CN104393304A - Lithium-selenium battery positive electrode material, preparation method thereof and lithium-selenium battery - Google Patents
Lithium-selenium battery positive electrode material, preparation method thereof and lithium-selenium battery Download PDFInfo
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- CN104393304A CN104393304A CN201410638938.6A CN201410638938A CN104393304A CN 104393304 A CN104393304 A CN 104393304A CN 201410638938 A CN201410638938 A CN 201410638938A CN 104393304 A CN104393304 A CN 104393304A
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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
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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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
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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 of a lithium-selenium battery. The preparation method comprises the steps of providing an oxidized graphene dispersing liquid with saturated inert atmosphere; feeding hydrogen selenide gas to the oxidized graphene dispersing liquid with saturated inert atmosphere, reducing the oxidized graphene to graphene by taking the insert atmosphere as carrier gas, and meanwhile, generating elemental selenium on the surface of the graphene to obtain an elemental selenium-graphene dispersing liquid; performing solvent thermal treatment on the selenium-loaded graphene dispersing liquid to obtain graphene-based gel; and drying the graphene-based gel. The invention further provides a lithium-selenium battery positive electrode material and a lithium-selenium battery using the positive electrode material.
Description
Technical field
The present invention relates to a kind of lithium selenium cell positive electrode and preparation method, and lithium selenium cell.
Background technology
Lithium selenium cell is a kind of Novel lithium secondary cell system, it utilizes elemental selenium as positive pole, lithium metal is negative pole, realizes mutually changing between chemical energy and electric energy by the chemical reaction between selenium and lithium, has the energy density higher than existing anode material for lithium-ion batteries.Chinese patent application CN103187559 A and CN103178246 A individually discloses elemental selenium and porous carrier or mesoporous supports Hybrid Heating, thus make elemental selenium be dispersed in the duct of porous carrier or mesoporous supports, the lithium secondary cell with high capacity with good circulation stability and high rate performance can be obtained.
But, the duct of poromerics or mesoporous material is minimum, said method is difficult to make elemental selenium fully and enter micropore canals equably, and the elemental selenium being introduced into duct makes blockage of the micro orifice, be difficult to make more elemental selenium fully enter poromerics or mesoporous material inside, cause elemental selenium and carrier cannot even compound, thus make said method be difficult to be applied to during actual industrialization produces.
Summary of the invention
In view of this, necessaryly provide a kind of lithium selenium cell positive electrode and preparation method thereof, and lithium selenium cell.
A preparation method for lithium selenium cell positive electrode, it comprises the following steps: provide the graphene oxide dispersion that an inert atmosphere is saturated; In the graphene oxide dispersion that this inert atmosphere is saturated, pass into hydrogen selenide gas, take inert atmosphere as carrier gas, generates elemental selenium, obtain elemental selenium-graphene dispersing solution while described graphene oxide is reduced to Graphene at graphenic surface; The graphene dispersing solution of described load selenium is carried out solvent thermal reaction, obtains a graphene-based gel; And described graphene-based gel is carried out drying process, to obtain a lithium selenium cell positive electrode.
A kind of lithium selenium cell positive electrode, comprise three-dimensional porous graphene macroform and multiple elemental selenium be distributed in this three-dimensional porous graphene macroform, wherein, described three-dimensional porous graphene macroform is mutually overlap by multiple graphene film the self supporting structure formed, have multiple hole between the plurality of graphene film, described multiple elemental selenium is uniformly distributed in the plurality of hole and multiple graphene sheet layer surface.
A kind of lithium selenium cell, comprise positive pole, negative pole, barrier film and electrolyte, described positive pole comprises a collector and is arranged at the above-mentioned positive electrode on this collector.
Compared with prior art, the present invention first utilizes redox reaction by the graphenic surface of elemental selenium in-situ preparation in dispersion, again the Graphene of dispersion is originally overlapped mutually, be assembled into porous macroscopic material, thus in the duct making elemental selenium be arranged on this porous macroscopic material uniformly and multiple graphene sheet layer surface, form Graphene and the complete mixed uniformly composite construction of elemental selenium, be conducive to the chemical property improving lithium selenium cell further.Further, this complex method is simple, is suitable for the application of suitability for industrialized production.
Accompanying drawing explanation
The flow chart of the preparation method of the lithium selenium cell positive electrode that Fig. 1 provides for the embodiment of the present invention.
The stereoscan photograph figure of the lithium selenium cell positive electrode that Fig. 2 provides for the embodiment of the present invention.
The structural representation of the lithium selenium cell that Fig. 3 provides for the embodiment of the present invention.
The first charge-discharge curve chart of the lithium selenium cell that Fig. 4 provides for the embodiment of the present invention.
Main element symbol description
| 10 | Lithium selenium cell |
| 12 | Positive plate |
| 122 | Collector |
| 124 | Positive electrode |
| 14 | Negative plate |
| 16 | Barrier film |
| 18 | Electrolyte |
Following embodiment will further illustrate the present invention in conjunction with above-mentioned accompanying drawing.
Embodiment
Below in conjunction with the accompanying drawings and the specific embodiments to the preparation method of lithium selenium cell positive electrode provided by the invention, its preparation method and lithium selenium cell are described in further detail.
Refer to Fig. 1, the embodiment of the present invention provides a kind of preparation method of lithium selenium cell positive electrode, and the method comprises the following steps:
S1: the graphene oxide dispersion that an inert atmosphere is saturated is provided;
S2: pass into hydrogen selenide gas in the graphene oxide dispersion that this inert atmosphere is saturated, inert atmosphere is carrier gas, generates elemental selenium, obtain elemental selenium-graphene dispersing solution while described graphene oxide is reduced to Graphene at graphenic surface;
S3: described elemental selenium-graphene dispersing solution is carried out solvent thermal reaction, makes Graphene be assembled into porous macroscopic material; And
S4: this porous macroscopic material is carried out drying process, obtain lithium selenium cell positive electrode.
In step S1, solvent in described graphene oxide dispersion can be water, also can be organic solvent, as one or several in ethanol, isopropyl alcohol, ethylene glycol, DMF (DMF), 1-METHYLPYRROLIDONE (NMP), oxolane.Certainly, the selection of described solvent be not limited to above-mentioned enumerate several, as long as described graphene oxide can be disperseed well.In described graphene oxide dispersion, the concentration of graphene oxide can be 0.05 ~ 30 mg/mL, and preferably, its concentration is 1 ~ 5 mg/mL.
The preparation method of described graphene oxide dispersion is: be added to by graphite oxide powder in described solvent; And adopt the mode such as ultrasonic disperse, stirring that the lamella of graphite oxide is peeled off mutually, and be uniformly dispersed, obtain this graphene oxide dispersion.In the present embodiment, 300 milligrams of graphite oxide powders are added in 100 ml deionized water, after 2.0 hours, obtain the graphene oxide dispersion that a concentration is 3 mg/mL in the ultrasonic agitation of 200 watts of power.
After obtaining this graphene oxide dispersion, in this graphene oxide dispersion, pass into inert gas further, make inert gas saturated in this graphene oxide dispersion.This inert gas can be nitrogen and rare gas, as argon gas, in one or more.
In step S2, graphene oxide is reduced to Graphene by this hydrogen selenide, obtains elemental selenium and water simultaneously, and reaction equation as the formula (1).
Graphene oxide+H
2se → Graphene+H
2o+Se ↓ (1)
Using inert gas as carrier gas during the passing into of described hydrogen selenide gas.The component of the lithium selenium cell positive electrode that the intake of described hydrogen selenide gas can obtain according to the concentration of graphene oxide dispersion, quality and expection regulates.This hydrogen selenide reacts in surface of graphene oxide, and the elemental selenium of generation is attached to graphenic surface uniformly, can be adsorbed, or connected by chemical bond with Graphene by Van der Waals force.This in-situ preparation is unformed or graininess in the elemental selenium of graphenic surface, and size is less than 1 micron, is preferably below 100 nanometers.
The reaction temperature of the redox reaction in step S2 should lower than the boiling point of described solvent, and should lower than the burning-point of hydrogen selenide, to prevent or to reduce described solvent and hydrogen selenide loss in this step.Particularly, described reaction temperature is between 5 ~ 300 DEG C.When described solvent is water, this reaction temperature is between 5 ~ 100 DEG C.In the present embodiment, described reaction temperature is 75 DEG C.This redox reaction is carried out in inert gas shielding.
While passing into hydrogen selenide gas, also can proceed sonic oscillation makes reaction more abundant, and obtains homodisperse elemental selenium-graphene dispersing solution.
In step S3, the temperature of described solvent thermal reaction be 50 ~ 217 DEG C the fusing point of selenium (217 DEG C be), the time is 0.1 ~ 120 hour.Preferably, the temperature of described solvent thermal reaction is 70 ~ 180 DEG C, and the time is 2 ~ 48 hours.During concrete operations, described elemental selenium-graphene dispersing solution can be placed in an airtight high-pressure closed vessel, and heat in a Muffle furnace, the pressure of course of reaction is more than or equal to 1 atmospheric pressure.Described solvent thermal reaction can make the Graphene of described load elemental selenium mutually overlap on the one hand and be assembled into porous macroscopic self supporting structure, can promote being uniformly distributed of selenium on the other hand.In the present embodiment, by described elemental selenium-graphene dispersing solution 150 DEG C of heat treated 6 hours, to obtain this porous macroscopic material.The porous macroscopic material that this obtains is macroscopical block structure of a self-supporting, can directly take out from reaction vessel.
In step S4, the object of described drying is solvent remaining in the described porous macroscopic material of removing.But in order to prevent the distillation of selenium, described drying should be carried out at a lower temperature.Particularly, the drying means of described graphene dispersing solution can for the heat drying under freeze drying, drying at room temperature, supercritical drying, vacuum and heating drying, normal heating drying or protective gas.In the present embodiment, the method for employing vacuum and heating drying removes the solvent in described porous macroscopic material, to obtain described positive electrode.Particularly, gained porous macroscopic material is placed in a vacuum drying oven and carries out drying.Described vacuum and heating drying can remove rapidly the solvent of porous macroscopic material internal, keeps its microcosmic loose structure simultaneously.Preferably, the temperature of described vacuum and heating drying is between 0 DEG C ~ 217 DEG C.Preferably, the temperature of described vacuum and heating drying is between 20 DEG C ~ 100 DEG C.Particularly, in the present embodiment, the temperature of described vacuum and heating drying is 60 DEG C.In addition, when adopting freeze drying, temperature is between-196 DEG C ~ 0 DEG C.
Refer to Fig. 2, the lithium selenium cell positive electrode utilizing the method for the present embodiment to prepare, comprise as elemental selenium carrier porous macroscopic material and be multiplely arranged in this porous macroscopic material hole and the elemental selenium on multiple graphene sheet layer surface.Described porous macroscopic material is mutually overlapped by multiple graphene film and is formed, these graphene films are network-like in this macroscopic body to be uniformly distributed, multiple hole is formed between these graphene films, the plurality of elemental selenium is then distributed in the surface of these graphene films equably with amorphous state, and combines closely with described Graphene.The porosity of described porous macroscopic material is at 0.05 ~ 4 cm
3between/g, the pore-size distribution of described hole is between 0.4 nm ~ 10 μm.Preferably, the porosity of described three-dimensional porous graphene macroform is at 0.1 ~ 3 cm
3between/g, the pore-size distribution of described hole is between 1 nm ~ 5 μm, and preferably, pore-size distribution is between 1 nm ~ 500 nm.
In described lithium selenium cell positive electrode, between elemental selenium and graphene film except being attracted each other by Van der Waals force, also there is certain chemical bonding effect.Therefore, this lithium selenium cell positive electrode has comparatively stable structure, ensures the stability of lithium selenium cell charge-discharge performance.
In described lithium selenium cell positive electrode, the mass percentage of described elemental selenium can be 5% ~ 95%.Described lithium selenium cell positive electrode can only be made up of elemental selenium and Graphene.In this lithium selenium cell positive electrode, the mass percentage of each composition controls by regulating the intake of hydrogen selenide.In the present embodiment, the mass percentage of described elemental selenium is 60%, and the mass percentage of described graphene macroform is 40%.
In described lithium selenium cell positive electrode, described porous macroscopic material mainly plays carrier and the electric action of elemental selenium.On the one hand, this porous macroscopic material can adsorb elemental selenium, in the hole enabling selenium stably be dispersed between graphene film well and graphene film surface; On the other hand, the conductivity that Graphene itself is excellent can be the conductive network that this positive electrode provides good.Meanwhile, the porous buffer structure that this lithium selenium cell positive electrode has has good confinement effect to the many selenides of discharge and recharge product.
Refer to Fig. 3, the embodiment of the present invention also provides a kind of lithium selenium cell 10 applying above-mentioned positive electrode, and it comprises positive plate 12, negative plate 14, barrier film 16 and electrolyte 18.Described positive plate 12 comprises a collector 122 and is arranged at the above-mentioned lithium selenium cell positive electrode 124 on this collector 122, comprises the elemental selenium in porous macroscopic material and multiple hole being arranged on this porous macroscopic material.
Described collector can be aluminium foil, nickel foam, stainless (steel) wire or painting carbon aluminium foil etc.Described negative plate is metal lithium sheet, lithium alloys sheet, lithium/carbon composite material sheet etc.Described electrolyte is two (trimethyl fluoride sulfonyl) imine lithium (LiTFSI), lithium hexafluoro phosphate (LiPF6) etc.; Described electrolyte solvent used is ethers, as glycol dimethyl ether (TEGDME), dimethyl ether (DME) etc.; Described barrier film is the co-polymer membrane etc. of polypropylene (PP) microporous barrier, polyethylene (PE) microporous barrier or propylene and ethene.
In the present embodiment, take aluminium foil as collector, take metal lithium sheet as negative plate, take microporous polypropylene membrane as barrier film, with 1.5 mol/L bis-(trimethyl fluoride sulfonyl) imine lithiums (LiTFSI)/DOX (DOL)+dimethyl ether (DME) (volume ratio 1:1) for electrolyte is assembled into a lithium selenium cell.The first charge-discharge curve of this lithium selenium cell refers to Fig. 4, and as seen from Figure 4, the discharge capacity first of this lithium selenium cell can reach 640 mAh/g.
Compared with prior art, the present invention is first by the graphenic surface of elemental selenium in-situ preparation in dispersion, again the Graphene of dispersion is originally overlapped mutually, be assembled into porous macroscopic material, thus make elemental selenium be arranged in the hole of this porous macroscopic material uniformly, form Graphene and the complete mixed uniformly composite construction of elemental selenium, be conducive to the chemical property improving lithium selenium cell further.Further, this complex method is simple, is suitable for the application of suitability for industrialized production.
In addition, those skilled in the art also can do other changes in spirit of the present invention, and certainly, these changes done according to the present invention's spirit, all should be included within the present invention's scope required for protection.
Claims (12)
1. a preparation method for lithium selenium cell positive electrode, it comprises the following steps:
The graphene oxide dispersion that one inert atmosphere is saturated is provided;
In the graphene oxide dispersion that this inert atmosphere is saturated, pass into hydrogen selenide gas, take inert atmosphere as carrier gas, generates elemental selenium, obtain elemental selenium-graphene dispersing solution while described graphene oxide is reduced to Graphene at graphenic surface;
Described elemental selenium-graphene dispersing solution is carried out solvent thermal reaction, makes Graphene be assembled into porous macroscopic material; And
This porous macroscopic material is carried out drying process, obtain lithium selenium cell positive electrode.
2. the preparation method of lithium selenium cell positive electrode as claimed in claim 1, it is characterized in that, the temperature of described solvent thermal reaction is 50 DEG C ~ 217 DEG C, and the time is 0.1 hour ~ 120 hours.
3. the preparation method of lithium selenium cell positive electrode as claimed in claim 1, it is characterized in that, in described graphene oxide dispersion, the concentration of graphene oxide is 0.05 mg/mL ~ 30 mg/mL.
4. the preparation method of lithium selenium cell positive electrode as claimed in claim 1; it is characterized in that, the mode of described drying is the one in the heat drying under the dry and protective gas of freeze drying, drying at room temperature, supercritical drying, vacuum and heating drying, normal heating.
5. the preparation method of lithium selenium cell positive electrode as claimed in claim 4, it is characterized in that, the mode of described drying is freeze drying or heat drying, and temperature during described drying is between-196 DEG C ~ 217 DEG C.
6. the preparation method of lithium selenium cell positive electrode as claimed in claim 1, it is characterized in that, be 5 DEG C ~ 300 DEG C passing into the reaction temperature controlling redox graphene in hydrogen selenide gas process.
7. a lithium selenium cell positive electrode, comprise a porous macroscopic material and multiple elemental selenium, described porous macroscopic material is mutually overlapped by multiple graphene film and is formed, have multiple hole between the plurality of graphene film, the plurality of elemental selenium is arranged in this porous macroscopic material hole and the plurality of graphene film surface.
8. lithium selenium cell positive electrode as claimed in claim 7, it is characterized in that, described porous macroscopic material is a self supporting structure.
9. lithium selenium cell positive electrode as claimed in claim 7, it is characterized in that, the mass percentage of described elemental selenium is between 5% ~ 95%.
10. lithium selenium cell positive electrode as claimed in claim 7, it is characterized in that, described multiple elemental selenium is evenly distributed on the surface of the plurality of graphene film with amorphous state.
11. lithium selenium cell positive electrodes as claimed in claim 8, is characterized in that, the porosity of described porous macroscopic material is 0.05cm
3/ g ~ 4cm
3/ g, the pore-size distribution of described multiple hole is between 0.4 nm ~ 10 μm.
12. 1 kinds of lithium selenium cells, comprise positive plate, negative plate, barrier film and electrolyte, it is characterized in that, described positive plate comprises collector and the lithium selenium cell positive electrode according to any one of claim 7 ~ 11, and described lithium selenium cell positive electrode is arranged at the surface of this collector.
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Cited By (14)
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| WO2017053144A1 (en) | 2015-09-22 | 2017-03-30 | Institute Of Chemistry, Chinese Academy Of Sciences | Method of preparing and application of carbon-selenium composites |
| CN106571460A (en) * | 2015-10-09 | 2017-04-19 | 中国科学院上海硅酸盐研究所 | Binder-free selenium cathode material with self-supporting structure and preparation method thereof |
| CN106784660A (en) * | 2016-12-02 | 2017-05-31 | 吉林大学 | Nickel foam as interlayer Se TiO2/ NFF lithium selenium secondary cells and preparation method thereof |
| CN107706404A (en) * | 2017-11-23 | 2018-02-16 | 东北师范大学 | A kind of selenium cladding tin ash/graphene nanocomposite material prepares and its application |
| CN107910536A (en) * | 2017-12-27 | 2018-04-13 | 东北师范大学 | A kind of selenium/graphene nanocomposite material prepares and its application |
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| CN114864903A (en) * | 2022-05-27 | 2022-08-05 | 山东海科创新研究院有限公司 | Graphene-based selenium positive electrode material embedded with two-dimensional metal selenide, preparation method of graphene-based selenium positive electrode material and lithium selenium battery |
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| CN110492068A (en) * | 2019-08-05 | 2019-11-22 | 中南大学 | Redox graphene-selenium nanowires hydrogel composite material and the preparation method and application thereof |
| DE102021102874A1 (en) | 2020-02-07 | 2021-08-12 | Consejo Superior De Investigaciones Cientificas (Csic) | IMMOBILIZED SELENIUM IN A POROUS CARBON IN THE PRESENCE OF OXYGEN, AND A METHOD OF MANUFACTURING AND USING IMMOBILIZED SELENIUM IN A RECHARGEABLE BATTERY |
| CN114864903A (en) * | 2022-05-27 | 2022-08-05 | 山东海科创新研究院有限公司 | Graphene-based selenium positive electrode material embedded with two-dimensional metal selenide, preparation method of graphene-based selenium positive electrode material and lithium selenium battery |
| CN114864903B (en) * | 2022-05-27 | 2024-04-19 | 山东海科创新研究院有限公司 | Graphene-based selenium positive electrode material embedded with two-dimensional metal selenide, preparation method of graphene-based selenium positive electrode material and lithium-selenium battery |
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