CN105609768A - Preparation method for shell-core structured graphene/carbon coated composite material doped with lithium sulfide - Google Patents
Preparation method for shell-core structured graphene/carbon coated composite material doped with lithium sulfide Download PDFInfo
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- CN105609768A CN105609768A CN201610096058.XA CN201610096058A CN105609768A CN 105609768 A CN105609768 A CN 105609768A CN 201610096058 A CN201610096058 A CN 201610096058A CN 105609768 A CN105609768 A CN 105609768A
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/366—Composites as layered products
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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 invention provides a preparation method for a shell-core structured graphene/carbon coated composite material doped with lithium sulfide. The preparation method comprises the following steps of (1) mixing commercial lithium sulfide and metal oxide powder, placing the mixture in a sealed ball milling tank, and placing the mixture in a ball milling machine for ball milling to obtain doping nanometer lithium sulfide; (2) adding a carbon source to ethanol while stirring, and dissolving the carbon source to form an ethanol solution containing the carbon source; (3) dispersing the obtained nanometer lithium sulfide in the ethanol solution, and dropwise adding the ethanol solution containing the carbon source to a suspension liquid to obtain carbon coated lithium sulfide; and (4) adding the carbon coated lithium sulfide and graphene to tetrahydrofuran, and carrying out ultrasonic reaction to obtain the shell-core structured graphene/carbon coated composite material doped with the lithium sulfide. With the doping of metal ions, a lithium sulfide crystal structure can be changed, the conductivity of a lithium sulfide body is favorably improved, and the electrochemical performance of the lithium sulfide body is improved.
Description
Technical field
The present invention relates to nano material synthetic, particularly a kind of preparation method of lithium sulfur battery anode material.
Background technology
Lithium-sulfur cell is taking lithium metal as negative pole, and elemental sulfur is anodal battery system. Lithium-sulfur cell there are two discharge platforms (being about 2.4V and 2.1V), but its electrochemical reaction mechanism more complicated. Lithium-sulfur cell has specific energy high (2600Wh/kg), specific capacity high (1675mAh/g), low cost and other advantages, is considered to very promising battery of new generation. But there is at present that active material utilization is low, cycle life is low and the problem such as poor stability, this is seriously restricting the development of lithium-sulfur cell. Cause the main cause of the problems referred to above to have the following aspects: (1) elemental sulfur is electronics and ion insulator, and room-temperature conductivity is low by (5 × 10-30S·cm-1), owing to there is no the sulphur of ionic state, thereby as positive electrode activation difficulty; (2) poly-many lithium sulfides of the state Li of height producing in electrode process2Sn(8 > n >=4) are soluble in electrolyte, form concentration difference between both positive and negative polarity, under the effect of concentration gradient, move to negative pole, and the high poly-many lithium sulfides of state are reduced into the many lithium sulfides of oligomeric state by lithium metal. Along with the carrying out of above reaction, the many lithium sulfides of oligomeric state are assembled at negative pole, finally between two electrodes, form concentration difference, move to again positive pole and are oxidized to the high poly-many lithium sulfides of state. This phenomenon is called as and flies shuttle effect, has reduced the utilization rate of sulphur active material. Insoluble Li simultaneously2S and Li2S2Be deposited on cathode of lithium surface, further worsened the performance of lithium-sulfur cell; (3) reaction end product Li2S is electronic body equally, can be deposited on sulfur electrode, and lithium ion migration velocity in solid-state lithium sulfide is slow, makes electrochemical reaction dynamics speed slack-off; (4) sulphur and end product Li2The density difference of S, after sulphur is by lithiumation volumetric expansion about 79%, easily cause Li2The efflorescence of S, causes the safety problem of lithium-sulfur cell. Above-mentioned deficiency is restricting the development of lithium-sulfur cell, and this is also that current lithium-sulfur cell research needs the Important Problems solving.
In lithium-sulfur cell system, because sulfenyl positive pole is not containing lithium, need to provide lithium source as negative pole with lithium metal, but in cyclic process, lithium anode is easily in Surface Creation Li dendrite and efflorescence, not only there is potential safety hazard, and consume clean electrolyte and cause lithium-sulfur rechargeable battery to lose efficacy in advance, limited the application of lithium-sulfur cell. Researcher adopts Li2S replaces sulfenyl positive pole, or by sulfenyl positive pole in advance after lithiumation, the silicon, tin that adopt carbon negative pole or have higher capacity are as negative material, object is to eliminate the impact of lithium anode, the theoretical capacity of lithium sulfide positive pole is higher, is 1166mAh/g, but it the same with sulfur electrode be also insulating properties material, need to add conductive additive, and carry out special coated processing and improve its electro-chemical activity.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of the coated doping lithium sulfide composite of a kind of graphene/carbon of nucleocapsid structure, preparation method is simple, the Graphene that electric conductivity is good and carbon shell provide conductive network, doped metal ion changes lithium sulfide lattice structure simultaneously, improve its electric conductivity, and then improve its electro-chemical activity.
The invention provides the preparation method of the coated doping lithium sulfide composite of a kind of graphene/carbon of nucleocapsid structure:
(1) in the glove box of inert gas shielding, commercial lithium sulfide is mixed with metal oxide powder, then pack in the ball grinder of sealing, reinstall ball mill and carry out ball milling, obtain dopen Nano lithium sulfide.
(2) by joining in ethanol under carbon source stirring, dissolve the ethanolic solution that formation contains carbon source.
(3) the nanometer lithium sulfide obtaining is distributed in ethanolic solution; constantly stir and form suspension; again the ethanolic solution that contains carbon source is added drop-wise in suspension; stirring at room temperature reaction; then solvent evaporated; join pyroreaction in the Muffle furnace of inert gas shielding, obtain the coated lithium sulfide of carbon.
(4) lithium sulfide coated carbon and Graphene are joined in oxolane, ultrasonic reaction, then evaporating solvent obtains the coated doping lithium sulfide composite of graphene/carbon.
In step (1), the mass ratio of lithium sulfide and metal oxide is 100:0.5-5; Metal oxide can be one or more in magnesia, manganese dioxide, cupric oxide, aluminium oxide, nickel oxide; Ball-milling Time is 0.5-3 hour, and ball milling speed is 500-3000 rev/min.
In step (2), organic carbon source is one or more in sucrose, glucose, starch, cellulose; The mass concentration that forms solution is 5-10%.
Step (3) lithium sulfide ethanolic solution mass concentration is 5-10%; The volume ratio that contains carbon source ethanolic solution and lithium sulfide ethanolic solution is 1:1-10; The stirring at room temperature reaction time is 1-5 hour, and the reaction temperature in Muffle furnace is 800-900 DEG C; Reaction time is 1-5 hour.
The mass ratio of the coated lithium sulfide of Graphene and carbon is 1:10-100 in step (4); Ultrasonic time is 0.5-3 hour.
The present invention has following beneficial effect: (1) Graphene and carbon all have the electrical conductivity of superelevation, and the electrical conductivity of material can be effectively improved on the surface that Graphene and carbon are coated on lithium sulfide; (2) doped metal ion can change lithium sulphite crystal structure, is conducive to the raising of lithium sulfide self-conductance rate, improves its chemical property.
Brief description of the drawings
Fig. 1 is the SEM figure of the coated doping lithium sulfide composite of the graphene/carbon prepared of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, preferably embodiment of the present invention is described in further detail:
Embodiment 1
(1) in the glove box of inert gas shielding, commercial 100mg lithium sulfide is mixed with 5mg magnesium oxide powder, then pack in the ball grinder of sealing, reinstall ball mill and carry out ball milling 0.5 hour, ball milling speed is 3000 revs/min, obtains nanometer lithium sulfide.
(2) sucrose is under agitation joined in ethanol, dissolve the sucrose ethanolic solution that forms mass concentration 10%.
(3) the nanometer lithium sulfide obtaining is distributed in ethanolic solution; constantly stir the 50ml suspension that forms mass concentration 10%; again the sucrose ethanolic solution of 50ml is added drop-wise in suspension; stirring at room temperature reaction 5 hours; then solvent evaporated; join in the Muffle furnace of inert gas shielding and react 5 hours at 800 DEG C, obtain the coated lithium sulfide of carbon.
(4) lithium sulfide coated 100mg carbon and 10mg Graphene are joined in oxolane, ultrasonic reaction 0.5 hour, then evaporating solvent obtains the coated doping lithium sulfide composite of graphene/carbon.
Embodiment 2
(1) in the glove box of inert gas shielding, commercial 100mg lithium sulfide is mixed with 0.5mg manganese dioxide powder, then pack in the ball grinder of sealing, reinstall ball mill and carry out ball milling 3 hours, ball milling speed is 500 revs/min, obtains nanometer lithium sulfide.
(2) by joining in ethanol under glucose stirring, dissolve the glucose ethanolic solution that forms mass concentration 5%.
(3) the nanometer lithium sulfide obtaining is distributed in ethanolic solution; constantly stir the 50ml suspension that forms mass concentration 5%; again 5ml glucose ethanolic solution is added drop-wise in suspension; stirring at room temperature reaction 1 hour; then solvent evaporated; join in the Muffle furnace of inert gas shielding 900 DEG C of pyroreactions 1 hour, obtain the coated lithium sulfide of carbon.
(4) lithium sulfide coated 100mg carbon and 1mg Graphene are joined in oxolane, ultrasonic reaction 3 hours, then evaporating solvent obtains the coated doping lithium sulfide composite of graphene/carbon.
Embodiment 3
(1) in the glove box of inert gas shielding, commercial 100mg lithium sulfide is mixed with 2.5mg cupric oxide powder, then pack ball mill into and carry out ball milling 1 hour, ball milling speed is 2000 revs/min, obtains nanometer lithium sulfide.
(2) by joining in ethanol under starch stirring, dissolve the starch ethanol solution that forms mass concentration 7%.
(3) the nanometer lithium sulfide obtaining is distributed in ethanolic solution; constantly stir the 50ml suspension that forms mass concentration 6%; again 10ml starch ethanol solution is added drop-wise in suspension; stirring at room temperature reaction 2 hours; then solvent evaporated; join in the Muffle furnace of inert gas shielding and react 3.5 hours at 850 DEG C, obtain the coated lithium sulfide of carbon.
(4) lithium sulfide coated 100mg carbon and 5mg Graphene are joined in oxolane, ultrasonic reaction 1 hour, then evaporating solvent obtains the coated doping lithium sulfide composite of graphene/carbon.
Embodiment 4
(1) in the glove box of inert gas shielding, commercial 100mg lithium sulfide is mixed with 1mg alumina powder, then pack ball mill into and carry out ball milling 2 hours, ball milling speed is 1000 revs/min, obtains nanometer lithium sulfide.
(2) by joining in ethanol under cellulose stirring, dissolve the cellulosic ethanol solution that forms mass concentration 6%.
(3) the nanometer lithium sulfide obtaining is distributed in ethanolic solution; constantly stir the 50ml suspension that forms mass concentration 7%; again 25ml cellulosic ethanol solution is added drop-wise in suspension; stirring at room temperature reaction 3 hours; then solvent evaporated; join in the Muffle furnace of inert gas shielding and react 4 hours at 820 DEG C, obtain the coated lithium sulfide of carbon.
(4) lithium sulfide coated 100mg carbon and 3mg Graphene are joined in oxolane, ultrasonic reaction 2 hours, then evaporating solvent obtains the coated doping lithium sulfide composite of graphene/carbon.
Embodiment 5
(1) in the glove box of inert gas shielding, commercial 100mg lithium sulfide is mixed with 3mg nickel oxide powder, then pack ball mill into and carry out ball milling 1.5 hours, ball milling speed is 1500 revs/min, obtains nanometer lithium sulfide.
(2) by joining in ethanol under sucrose stirring, dissolve the sucrose ethanolic solution that forms mass concentration 8%.
(3) the nanometer lithium sulfide obtaining is distributed in ethanolic solution; constantly stir the 50ml suspension that forms mass concentration 8%; again 30ml sucrose ethanolic solution is added drop-wise in suspension; stirring at room temperature reaction 4 hours; then solvent evaporated; join in the Muffle furnace of inert gas shielding and react 3 hours at 870 DEG C, obtain the coated lithium sulfide of carbon.
(4) lithium sulfide coated 100mg carbon and 7mg Graphene are joined in oxolane, ultrasonic reaction 2.5 hours, then evaporating solvent obtains the coated doping lithium sulfide composite of graphene/carbon.
The preparation and property test of electrode; By electrode material, acetylene black and PVDF in mass ratio 80:10:10 in NMP, mix, be coated on aluminium foil is electrode film, metal lithium sheet is to electrode, CELGARD2400 is barrier film, the LiTFSI/DOL-DME (volume ratio 1:1) of 1mol/L is electrolyte, the LiNO3 of 1mol/L is additive, is assembled into button cell being full of in Ar glove box, adopts Land battery test system to carry out constant current charge-discharge test. Charging/discharging voltage scope is 1-3V, and current density is 0.1C, and performance is as shown in table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Specific discharge capacity after circulation first | 980mAh/g | 950mAh/g | 920mAh/g | 950mAh/g | 930mAh/g |
| Specific discharge capacity after 100 circulations | 850mAh/g | 810mAh/g | 800mAh/g | 820mAh/g | 830mAh/g |
Fig. 1 is the SEM figure that the present invention prepares positive electrode, and as can be seen from the figure coated evengranular being distributed on Graphene surface of lithium sulfide of carbon, is conducive to improve the chemical property of material.
Above content is in conjunction with concrete preferred embodiment further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations. For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Claims (7)
1. a preparation method for the coated doping lithium sulfide composite of the graphene/carbon of nucleocapsid structure, is characterized in that, comprises following step:
Step (1): in the glove box of inert gas shielding, commercial lithium sulfide is mixed with metal oxide powder, then pack in the ball grinder of sealing, reinstall ball mill and carry out ball milling, obtain dopen Nano lithium sulfide;
Step (2): join in ethanol under carbon source is stirred, dissolve and form the ethanolic solution that contains carbon source;
Step (3): the nanometer lithium sulfide obtaining is distributed in ethanolic solution, constantly stir and form suspension, again the ethanolic solution that contains carbon source is added drop-wise in suspension, stirring at room temperature reaction, then solvent evaporated, join in the Muffle furnace of inert gas shielding and react, obtain the coated lithium sulfide of carbon;
Step (4) joins lithium sulfide coated carbon and Graphene in oxolane, ultrasonic reaction, and then evaporating solvent obtains the coated doping lithium sulfide composite of graphene/carbon of nucleocapsid structure.
2. the method for claim 1, is characterized in that, in described step (1), the mass ratio of lithium sulfide and metal oxide is 100:0.5-5.
3. the method for claim 1, is characterized in that, in described step (1), metal oxide adopts one or more in magnesia, manganese dioxide, cupric oxide, aluminium oxide, nickel oxide.
4. the method for claim 1, is characterized in that, in described step (1), Ball-milling Time is 0.5-3 hour, and ball milling speed is 500-3000 rev/min.
5. the method for claim 1, is characterized in that, in described step (2), organic carbon source is one or more in sucrose, glucose, starch, cellulose; The mass concentration of the ethanolic solution that formation contains carbon source is 5-10%.
6. the method for claim 1, is characterized in that, described step (3) lithium sulfide ethanolic solution mass concentration is 5-10%; The volume ratio that contains carbon source ethanolic solution and lithium sulfide ethanolic solution is 1:1-10; The stirring at room temperature reaction time is 1-5 hour, and the reaction temperature in Muffle furnace is 800-900 DEG C; Reaction time is 1-5 hour.
7. the method for claim 1, is characterized in that, the mass ratio of the coated lithium sulfide of Graphene and carbon is 1:10-100 in described step (4); Ultrasonic time is 0.5-3 hour.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105609738A (en) * | 2016-02-21 | 2016-05-25 | 钟玲珑 | Preparation method for shell-core structured positive electrode material doped with carbon and lithium sulfide |
| CN105914369A (en) * | 2016-05-31 | 2016-08-31 | 浙江大学 | Nanoscale carbon coated lithium sulfide composite material, preparation method and application thereof |
| WO2017139997A1 (en) * | 2016-02-21 | 2017-08-24 | 肖丽芳 | Method for fabricating anode material doped with carbon lithium sulfide core-shell structure |
| WO2017139993A1 (en) * | 2016-02-21 | 2017-08-24 | 肖丽芳 | Method for preparing doped lithium sulfide composite coated with graphene/carbon and having core-shell structure |
| CN107331845A (en) * | 2017-07-05 | 2017-11-07 | 陈建超 | A kind of graphene battery anode composite material |
| CN108417811A (en) * | 2018-03-26 | 2018-08-17 | 电子科技大学 | A kind of carbon coating club shaped structure ternary ferrimanganic sulfide graphene composite material and its synthetic method |
| CN109346697A (en) * | 2018-10-12 | 2019-02-15 | 桑德集团有限公司 | Positive electrode active materials and preparation method thereof, solid lithium battery |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105609738A (en) * | 2016-02-21 | 2016-05-25 | 钟玲珑 | Preparation method for shell-core structured positive electrode material doped with carbon and lithium sulfide |
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| WO2017139993A1 (en) * | 2016-02-21 | 2017-08-24 | 肖丽芳 | Method for preparing doped lithium sulfide composite coated with graphene/carbon and having core-shell structure |
| CN105914369A (en) * | 2016-05-31 | 2016-08-31 | 浙江大学 | Nanoscale carbon coated lithium sulfide composite material, preparation method and application thereof |
| CN107331845A (en) * | 2017-07-05 | 2017-11-07 | 陈建超 | A kind of graphene battery anode composite material |
| CN108417811A (en) * | 2018-03-26 | 2018-08-17 | 电子科技大学 | A kind of carbon coating club shaped structure ternary ferrimanganic sulfide graphene composite material and its synthetic method |
| CN108417811B (en) * | 2018-03-26 | 2021-02-02 | 电子科技大学 | Carbon-coated rod-shaped structure ternary iron-manganese sulfide graphene composite material and synthesis method thereof |
| CN109346697A (en) * | 2018-10-12 | 2019-02-15 | 桑德集团有限公司 | Positive electrode active materials and preparation method thereof, solid lithium battery |
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Application publication date: 20160525 |