CN105047982A - Lithium sulfur battery based on modification of graphene oxide thin film - Google Patents
Lithium sulfur battery based on modification of graphene oxide thin film Download PDFInfo
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- CN105047982A CN105047982A CN201510290505.0A CN201510290505A CN105047982A CN 105047982 A CN105047982 A CN 105047982A CN 201510290505 A CN201510290505 A CN 201510290505A CN 105047982 A CN105047982 A CN 105047982A
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic material
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/46—Separators, membranes or diaphragms characterised by their combination with electrodes
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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
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Abstract
The invention discloses a lithium sulfur battery. The lithium sulfur battery comprises a sulfur electrode, a metallic lithium electrode and a diaphragm and an electrolyte which are arranged between the sulfur electrode and the metallic lithium electrode. The lithium sulfur battery is characterized in that the sulfur electrode is modified by a graphene oxide thin film, and the sulfur electrode is prepared according to the following steps of: grinding and mixing a carbon sulfur compound, a conductive agent and an adhesive according to proportions, dissolving the obtained materials in N-methyl pyrrolidone to prepare paste, applying the paste onto a current collector, and drying the current collector to prepare the sulfur electrode for modification; preparing graphene oxide, and dissolving the graphene oxide in ethanol, wherein the concentration is 0.5-5 mg/mL; and uniformly adding the ethanol solution of the graphene oxide onto the surface of the modified sulfur electrode dropwise, and drying the surface of the modified sulfur electrode. By the graphene oxide thin film prepared according to the invention, polysulfide ions can be effectively bound and are greatly prevented from diffusing to the outside of the sulfur electrode, meanwhile, lithium ion transmission cannot be blocked, thus, oxidation shuttle effect in the lithium sulfur battery is suppressed, and the problem that the capacity is reduced dramatically due to the loss of active substance sulfur is solved.
Description
Technical field
The present invention relates to lithium-sulfur cell, lithium-sulfur cell of the sulfur electrode that especially a kind of graphene oxide film is modified and preparation method thereof.
Background technology
Compared with the lithium ion battery of main flow on market, lithium-sulfur cell has the former theoretical energy density of 2 ~ 5 times, thus deepens continuously to the research of lithium-sulfur cell, but, still there is the problem that capacity declines acutely, energy efficiency is low in lithium-sulfur cell, its main cause is the loss of active material sulphur; On the one hand, in charge and discharge process, inevitably there is " oxidation shuttle back and forth effect ", the polysulfide namely produced at sulfur electrode can diffuse in electrolyte, thus causes the drop of capacity; When polysulfide diffuses to cathode of lithium, they can generate Li with lithium metal reaction
2s
x, meanwhile, partial reduction products Li
2s
4can spread and get back to sulfur electrode and to go forward side by side single step reaction; On the other hand, the final reduzate Li of polysulfide and lithium metal reaction
2s
2and Li
2s
2all do not have conductivity, portion of product also can be deposited on lithium metal surface, thus loses electro-chemical activity formation " dead lithium ", causes the loss of part sulphur; By the restriction of " oxidation shuttle back and forth effect " and " dead lithium ", the capacity of lithium-sulfur cell declines violent, be difficult to still keep higher specific capacity after 300 circulations, thus lithium-sulfur cell cyclical stability is poor, energy efficiency is low, useful life, short basic reason was the loss of active material sulphur, and this is also the major reason that lithium-sulfur cell is difficult to the marketization.
Summary of the invention
For solving the problem, the invention provides a kind of lithium-sulfur cell and sulfur electrode preparation method thereof of the sulfur electrode based on graphene oxide film modification.
According to an embodiment of the present invention, a kind of lithium-sulfur cell, comprise sulfur electrode, metal lithium electrode and the barrier film be arranged between described sulfur electrode and metal lithium electrode and electrolyte, it is characterized in that: described sulfur electrode is the sulfur electrode (M-GO sulfur electrode) modified by graphite oxide film alkene.
According to an embodiment of the present invention, described lithium-sulfur cell, it is characterized in that: the active material in described sulfur electrode is the carbon-sulfur compound prepared by solwution method or additive method, the visible list of references of preparation method is L.-X.Miao, W.-K.Wang, A.-B.Wang, K.-G.Yuan, Y.-S.Yangb, JMaterChemA, 1 (2013) 11659 – 11664.
According to an embodiment of the present invention, described sulfur electrode, is characterized in that: the sulfur electrode for modifying is carbon-sulfur compound and conductive agent, adhesive mixing according to a certain percentage coating preparation; Wherein, the percentage of adhesive in carbon-sulfur compound, conductive agent and adhesive gross mass is 5 ~ 15%, the percentage of conductive agent in carbon-sulfur compound, conductive agent and adhesive gross mass is 5 ~ 15%, and the percentage of carbon-sulfur compound in carbon-sulfur compound, conductive agent and adhesive gross mass is 70 ~ 90%.
According to an embodiment of the present invention, described sulfur electrode, is characterized in that: described adhesive is Kynoar, the one in polyacrylic acid and sodium carboxymethylcellulose; Described conductive agent is acetylene black or oxidized black.
According to an embodiment of the present invention, the preparation method of the sulfur electrode that graphene oxide film is modified, is characterized in that being completed by following step:
(1) by carbon-sulfur compound and conductive agent, adhesive is ground and mixed proportionally, being dissolved in 1-METHYLPYRROLIDONE and preparing slurry and coat collector, preparing the sulfur electrode for modifying after drying.
(2) prepare graphene oxide, be dissolved in ethanol, concentration is 0.5 ~ 5mg/mL.
(3) ethanolic solution of graphene oxide step (2) configured evenly drips the sulfur electrode surface of the modification of preparation in step (1), 50 degrees Celsius to 120 degrees Celsius oven dry.
According to an embodiment of the present invention, described graphene oxide, is characterized in that: described graphene oxide with graphite or carbon black for raw material.
According to an embodiment of the present invention, described graphene oxide, is characterized in that: described graphene oxide for oxidant with the concentrated sulfuric acid and potassium permanganate, reacts and uses hydrochloric acid cleaning after 5 days to 7 days, after cleaning up ultrasonic 3 ~ 9 hours at 50 c.
According to an embodiment of the present invention, described graphene oxide solution, is characterized in that: described graphene oxide solution is the ethanolic solution of graphene oxide, and concentration is 0.5 ~ 5mg/mL.
According to an embodiment of the present invention, the sulfur electrode that described graphene oxide film is modified, is characterized in that: described graphene oxide film thickness controls according to the ethanol solution concentration of graphene oxide and dripping quantity, and general control is at 1 ~ 30nm.
According to another embodiment of the present invention, a kind of method preparing lithium-sulfur cell, is characterized in that: comprise the steps:
For the preparation of the step of the sulfur electrode modified, prepare the step of the sulfur electrode that graphene oxide film is modified, and prepare the step of button cell or flexible-packed battery.
The invention provides a kind of lithium-sulfur cell and sulfur electrode preparation method thereof of the sulfur electrode based on graphene oxide film modification, by this simple and effective titration, the controlled graphene oxide film of a layer thickness is prepared on the surface at the sulfur electrode for modifying, stop that polysulfide is diffused in electrolyte in charge and discharge process, weaken " oxidation shuttle back and forth effect ", improve cyclical stability, energy efficiency and the useful life of lithium-sulfur cell.
The sulfur electrode that graphite oxide film alkene prepared by the present invention is modified, the lithium-sulfur cell that the sulfur electrode modified with this graphene oxide film is prepared for positive pole has good cycling stability, and energy efficiency is high, the feature of long service life; Graphene oxide film prepared by the present invention modifies the lithium-sulfur cell performance test of sulfur electrode, with the method for this area routine, is namely assembled into button half-cell or full battery carries out charge-discharge test investigation.
Accompanying drawing explanation
Fig. 1 is the shape appearance figure of the areal cross-section for modifying sulfur electrode of embodiment 1.
Fig. 2 is the shape appearance figure of the areal cross-section of the sulfur electrode that the graphene oxide film of embodiment 2 is modified.
Fig. 3 is the cycle-index-discharge capacity curve of the sulfur electrode that the graphene oxide film of embodiment 3 is modified.
Fig. 4 is the high rate performance curve of the sulfur electrode that the graphene oxide film of embodiment 3 is modified.
Embodiment
Below, in conjunction with embodiment, lithium-sulfur cell of a kind of sulfur electrode based on graphene oxide film modification of the present invention and preparation method thereof is elaborated.
Carbon sulphur composite material is in embodiments of the present invention nucleocapsid structure, but the carbon sulphur composite material of the application is not limited to nucleocapsid structure, can also be mesoporous carbon, carbon nano-tube or other can the carbon guest materials of coated sulphur.
In embodiments of the present invention, described carbon sulphur composite material is CBOS, and its preparation method is solwution method.
the preparation of sulfur electrode of embodiment 1 for modifying
By carbon-sulfur compound, binding agent, conductive agent mixes and ball milling 30 minutes sulfur electrodes for the preparation of modification according to a certain percentage.
Wherein, adhesive is Kynoar, and the ratio in the sulfur electrode for modifying is 5%; Conductive agent is oxidized black, and the ratio in the sulfur electrode for modifying is 10%.
That prepares above method carries out morphology characterization for the electrode slice modified, and as shown in Figure 1, (a) is surface topography map to SEM figure, the shape appearance figure that (b) is cross section; Can find out according to shape appearance figure (a), active material even all be distributed in current collector aluminum foil, can find out according to shape appearance figure (b), the cross section of this active material is the fluff structure of porous.
the preparation of the sulfur electrode that embodiment 2 graphene oxide film is modified
By carbon-sulfur compound, binding agent, conductive agent mixes and ball milling 30 minutes sulfur electrodes for the preparation of modification according to a certain percentage; Wherein, adhesive is Kynoar, and the ratio in the sulfur electrode for modifying is 5%; Conductive agent is oxidized black, and the ratio in the sulfur electrode for modifying is 10%.
Prepare graphene oxide, and be dissolved in ethanol, its concentration is 1mg/mL.
The ethanolic solution of the graphene oxide configured by 10mL evenly drips and is used for the sulfur electrode surface modified, 50 degrees Celsius to 120 degrees Celsius oven dry at 10 square centimeters.
Carry out morphology characterization to the sulfur electrode sheet of graphene oxide film modification prepared by above method, as shown in Figure 2, (a) is surface topography map to SEM figure, the shape appearance figure that (b) is cross section.
Can find out according to shape appearance figure (a), after graphene oxide modification is carried out to the sulfur electrode in embodiment 1, the film of one deck uniformly continous is covered in surface of active material, as can be seen from shape appearance figure (b), at the thickness of the graphene oxide film of surface of active material, this thickness can be controlled by the consumption of graphene oxide solution or concentration.
the performance test of embodiment 3 lithium-sulfur cell
The sulfur electrode that graphite oxide film alkene prepared by Example 2 is modified, and the sulfur electrode for modifying prepared by embodiment 1, be assembled into button cell and carry out charge-discharge test.
The test curve of button cell as Fig. 3, shown in 4.
Can find out according to Fig. 3 cycle-index under 0.5A/g measuring current-specific volume spirogram, the sulfur electrode initial specific capacities of unmodified is about 1050mAh/g, a little more than the initial specific capacities 1010mAh/g of the sulfur electrode that graphene oxide film is modified, this may be relevant with initial condition lithium ion diffusion velocity, but as can be seen from discharge and recharge subsequently, the specific capacity of unmodified sulfur electrode acutely declines, after 100 circulations, specific capacity is only about 500mAh/g, capability retention only has an appointment 47.5%, and each recycle ratio capacity declines about 0.525%; But, sulfur electrode specific capacity after 100 circulations that graphene oxide film is modified still has 910mAh/g, capability retention is about 90%, after 500 circulations, specific capacity is up to 750mAh/g, in whole charge and discharge process, capability retention about 75%, the specific capacity of each circulation declines about 0.05%, compare the sulfur electrode termination capacity 300mAh/g of unmodified, and cyclical stability significantly improves; Its main cause is that graphene oxide film can stop polysulfide to sulfur electrode effectively with outdiffusion, greatly reduces the loss of sulphur, improves the cyclical stability of battery.
Can find out according to cycle-index-specific volume spirogram that Fig. 4 tests under different electric current, when electric current is 0.1A/g, the sulfur electrode that the specific capacity of sulfur electrode in the first five circulation of unmodified is modified compared with graphene oxide film is high, but the sulfur electrode that after 5 circulations, specific capacity is modified a little less than graphene oxide film, 0.5A/g is respectively at electric current, 1A/g, during 2A/g, the specific capacity of the sulfur electrode that graphene oxide film is modified is relatively high, specific capacity under each electric current is almost constant, and specific capacity is very stable; And, when electric current resets to 0.1A/g, the specific capacity that the sulfur electrode of graphene oxide film modification is corresponding returns to about 1120mAh/g, 7.4% is reduced by only relative to initial specific capacities 1210mAh/g, the sulfur electrode specific capacity of unmodified returns to 800mAh/g, decreases 40% relative to initial specific capacities 1350mAh/g.
According to Fig. 3, the test curve analysis of 4, the known electrochemical performance of sulfur electrode with graphene oxide film modification is comparatively superior, although initial specific capacities is lower slightly, the migration initial to lithium ion of possible graphene oxide film has certain inhibition, but along with constantly carrying out of discharge and recharge, battery is constantly activated, show superior cyclical stability and high rate performance, thus the impact that graphene oxide film is not bad on lithium-sulfur cell, simultaneously effectively hinder polysulfide to sulfur electrode with outdiffusion, improve the utilance of sulphur.
Claims (7)
1. the lithium-sulfur cell modified based on graphene oxide film, comprise sulfur electrode, metal lithium electrode and the barrier film be arranged between described sulfur electrode and metal lithium electrode and electrolyte, it is characterized in that: described sulfur electrode is the sulfur electrode modified by graphene oxide film, is M-GO sulfur electrode.
2. a kind of lithium-sulfur cell modified based on graphene oxide film according to claim 1, is characterized in that: the active material in described sulfur electrode is the carbon-sulfur compound prepared by solwution method or additive method.
3. a kind of lithium-sulfur cell modified based on graphene oxide film according to claim 1, is characterized in that the preparation method of the sulfur electrode modified by graphene oxide film is as follows:
(1) by carbon-sulfur compound and conductive agent, adhesive proportionally ball milling mixing, being dissolved in 1-METHYLPYRROLIDONE and preparing slurry and coat collector, preparing the sulfur electrode for modifying after drying;
(2) prepare graphene oxide, be dissolved in ethanol, concentration is 0.5 ~ 5mg/mL;
(3) ethanolic solution of graphene oxide step (2) configured evenly drips the sulfur electrode surface of the modification of preparation in step (1), dries.
4. a kind of lithium-sulfur cell modified based on graphene oxide film according to claim 3, it is characterized in that: the percentage of described adhesive in carbon-sulfur compound, conductive agent and adhesive gross mass is 5 ~ 15%, the percentage of conductive agent in carbon-sulfur compound, conductive agent and adhesive gross mass is 5 ~ 15%, and the percentage of carbon-sulfur compound in carbon-sulfur compound, conductive agent and adhesive gross mass is 70 ~ 90%.
5. a kind of lithium-sulfur cell modified based on graphene oxide film according to claim 4, is characterized in that: described adhesive is Kynoar, the one in polyacrylic acid and sodium carboxymethylcellulose; Described conductive agent is acetylene black or oxidized black.
6. a kind of lithium-sulfur cell modified based on graphene oxide film according to claim 3, is characterized in that: the bake out temperature in step (3) is at 50 degrees Celsius to 120 degrees Celsius.
7. a kind of lithium-sulfur cell modified based on graphene oxide film according to claim 3, it is characterized in that: the liquor capacity that the thickness of described graphene oxide film drips according to the ethanol solution concentration of graphene oxide and unit are controls, and controls at 1 ~ 30nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106129376A (en) * | 2016-08-30 | 2016-11-16 | 上海大学 | The lithium ion battery cathode pole piece of Graphene hollow ball load stannic disulfide composite |
| CN109148863A (en) * | 2018-09-03 | 2019-01-04 | 新奥石墨烯技术有限公司 | lithium titanate-graphene composite material and its preparation method and application |
| JP2019517116A (en) * | 2016-12-27 | 2019-06-20 | エルジー・ケム・リミテッド | Separation membrane and lithium-sulfur battery containing the same |
| WO2022035172A1 (en) * | 2020-08-10 | 2022-02-17 | 주식회사 엘지에너지솔루션 | Anode coating for lithium secondary battery, manufacturing method therefor, and anode and lithium secondary battery, each including same coating |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106129376A (en) * | 2016-08-30 | 2016-11-16 | 上海大学 | The lithium ion battery cathode pole piece of Graphene hollow ball load stannic disulfide composite |
| JP2019517116A (en) * | 2016-12-27 | 2019-06-20 | エルジー・ケム・リミテッド | Separation membrane and lithium-sulfur battery containing the same |
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| CN109148863A (en) * | 2018-09-03 | 2019-01-04 | 新奥石墨烯技术有限公司 | lithium titanate-graphene composite material and its preparation method and application |
| WO2022035172A1 (en) * | 2020-08-10 | 2022-02-17 | 주식회사 엘지에너지솔루션 | Anode coating for lithium secondary battery, manufacturing method therefor, and anode and lithium secondary battery, each including same coating |
| CN114556631A (en) * | 2020-08-10 | 2022-05-27 | 株式会社Lg新能源 | Coating material for positive electrode of lithium secondary battery, method for preparing same, and positive electrode and lithium secondary battery comprising same |
| JP2023500942A (en) * | 2020-08-10 | 2023-01-11 | エルジー エナジー ソリューション リミテッド | Positive electrode coating material for lithium secondary battery, manufacturing method thereof, positive electrode and lithium secondary battery containing the coating material |
| JP7410291B2 (en) | 2020-08-10 | 2024-01-09 | エルジー エナジー ソリューション リミテッド | A positive electrode coating material for a lithium secondary battery, a method for producing the same, a positive electrode including the coating material, and a lithium secondary battery |
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