CN104393304B - Lithium selenium cell positive electrode and preparation method thereof and lithium selenium cell - Google Patents
Lithium selenium cell positive electrode and preparation method thereof and lithium selenium cell Download PDFInfo
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- CN104393304B CN104393304B CN201410638938.6A CN201410638938A CN104393304B CN 104393304 B CN104393304 B CN 104393304B CN 201410638938 A CN201410638938 A CN 201410638938A CN 104393304 B CN104393304 B CN 104393304B
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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
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Abstract
The present invention provides a kind of preparation method of lithium selenium cell positive electrode, and it comprises the following steps：The graphene oxide dispersion of one inert atmosphere saturation is provided；Hydrogen selenide gas is passed through into the graphene oxide dispersion of the inert atmosphere saturation, using inert atmosphere as carrier gas, elemental selenium is generated in graphenic surface while the graphene oxide is reduced into graphene, obtains elemental selenium graphene dispersing solution；The graphene dispersing solution of the load selenium is subjected to solvent heat treatment, a graphene-based gel is obtained；And processing is dried in the graphene-based gel.The present invention also provides the lithium selenium cell of a kind of lithium selenium cell positive electrode and the application positive electrode.
Description
Technical field
The present invention relates to a kind of lithium selenium cell positive electrode and its preparation method, and lithium selenium cell.
Background technology
Lithium selenium cell is a kind of new lithium secondary battery system, and it is by the use of elemental selenium as positive pole, and lithium metal is negative pole, is led to
The chemical reaction crossed between selenium and lithium is realized and mutually changed between chemical energy and electric energy, with than existing anode material for lithium-ion batteries
Higher energy density.Chinese patent application CN103187559 A and CN103178246 A individually disclose by elemental selenium with it is micro-
Hole carrier or mesoporous supports Hybrid Heating, so that elemental selenium is dispersed in the duct of porous carrier or mesoporous supports, can be obtained
To the lithium secondary cell with high capacity with good circulation stability and high rate performance.
However, the duct of poromerics or mesoporous material is minimum, the above method is difficult to make elemental selenium fully and equably entered
Entering micropore canals, and be introduced into the elemental selenium in duct makes blockage of the micro orifice, it is difficult to make more elemental seleniums well into poromerics
Or inside mesoporous material, cause elemental selenium can not to be uniformly combined with carrier, so that the above method is dfficult to apply to actual industrial
In metaplasia production.
The content of the invention
In view of this, it is necessory to provide a kind of lithium selenium cell positive electrode and preparation method thereof, and lithium selenium cell.
A kind of preparation method of lithium selenium cell positive electrode, it comprises the following steps：The oxygen of one inert atmosphere saturation is provided
Graphite alkene dispersion liquid；Hydrogen selenide gas is passed through into the graphene oxide dispersion of the inert atmosphere saturation, with inert atmosphere
For carrier gas, elemental selenium is generated in graphenic surface while the graphene oxide is reduced into graphene, elemental selenium-stone is obtained
Black alkene dispersion liquid；The graphene dispersing solution of the load selenium is subjected to solvent thermal reaction, a graphene-based gel is obtained；And will
Processing is dried in the graphene-based gel, to obtain a lithium selenium cell positive electrode.
A kind of lithium selenium cell positive electrode, including three-dimensional porous graphene macroform and multiple to be distributed in this three-dimensional porous
Elemental selenium in graphene macroform, wherein, the three-dimensional porous graphene macroform is mutually to be overlapped by multiple graphene films
There are multiple holes, it is many that the multiple elemental selenium is uniformly distributed in this between the self supporting structure of formation, the plurality of graphene film
Individual hole and multiple graphene film layer surfaces.
A kind of lithium selenium cell, including positive pole, negative pole, barrier film and electrolyte, the positive pole include a collector and setting
In the above-mentioned positive electrode on the collector.
Compared with prior art, the present invention first with redox reaction by elemental selenium in-situ preparation in scattered graphite
Alkene surface, then the scattered graphene of script is mutually overlapped, porous macroscopic material is assembled into, so that elemental selenium is uniformly set
Put in the duct of the porous macroscopic material and multiple graphene film layer surfaces, form graphene and mixed with elemental selenium substantially uniformity
The composite construction of conjunction, is conducive to further improving the chemical property of lithium selenium cell.Also, the complex method is simple, suitable for work
The application of industry metaplasia production.
Brief description of the drawings
Fig. 1 is the flow chart of the preparation method of lithium selenium cell positive electrode provided in an embodiment of the present invention.
Fig. 2 is the stereoscan photograph figure of lithium selenium cell positive electrode provided in an embodiment of the present invention.
Fig. 3 is the structural representation of lithium selenium cell provided in an embodiment of the present invention.
Fig. 4 is the first charge-discharge curve map of lithium selenium cell provided in an 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 with reference to above-mentioned accompanying drawing.
Embodiment
The preparation method of the lithium selenium cell positive electrode provided below in conjunction with the accompanying drawings and the specific embodiments the present invention, its
Preparation method and lithium selenium cell are described in further detail.
Referring to Fig. 1, the embodiment of the present invention provides a kind of preparation method of lithium selenium cell positive electrode, this method include with
Lower step：
S1：The graphene oxide dispersion of one inert atmosphere saturation is provided；
S2：Hydrogen selenide gas is passed through into the graphene oxide dispersion of the inert atmosphere saturation, inert atmosphere is carrier gas,
Elemental selenium is generated in graphenic surface while the graphene oxide is reduced into graphene, elemental selenium-graphene point is obtained
Dispersion liquid；
S3：The elemental selenium-graphene dispersing solution is subjected to solvent thermal reaction, graphene is assembled into porous macroscopic material
Material；And
S4：Processing is dried in the porous macroscopic material, lithium selenium cell positive electrode is obtained.
In step S1, the solvent in the graphene oxide dispersion can be water, or organic solvent, such as second
Alcohol, isopropanol, ethylene glycol, N,N-dimethylformamide（DMF）, 1-METHYLPYRROLIDONE（NMP）, one kind in tetrahydrofuran or
Person is several.Certainly, the selection of the solvent be not limited to it is above-mentioned enumerate it is several, as long as the graphene oxide can be disperseed well
.The concentration of graphene oxide can be 0.05 ~ 30 mg/mL in the graphene oxide dispersion, it is preferable that its concentration
For 1 ~ 5 mg/mL.
The preparation method of the graphene oxide dispersion is：Graphite oxide powder is added into the solvent；And
The lamella for making graphite oxide using modes such as ultrasonic disperse, stirrings is mutually peeled off, and is uniformly dispersed, and obtains the graphene oxide point
Dispersion liquid.In the present embodiment, 300 milligrams of graphite oxide powders are added into 100 ml deionized waters, in the super of 200 watts of power
After sound is stirred 2.0 hours, the graphene oxide dispersion that a concentration is 3 mg/mL is obtained.
Inert gas further is being passed through into the graphene oxide dispersion after obtaining the graphene oxide dispersion, is being made
Inert gas saturation in the graphene oxide dispersion.The inert gas can be nitrogen and rare gas, such as argon gas, in
It is one or more.
In step S2, graphene oxide is reduced to graphene by the hydrogen selenide, while obtaining elemental selenium and water, reaction equation is such as
Formula（1）It is shown.
Graphene oxide+H2Se → graphene+H2O+Se↓ （1）
The hydrogen selenide gas when being passed through using inert gas is used as carrier gas.The intake of the hydrogen selenide gas can basis
The component for the lithium selenium cell positive electrode that concentration, quality and the expection of graphene oxide dispersion are obtained is adjusted.The selenium
Change hydrogen to be reacted in surface of graphene oxide, the elemental selenium of generation is uniformly adhered to graphenic surface, can be with graphene
Adsorbed, or connected by chemical bond by Van der Waals force.The in-situ preparation graphenic surface elemental selenium to be unformed or
Graininess, size is less than 1 micron, preferably less than 100 nanometers.
The reaction temperature of redox reaction in step S2 should be less than the boiling point of the solvent, and should be less than hydrogen selenide
Burning-point, is lost in this step with preventing or reducing the solvent and hydrogen selenide.Specifically, the reaction temperature is at 5 ~ 300 DEG C
Between.When the solvent is water, the reaction temperature is between 5 ~ 100 DEG C.In the present embodiment, the reaction temperature is 75 DEG C.
The redox reaction is carried out in inert gas shielding.
Progress sonic oscillation is can continue to while hydrogen selenide gas is passed through makes reaction more abundant, and obtains
Even scattered elemental selenium-graphene dispersing solution.
In step S3, the temperature of the solvent thermal reaction is 50 ~ 217 DEG C（217 DEG C of fusing points for selenium）, the time be 0.1 ~
120 hours.Preferably, the temperature of the solvent thermal reaction is 70 ~ 180 DEG C, and the time is 2 ~ 48 hours., can be by during concrete operations
Elemental selenium-the graphene dispersing solution is placed in a closed high-pressure closed vessel, and heated in a Muffle furnace, reaction
The pressure of process is more than or equal to 1 atmospheric pressure.On the one hand the solvent thermal reaction can make the graphene of the load elemental selenium
Mutually overlap joint is assembled into porous macroscopic self supporting structure, on the other hand can promote being uniformly distributed for selenium., will in the present embodiment
Elemental selenium-the graphene dispersing solution heats 6 hours at 150 DEG C, to obtain the porous macroscopic material.It is many that this is obtained
Hole macroscopic body material is macroscopical block structure of a self-supporting, can be taken out directly from reaction vessel.
In step S4, the purpose of the drying is to remove solvent remaining in the porous macroscopic material.But in order to anti-
The only distillation of selenium, the drying should be carried out at a lower temperature.Specifically, the drying means of the graphene dispersing solution can be with
For the heating under freeze-drying, drying at room temperature, supercritical drying, vacuum and heating drying, normal heating drying or protective gas
Dry.In the present embodiment, the solvent in the porous macroscopic material is removed using the method for vacuum and heating drying, to obtain
State positive electrode.Specifically, gained porous macroscopic material is placed in a vacuum drying oven and be dried.The heating in vacuum is done
It is dry to remove the solvent of porous macroscopic material internal rapidly, while keeping its microcosmic loose structure.Preferably, the vacuum
The temperature of heat drying is between 0 DEG C ~ 217 DEG C.Preferably, the temperature of the vacuum and heating drying is between 20 DEG C ~ 100 DEG C.
Specifically, in the present embodiment, the temperature of the vacuum and heating drying is 60 DEG C.In addition, when using freeze-drying when, temperature for-
Between 196 DEG C ~ 0 DEG C.
Referring to Fig. 2, the lithium selenium cell positive electrode prepared using the method for the present embodiment, including it is used as elemental selenium
The porous macroscopic material of carrier and multiple it is arranged in the porous macroscopic material hole and multiple graphene film layer surfaces
Elemental selenium.The porous macroscopic material is mutually overlapped by multiple graphene films to be formed, and these graphene films are in the macroscopic body
In it is network-like be uniformly distributed, multiple holes are formed between these graphene films, and the plurality of elemental selenium is then equal with amorphous state
The surface of these graphene films is distributed in evenly, and is combined closely with the graphene.The hole of the porous macroscopic material
Rate is in 0.05 ~ 4 cm3Between/g, the pore-size distribution of the hole is between 0.4 nm ~ 10 μm.Preferably, it is described three-dimensional porous
The porosity of graphene macroform is in 0.1 ~ 3 cm3Between/g, the pore-size distribution of the hole is between 1 nm ~ 5 μm, preferably
Ground, pore-size distribution is between the nm of 1 nm ~ 500.
In the lithium selenium cell positive electrode, except being attracted each other by Van der Waals force between elemental selenium and graphene film
Outside, also there is certain chemical bonding effect.Therefore, the lithium selenium cell positive electrode has relatively stable structure, it is ensured that lithium selenium
The stability of battery charging and discharging performance.
In the lithium selenium cell positive electrode, the weight/mass percentage composition of the elemental selenium can be 5% ~ 95%.The lithium selenium
Cell positive material only can be made up of elemental selenium with graphene.The quality percentage of each composition contains in the lithium selenium cell positive electrode
Amount can be controlled by adjusting the intake of hydrogen selenide.In the present embodiment, the weight/mass percentage composition of the elemental selenium is 60%, institute
The weight/mass percentage composition for stating graphene macroform is 40%.
In the lithium selenium cell positive electrode, the porous macroscopic material primarily serves the carrier and conductive work of elemental selenium
With.On the one hand, the porous macroscopic material can adsorb elemental selenium, enable selenium be dispersed stably in well graphene film it
Between hole in and graphene film surface；On the other hand, excellent electric conductivity can provide good to graphene for the positive electrode in itself
Good conductive network.Meanwhile, the porous buffer structure that the lithium selenium cell positive electrode has is to many selenides of discharge and recharge product
With good confinement effect.
Referring to Fig. 3, the embodiment of the present invention also provides a kind of lithium selenium cell 10 of the above-mentioned positive electrode of application, it is included just
Pole piece 12, negative plate 14, barrier film 16 and electrolyte 18.The positive plate 12 includes a collector 122 and is arranged at the afflux
Above-mentioned lithium selenium cell positive electrode 124 on body 122, including porous macroscopic material and multiple it is arranged on the porous macroscopic
Elemental selenium in the hole of material.
The collector can be aluminium foil, nickel foam, stainless (steel) wire or carbon-coated aluminum foils etc..The negative plate is lithium metal
Piece, lithium alloys piece, lithium/carbon composite material piece etc..The electrolyte is two（Trimethyl fluoride sulfonyl）Imine lithium（LiTFSI）, six
Lithium fluophosphate（LiPF6）Deng；Solvent used in the electrolyte is ethers, such as glycol dimethyl ether（TEGDME）, dimethyl ether
（DME）Deng；The barrier film is polypropylene（PP）Microporous barrier, polyethylene（PE）Co-polymer membrane of microporous barrier or propylene and ethene etc..
In the present embodiment, using aluminium foil as collector, using metal lithium sheet as negative plate, using microporous polypropylene membrane as barrier film, with
1.5 mol/L bis-（Trimethyl fluoride sulfonyl）Imine lithium（LiTFSI）/ 1,3- dioxolanes（DOL）+ dimethyl ether（DME）（Volume ratio
1:1）A lithium selenium cell is assembled into for electrolyte.The first charge-discharge curve of the lithium selenium cell is referring to Fig. 4, as seen from Figure 4, be somebody's turn to do
The discharge capacity first of lithium selenium cell is up to 640 mAh/g.
Compared with prior art, the present invention divides first by elemental selenium in-situ preparation in scattered graphenic surface, then by script
Scattered graphene is mutually overlapped, and is assembled into porous macroscopic material, so that elemental selenium is uniformly arranged on the porous macroscopic
In the hole of material, the composite construction that graphene is mixed with elemental selenium substantially uniformity is formed, is conducive to further improving lithium selenium electricity
The chemical property in pond.Also, the complex method is simple, the application suitable for industrialized production.
In addition, those skilled in the art can also do other changes in spirit of the invention, certainly, these are according to present invention essence
The change that god is done, should all be included within scope of the present invention.
Claims (11)
1. a kind of preparation method of lithium selenium cell positive electrode, it comprises the following steps：
The graphene oxide dispersion of one inert atmosphere saturation is provided；
Hydrogen selenide gas is passed through into the graphene oxide dispersion of the inert atmosphere saturation, using inert atmosphere as carrier gas, by institute
The elemental selenium that graphene oxide is reduced to generate amorphous state in graphenic surface while graphene is stated, elemental selenium-stone is obtained
Black alkene dispersion liquid；
The elemental selenium-graphene dispersing solution is subjected to solvent thermal reaction, graphene is assembled into porous macroscopic material；And
Processing is dried in the porous macroscopic material, lithium selenium cell positive electrode is obtained.
2. the preparation method of lithium selenium cell positive electrode as claimed in claim 1, it is characterised in that the solvent thermal reaction
Temperature 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 characterised in that the graphene oxide point
The concentration of graphene oxide is 0.05mg/mL~30mg/mL in dispersion liquid.
4. the preparation method of lithium selenium cell positive electrode as claimed in claim 1, it is characterised in that the mode of the drying is
Heat drying under freeze-drying, drying at room temperature, supercritical drying, vacuum and heating drying, normal heating drying and protective gas
In one kind.
5. the preparation method of lithium selenium cell positive electrode as claimed in claim 1, it is characterised in that be passed through hydrogen selenide gas
During control redox graphene reaction temperature be 5 DEG C~300 DEG C.
6. lithium selenium cell positive electrode prepared by the preparation method in a kind of 1-5 such as claim as described in any one, including one
Porous macroscopic material and multiple elemental seleniums, the porous macroscopic material is mutually overlapped by multiple graphene films to be formed, and this is more
There are multiple holes, the plurality of elemental selenium is evenly distributed in the porous macroscopic material hole and this is more between individual graphene film
Individual graphene film surface.
7. lithium selenium cell positive electrode as claimed in claim 6, it is characterised in that the porous macroscopic material is propped up certainly for one
Support structure.
8. lithium selenium cell positive electrode as claimed in claim 6, it is characterised in that the weight/mass percentage composition of the elemental selenium exists
Between 5%~95%.
9. lithium selenium cell positive electrode as claimed in claim 6, it is characterised in that the multiple elemental selenium is equal with amorphous state
The even surface for being distributed in the plurality of graphene film.
10. lithium selenium cell positive electrode as claimed in claim 7, it is characterised in that the hole of the porous macroscopic material
Rate is 0.05cm3/ g~4cm3/ g, the pore-size distribution of the multiple hole is between 0.4nm~10 μm.
11. a kind of lithium selenium cell, including positive plate, negative plate, barrier film and electrolyte, it is characterised in that the positive plate bag
Include collector and the lithium selenium cell positive electrode as any one of claim 6~10, the lithium selenium cell positive pole material
Material is arranged at the surface of the collector.
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| US11784303B2 (en) | 2015-09-22 | 2023-10-10 | Ii-Vi Delaware, Inc. | Immobilized chalcogen and use thereof in a rechargeable battery |
| US11588149B2 (en) | 2015-09-22 | 2023-02-21 | Ii-Vi Delaware, Inc. | Immobilized selenium in a porous carbon with the presence of oxygen, a method of making, and uses of immobilized selenium in a rechargeable battery |
| US10734638B2 (en) | 2015-09-22 | 2020-08-04 | Ii-Vi Delaware, Inc. | Immobilized selenium, a method of making, and uses of immobilized selenium in a rechargeable battery |
| CN105070892B (en) | 2015-09-22 | 2018-03-06 | 中国科学院化学研究所 | A kind of preparation method and application of selenium carbon complex |
| CN106571460B (en) * | 2015-10-09 | 2019-02-26 | 中国科学院上海硅酸盐研究所 | A kind of binder free, selenium positive electrode of self supporting structure and preparation method thereof |
| CN106784660B (en) * | 2016-12-02 | 2019-04-05 | 吉林大学 | Se-TiO of the nickel foam as interlayer2/ NFF lithium selenium secondary cell and preparation method thereof |
| US11870059B2 (en) | 2017-02-16 | 2024-01-09 | Consejo Superior De Investigaciones Cientificas (Csic) | Immobilized selenium in a porous carbon with the presence of oxygen, a method of making, and uses of immobilized selenium in a rechargeable battery |
| CN107706404B (en) * | 2017-11-23 | 2020-04-21 | 东北师范大学 | Preparation and application of selenium-coated tin dioxide/graphene nanocomposite |
| 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 |
| JP7253559B2 (en) * | 2019-02-08 | 2023-04-06 | トゥー－シックス デラウェア，インコーポレイテッド | Method for preparing immobilized selenium |
| 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 |
| CA3107294A1 (en) | 2020-02-07 | 2021-08-07 | Ii-Vi Delaware, Inc. | Immobilized selenium in a porous carbon with the presence of oxygen, a method of making, and uses of immobilized selenium in a rechargeable 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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| US9005808B2 (en) * | 2011-03-01 | 2015-04-14 | Uchicago Argonne, Llc | Electrode materials for rechargeable batteries |
| CN103178246B (en) * | 2013-03-04 | 2015-05-06 | 中国科学院化学研究所 | Selenium-mesoporous carrier compound, as well as preparation method and application thereof |
| CN103390752B (en) * | 2013-07-05 | 2016-06-01 | 清华大学深圳研究生院 | Graphene-based matrix material, its preparation method and the application in lithium-sulfur cell thereof |
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