can then make its porous structure more be easy to carry sulphur the ZIF-67 GO/CNTS carbonization after spray drying, to promote the capacity of lithium-sulfur cell, and enhance the stability of its circulation.
Description
Technical field
Technical solution of the present invention is related to that electrode is made of active material, is exactly a kind of positive material of lithium-sulfur cell
The preparation method of material.
Background technique
With development in science and technology, portable electronic product, electric vehicle, space flight military industry field all expect there is energy
Density is higher, the longer battery system of working life.However, traditional lithium ion battery is by its theoretical capacity (300mAh/g)
Limitation, can no longer meet the requirement of the electric car or hybrid vehicle for long-distance transportation.Lithium-sulfur cell conduct
A kind of electrochemical energy storage system has the advantages that specific energy height, memory-less effect, good cycling stability.With Novel clean energy
The development of the development and utilization in source, especially electric car, to battery energy density, more stringent requirements are proposed.Lithium-sulfur cell exists
The theoretically energy density per unit volume of the specific energy with 2600Wh/kg and 2800Wh/L, and lower cost for material, environment
Close friend can satisfy the requirement of many emerging technologies.
But the poor cycle performance of lithium-sulfur cell and high rate performance limit its industrial applications, because lithium is repeatedly
Insertion abjection will lead to this kind of electrode and biggish volume change occur in charge and discharge process, destroys battery structure, causes electrode
Gradually dusting is failed, and keeps cycle performance of battery poor.In order to overcome the disadvantage of metal oxide battery performance rapid decay, nanometer
Change technology provides great feasible scheme to solve performance degradation.But it still has yield during industrialization development
Smaller, many technical problems such as preparation method complexity, in order to improve charge storage ability and the safety of battery, researcher is developed
More efficient nanocomposite is as anode.And nanocomposite in charge and discharge process absolute volume variation compared with
Small, electrode structure has higher stability.The specific area of nano material is very big simultaneously, and there are a large amount of crystal boundary, these structures
On feature be conducive to improve electrode reaction dynamic performance.
ZIF-67 is the molecular sieve analog imidazoles coordination polymer being complexed by metal ion Co and imidazoles or imdazole derivatives.
Compared with traditional molecular sieve, ZIF-67 has yield higher, reconfigurable, pore size, specific surface area height, structure and function
The series of advantages such as multiplicity.And graphene oxide is product of the powdered graphite after chemical oxidation and removing, graphene oxide is
Single atomic layer can expand to some tens of pm on lateral dimension at any time, be a kind of new carbon haveing excellent performance, tool
Have higher specific surface area and surface functional group abundant, can be considered a kind of flexible material of non-traditional kenel, have polymer,
The characteristics such as colloid, film and amphiphatic molecule.And carbon nanotube is monodimension nanometer material, light-weight, hexagonal structure connection
Perfection has many superior mechanics, electricity and chemical property.
We prepare ZIF-67@GO/CNTS composite material using spray drying device at innovative mix GO with CNT
Lithium-sulfur cell is improved as the positive electrode of lithium-sulfur cell.
Summary of the invention
It is an object of the invention to: a kind of positive electrode and preparation method thereof of lithium-sulfur cell is provided, to overcome existing skill
The defect of art.Specifically, ZIF-67 nano material is prepared first, then it is utilized into spray drying skill with GO/CNTS mixed solution
Art is prepared ZIF-67 GO/CNTS composite material, and will mix sulphur after composite material carbonization as a kind of lithium-sulfur cell just
Pole material.Wherein, the preparation process of ZIF-67 is simple, and yield is higher, and product morphology is good, spray drying can increase graphene with
The synergistic effect of carbon nanotube, increases the electric conductivity of sample, and it is easy to reunite not allow its balling-up.By the ZIF- after spray drying
67 GO/CNTS carbonization can then make its porous structure more be easy to carry sulphur, to promote the capacity of lithium-sulfur cell, and increase
The stability of its strong circulation.
The preparation method of lithium sulfur battery anode material provided by the invention, specifically includes that steps are as follows:
Step 1: the preparation of ZIF-67@GO/CNTS composite material:
By Co (NO3)2·6H2O and 2-methylimidazole are separately added into stirring configuration homogeneous solution in methanol, will be mixed with 2- methyl miaow
The solution of azoles is poured slowly into also in stirring equipped with Co (NO3)2·6H2In the solution of O, stood after stirring 30min.It for 24 hours afterwards will be molten
Liquid is centrifuged and dries, and obtains ZIF-67.Graphene and carbon nanotube are added in deionized water, mixed solution is made.It will preparation
Good ZIF-67 is added into the mixed solution equipped with graphene and carbon nanotube, and ZIF-67@GO/ is made using being spray-dried
CNTS composite material.
Step 2: the carbonization of ZIF-67@GO/CNTS composite material:
The ZIF-67@GO/CNTS composite material of first step preparation is warming up to 350 DEG C of heating 2h under conditions of argon gas is protected,
It is warming up to 600-700 DEG C of heating 30min later, then naturally cools at room temperature, obtains ZIF-67@GO/CNTS composite material
Carbonized samples.
Step 3: ZIF-67 GO/CNTS composite material carbonization sample mixes sulphur:
By ZIF-67 GO/CNTS composite material carbonization sample and sulphur powder, it is placed in mixed grinding in mortar.It is dripped into mixed-powder
Enter CS2It is ground to CS2Volatilization completely, repetitive operation is into sulphur powder without yellow particle.Mixed-powder is placed in the reaction full of argon gas
In kettle, reaction kettle is placed in Constant Temp. Oven, 155 DEG C of set temperature, the time is set as 12h.
Preferably, Co (NO3)2·6H2The quality of O is 1400 ~ 1500mg, the quality of 2-methylimidazole is 1600 ~
1700mg, the dosage of methanol are 125ml.
Preferably, the mass ratio of graphene and carbon nanotube is 1:1.
A kind of preparation method of above-mentioned lithium sulfur battery anode material, related raw material are commercially available.
Beneficial effects of the present invention are as follows:
(1) in design process of the invention, the structure problem of sulfenyl composite material in lithium sulfur battery anode material has been fully considered,
Innovatively propose prepare ZIF-67@GO/CNTS composite material with spray drying and material that sample carbonization treatment obtains into
Row sulfur doping is as lithium sulfur battery anode material.
(2) in design process of the invention, cooperateing with for graphene and carbon nanotube is increased during dry spraying
Effect, promotes the electric conductivity of sample, and makes its balling-up and do not allow easy to reunite, greatly improves lithium sulfur battery anode material
Chemical property, discharge capacity decays very little in cyclic process, and cyclical stability significantly improves.And the carbonization of ZIF-67 is so that more
Pore structure is more easier to carry sulphur, can significantly improve positive electrode electric conductivity.
(3) positive electrode prepared by the method for the present invention is applied in lithium-sulfur cell, the charge and discharge for the first time of battery at 0.1C
Electric specific capacity reaches 1557mAh/g, and with high discharge capacity and brilliant cyclical stability, chemical property, which is substantially better than, to be made
With the performance of the lithium-sulfur cell of other positive electrodes.
Detailed description of the invention
Fig. 1 is the electron scanning micrograph of ZIF-67@GO/CNTS composite material obtained by embodiment 1.
Fig. 2 is the charge discharge curve of positive electrode obtained by embodiment 1.
The present invention is further described with case study on implementation with reference to the accompanying drawing.
Embodiment 1:
Step 1: the preparation of ZIF-67@GO/CNTS composite material:
Co (the NO for the 1455mg for being by weight3)2·6H2O, which is added, stirs 10min into the methanol solution of 125ml；By 1640mg
2-methylimidazole be added and stir 10min into the methanol solution of 125ml, the solution for being mixed with 2-methylimidazole is poured slowly into also
It is furnished with Co (NO in stirring3)2·6H2In the solution of O, stood after stirring 30min.Solution is centrifuged and is dried afterwards for 24 hours.By stone
Black alkene and carbon nanotube are made into the mixed solution that mass ratio is 1:1.The ZIF-67 prepared is added to equipped with graphene and carbon
In the mixed solution of nanotube, ZIF-67@GO/CNTS composite material is made using being spray-dried.
Step 2: the carbonization of ZIF-67@GO/CNTS composite material:
ZIF-67@GO/CNTS composite material prepared by the first step is placed in porcelain boat, then porcelain boat is placed in tube furnace
Under conditions of argon gas protection sample is warming up to 600 DEG C of heating 30min after 350 DEG C of heating 2h, then naturally cools to room
The carbonized samples of ZIF-67@GO/CNTS composite material are obtained under temperature.
Step 3: ZIF-67 GO/CNTS composite material carbonization sample mixes sulphur:
By ZIF-67 GO/CNTS composite material carbonization sample and sulphur powder, it is placed in mixed grinding in mortar.It is dripped into mixed-powder
Enter CS2It is ground to CS2Volatilization completely, repetitive operation is into sulphur powder without yellow particle.Mixed-powder is placed in reaction kettle, is made anti-
It answers in kettle full of argon gas.Reaction kettle is placed in Constant Temp. Oven, 155 DEG C of set temperature, the time is set as 12h.
Fig. 1 is the electron scanning micrograph of ZIF-67@GO/CNTS composite material obtained by the present embodiment.It is sweeping
It traces designs in piece, more intuitively shows the porous structure for the ZIF-67@GO/CNTS composite material that the present invention designs.
Fig. 2 is the charge discharge curve of positive electrode obtained by the present embodiment.It may be seen that in 0.1C electric current
Under density, the discharge capacity for the first time of the material is up to 1557mAh/g.
Specific embodiment
Embodiment 2
Step 1: the preparation of ZIF-67@GO/CNTS composite material:
Co (the NO for the 1455mg for being by weight3)2·6H2O, which is added, stirs 10min into the methanol solution of 125ml；By 1640mg
2-methylimidazole be added and stir 10min into the methanol solution of 125ml, the solution for being mixed with 2-methylimidazole is poured slowly into also
It is furnished with Co (NO in stirring3)2·6H2In the solution of O, stood after stirring 30min.Solution is centrifuged and is dried afterwards for 24 hours.By stone
Black alkene and carbon nanotube are made into the mixed solution that mass ratio is 1:1.The ZIF-67 prepared is added to equipped with graphene and carbon
In the mixed solution of nanotube, ZIF-67@GO/CNTS composite material is made using being spray-dried.
Step 2: the carbonization of ZIF-67@GO/CNTS composite material:
ZIF-67@GO/CNTS composite material prepared by the first step is placed in porcelain boat, then porcelain boat is placed in tube furnace
Under conditions of argon gas protection sample is warming up to 700 DEG C of heating 30min after 350 DEG C of heating 2h, then naturally cools to room
The carbonized samples of ZIF-67@GO/CNTS composite material are obtained under temperature.
Step 3: ZIF-67 GO/CNTS composite material carbonization sample mixes sulphur:
By ZIF-67 GO/CNTS composite material carbonization sample and sulphur powder, it is placed in mixed grinding in mortar.It is dripped into mixed-powder
Enter CS2It is ground to CS2Volatilization completely, repetitive operation is into sulphur powder without yellow particle.Mixed-powder is placed in reaction kettle, is made anti-
It answers in kettle full of argon gas.Reaction kettle is placed in Constant Temp. Oven, 155 DEG C of set temperature, the time is set as 12h.
Claims (3)
1. a kind of preparation method of lithium sulfur battery anode material, it is characterised in that: specifically comprise the following steps:
Step 1: the preparation of ZIF-67@GO/CNTS composite material
By Co (NO3)2·6H2O and 2-methylimidazole are separately added into stirring configuration homogeneous solution in methanol, will be mixed with 2- methyl miaow
The solution of azoles is poured slowly into also in stirring equipped with Co (NO3)2·6H2In the solution of O, stood after stirring 30min, it for 24 hours afterwards will be molten
Liquid is centrifuged and dries, and obtains ZIF-67；Graphene and carbon nanotube are added in deionized water, mixed solution is made, will prepared
Good ZIF-67 is added into the mixed solution equipped with graphene and carbon nanotube, and ZIF-67@GO/ is made using being spray-dried
CNTS composite material；
Step 2: the carbonization of ZIF-67@GO/CNTS composite material
The ZIF-67@GO/CNTS composite material of first step preparation is warming up to 350 DEG C of heating 2h under conditions of argon gas is protected,
It is warming up to 600-700 DEG C of heating 30min later, then naturally cools at room temperature, obtains ZIF-67@GO/CNTS composite material
Carbonized samples；
Step 3: ZIF-67 GO/CNTS composite material carbonization sample mixes sulphur
By ZIF-67 GO/CNTS composite material carbonization sample and sulphur powder, it is placed in mixed grinding in mortar, is dripped into mixed-powder
Enter CS2It is ground to CS2Mixed-powder, without yellow particle, is placed in the reaction full of argon gas into sulphur powder by volatilization, repetitive operation completely
In kettle, reaction kettle is placed in Constant Temp. Oven, 155 DEG C of set temperature, the time is set as 12h.
2. preparation method according to claim 1, it is characterised in that: Co (NO3)2·6H2The quality of O be 1400 ~
1500mg, the quality of 2-methylimidazole are 1600 ~ 1700mg, and the dosage of methanol is 125ml.
3. preparation method according to claim 1, it is characterised in that: the mass ratio of graphene and carbon nanotube is 1:1.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110010876A (en) * | 2019-04-15 | 2019-07-12 | 深圳市高能达电池有限公司 | A kind of controllable method for preparing of lithium sulphur one-shot battery nano anode material |
| CN110380062A (en) * | 2019-07-16 | 2019-10-25 | 运城学院 | The preparation method of the difunctional VPO catalysts of sulfur doping based on ZIF-67 and conductive graphene |
| CN110627136A (en) * | 2019-09-16 | 2019-12-31 | 肇庆市华师大光电产业研究院 | 3D-NiO/Co3O4Preparation method of/CNT/S composite material and application of/CNT/S composite material in lithium-sulfur battery |
| CN110752359A (en) * | 2019-10-29 | 2020-02-04 | 肇庆市华师大光电产业研究院 | Preparation method of sulfur-three-dimensional hollow graphene-carbon nanotube composite lithium-sulfur battery positive electrode material |
| CN110767889A (en) * | 2019-10-29 | 2020-02-07 | 肇庆市华师大光电产业研究院 | Preparation method of lithium-sulfur battery positive electrode material |
| CN111446427A (en) * | 2020-03-18 | 2020-07-24 | 肇庆市华师大光电产业研究院 | S @3DOM ZIF-8 composite positive electrode material for lithium-sulfur battery and preparation method thereof |
| CN112038637A (en) * | 2020-08-07 | 2020-12-04 | 合肥国轩高科动力能源有限公司 | Composite conductive agent, preparation method thereof and lithium ion battery |
| CN114162876A (en) * | 2021-12-10 | 2022-03-11 | 盐城工学院 | Preparation method and application of Co9S8@ carbon nanotube @ graphene composite material |
| CN115117349A (en) * | 2022-06-30 | 2022-09-27 | 合肥国轩高科动力能源有限公司 | Elastic conductive network conductive agent for silicon-carbon cathode of lithium ion battery, preparation method of slurry of conductive agent and lithium ion battery |
| CN115602997A (en) * | 2022-10-13 | 2023-01-13 | 河北工业大学（Cn） | Co 3 O 4 -PVA-PPy-PP diaphragm, preparation method and application thereof, and lithium-sulfur battery containing diaphragm |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110010876A (en) * | 2019-04-15 | 2019-07-12 | 深圳市高能达电池有限公司 | A kind of controllable method for preparing of lithium sulphur one-shot battery nano anode material |
| CN110380062A (en) * | 2019-07-16 | 2019-10-25 | 运城学院 | The preparation method of the difunctional VPO catalysts of sulfur doping based on ZIF-67 and conductive graphene |
| CN110627136A (en) * | 2019-09-16 | 2019-12-31 | 肇庆市华师大光电产业研究院 | 3D-NiO/Co3O4Preparation method of/CNT/S composite material and application of/CNT/S composite material in lithium-sulfur battery |
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| CN111446427A (en) * | 2020-03-18 | 2020-07-24 | 肇庆市华师大光电产业研究院 | S @3DOM ZIF-8 composite positive electrode material for lithium-sulfur battery and preparation method thereof |
| CN112038637A (en) * | 2020-08-07 | 2020-12-04 | 合肥国轩高科动力能源有限公司 | Composite conductive agent, preparation method thereof and lithium ion battery |
| CN114162876A (en) * | 2021-12-10 | 2022-03-11 | 盐城工学院 | Preparation method and application of Co9S8@ carbon nanotube @ graphene composite material |
| CN115117349A (en) * | 2022-06-30 | 2022-09-27 | 合肥国轩高科动力能源有限公司 | Elastic conductive network conductive agent for silicon-carbon cathode of lithium ion battery, preparation method of slurry of conductive agent and lithium ion battery |
| CN115117349B (en) * | 2022-06-30 | 2023-10-10 | 合肥国轩高科动力能源有限公司 | Elastic conductive network conductive agent for silicon-carbon negative electrode of lithium ion battery, preparation method of slurry of elastic conductive network conductive agent and lithium ion battery |
| CN115602997A (en) * | 2022-10-13 | 2023-01-13 | 河北工业大学（Cn） | Co 3 O 4 -PVA-PPy-PP diaphragm, preparation method and application thereof, and lithium-sulfur battery containing diaphragm |
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Application publication date: 20190312 |