CN108039469A - The preparation method of fluorographite-sulfur electrode - Google Patents

The preparation method of fluorographite-sulfur electrode Download PDF

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Publication number
CN108039469A
CN108039469A CN201711272570.6A CN201711272570A CN108039469A CN 108039469 A CN108039469 A CN 108039469A CN 201711272570 A CN201711272570 A CN 201711272570A CN 108039469 A CN108039469 A CN 108039469A
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China
Prior art keywords
fluorographite
preparation
sulfur
conductive agent
sulfur electrode
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CN201711272570.6A
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Chinese (zh)
Inventor
王振
张红梅
魏俊华
王庆杰
张云朋
万伟华
石斌
陈铤
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Guizhou Meiling Power Supply Co Ltd
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Guizhou Meiling Power Supply Co Ltd
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Priority to CN201711272570.6A priority Critical patent/CN108039469A/en
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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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • H01M4/5835—Comprising fluorine or fluoride salts
    • 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
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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 discloses the preparation method of fluorographite sulfur electrode, fluorographite and elemental sulfur, ball milling mixing is uniform, sieving, is placed in hermetically sealed can and is sealed and be passed through inert gas, and hermetically sealed can is placed in Muffle furnace and is heated to keeping 5h ~ 6h at 155 DEG C, continue to be heated to afterwards to keep 2h ~ 3h at 320 DEG C, natural cooling, is ground up, sieved, and fluorographite sulphur composite material is prepared；Then fluorographite sulphur composite material is added in the mixed solution of pure water and dispersant sodium carboxymethylcellulose, and is stirred；Conductive agent carbon nanotubes is added, and is stirred；Conductive agent superconduction carbon black is added, and is stirred；Binding agent butadiene-styrene latex is added, and is stirred；Slurry is made and is coated in aluminum foil current collector, is placed in 60 DEG C ~ 70 DEG C of baking oven and dries, that is, obtains fluorographite sulphur cathode.

Description

The preparation method of fluorographite-sulfur electrode
Technical field
A kind of preparation method the present invention relates to lithium battery with fluorographite-sulfur electrode, belongs to lithium battery preparation field.
Background technology
The lithium metal battery battery system high as theoretical energy density, receives more and more research concern.Lithium fluorine Graphite battery theoretical energy density reaches 2180Wh/kg, is the commercialized a kind of electricity that takes the lead in solid electrode lithium battery system Pond, is widely used to the instrument and equipments such as emergency lamp signal telegraph, communication power supply, pacemaker；Lithium-sulfur cell is considered as most Potential to realize commercialized novel secondary lithium battery system, its theoretical energy density reaches 2600Wh/kg, at present still in reality Test room conceptual phase.Two kinds of battery systems are each advantageous, can prepare fluorographite-sulphur by the mutual supplement with each other's advantages of positive electrode Electrode, so as to prepare lithium battery.
Lithium fluorographite battery operating voltage is high, energy density is big, storage life length, but fluorographite is expensive, and With relatively low electronic conductivity, battery polarization can be caused to increase initial stage in battery discharge, internal resistance increase, causes voltage delay to show As operating voltage range narrows.Lithium-sulfur cell energy density is big, rich reserves of good rate capability, sulphur and cheap, but lithium Sulphur battery in charge and discharge process " shuttle effect " presence so that the capacity attenuation of battery is fast, and cyclical stability is poor.
For lithium fluorographite battery and lithium-sulfur cell there are the problem of, with reference to the characteristics of two kinds of battery electrode materials, system The composite material of standby fluorographite-sulphur simultaneously prepares its electrode, to achieve the purpose that mutual supplement with each other's advantages.
The content of the invention
It is an object of the invention to provide the preparation method of fluorographite-sulfur electrode, and fluorine is prepared by substep heat treating process Graphite-sulphur composite material, then prepares fluorographite-sulfur electrode, to have complementary advantages, improves the voltage delay problem of battery, The voltage range of battery is widened, reduces battery cost.
The technical solution used in the present invention for：The preparation method of fluorographite-sulfur electrode, its preparation process include as follows Step：Comprise the following steps：（1）Fluorographite and elemental sulfur are weighed, uniform by ball milling mixing, sieving, obtains fluorographite With the mixed-powder material of elemental sulfur；（2）By step 1）The mixed-powder material of preparation loads hermetically sealed can and vacuumizing is passed through Inert gas, hermetically sealed can is placed in Muffle furnace and is heated to keeping 5h ~ 6h at 150 DEG C ~ 160 DEG C, then heats to 320 DEG C ~ 330 2h ~ 3h is kept at DEG C, is ground up, sieved after natural cooling, that is, fluorographite-sulphur composite material is prepared；（3）By step 2）System Standby composite material is added in the mixed liquor of pure water and dispersant, and is stirred；（4）In step 3）Added in obtained slurry conductive Agent I, and stir；（5）In step 4）Conductive agent II is added in obtained slurry, and is stirred；（6）In step 5）In obtained slurry Binding agent is added, and is stirred；（7）By step 6）Obtained slurry is coated uniformly in aluminum foil current collector, is placed in 60 DEG C ~ 70 DEG C Dried in baking oven.
Above-described composite material, dispersant, conductive agent I, the mass ratio of conductive agent II and binding agent are 80：2.5： 5.5：7：5.
The fluorographite（CFx）Fluorine carbon ratio between 0.9 ~ 1.0.
The hermetically sealed can is ceramic pot or the stainless cylinder of steel for having the function of to vacuumize, and tank body volume is in 100ml ~ 300ml Between.
Fluorographite-the sulphur（CFx/S）By percentage to the quality, sulfur content is in 60wt.% for sulfur content in composite material Between ~ 80wt.%.
The dispersant is sodium carboxymethylcellulose（CMC）.
The conductive agent I is carbon nanotubes（CNTs）.
The conductive agent II is superconduction carbon black（SuperP Li）.
The binding agent is butadiene-styrene latex（SBR）.
Beneficial effects of the present invention：
Present invention determine that technology prepared by a kind of fluorographite-sulfur electrode, each for fluorographite electrode and sulfur electrode From advantage and disadvantage, have complementary advantages, the cell voltage of preparation hysteresis makes moderate progress, and battery operating voltage scope is widened, cost Reduce.The present invention is simple to equipment requirement, and material preparation method is workable, and production process is pollution-free.
In order to detect the chemical property of fluorographite-sulfur electrode of the method for the present invention preparation, the present invention is assembled with Soft Roll Packed battery, its composition include cathode, anode, membrane and electrolyte, it is characterised in that：
1）Just extremely fluorographite-sulfur electrode；
2）Anode is lithium metal or lithium alloys such as Li, Li-Al, Li-Si etc.；
3）Electrolyte system can be organic liquid electrolyte, ionic liquid, gel polymer electrolyte, solid electrolyte etc..
Brief description of the drawings
Fig. 1 is that electric discharge of the flexible-packed battery of fluorographite-sulfur electrode assembling prepared by embodiment under 0.05C multiplying powers is bent Line；
Fig. 2 is discharge curve of the flexible-packed battery of fluorographite-sulfur electrode assembling prepared by embodiment under 0.1C multiplying powers.
Embodiment
Embodiment 1：
In mass ratio 70：30 weigh elemental sulfur respectively（S）And fluorographite（CFx）, it is uniform to be placed in ball milling mixing in ball mill, mistake Sieve, is placed in hermetically sealed can by mixing material and seal and vacuumizing, be passed through into hermetically sealed can nitrogen as inert gas 15 ~ 20min.Hermetically sealed can is placed in Muffle furnace be heated at 155 DEG C keep 5h ~ 6h, continue to be heated to afterwards at 325 DEG C keep 2h ~ 3h, then closes Muffle furnace heater switch, and natural cooling, is ground up, sieved, that is, the fluorination that sulfur content is 70 wt.% is prepared Graphite-sulphur（CFx/S）Composite material.
In pure water and dispersant sodium carboxymethylcellulose（CMC）Mixed solution in add fluorographite-sulphur（CFx/S）It is multiple Condensation material, stirs 1h；Add conductive agent carbon nanotubes（CNTs）, stir 1h；Add conductive agent superconduction carbon black（SuperP Li）, Stir 1h；Add binding agent butadiene-styrene latex（SBR）, stir 2h；Slurry is made and is coated in aluminum foil current collector, obtains fluorination stone Ink-sulphur cathode.Then using lithium band as anode, Celgard2325 films are membrane, are encapsulated with plastic-aluminum packaging film, inject 1.0M LiTFSI+0.2M LiNO3/DOL+ DME（V/v, 1：1）Organic electrolyte, battery is formed after sealing.
The battery of assembling is respectively with 0.05C and 0.1C multiplying power dischargings, discharge cut-off voltage 1.0V, and discharge curve is respectively such as Shown in Fig. 1, Fig. 2.Battery discharges under 0.05C multiplying powers, the minimum 2.25V of voltage delay when discharging initial, and subsequent voltage returns 2.46V or so is risen to, with the progress of electric discharge, voltage is slowly drop down to 2.02V or so and forms stable discharge platform, electric discharge Time is about 13.3h, and the discharge capacity for calculating battery is about 1.26Ah, and the ratio energy of battery is about 271.5Wh/kg.Battery exists Discharge under 0.1C multiplying powers, the minimum 2.24V of voltage delay when discharging initial, subsequent voltage recovery to 2.44V or so, with putting The progress of electricity, voltage are slowly drop down to 2.08V or so and form stable discharge platform, and discharge time is about 6.4h, calculate electricity The discharge capacity in pond is about 1.22Ah, and the ratio energy of battery is about 269.6Wh/kg.
Embodiment 2：
In mass ratio 60：40 weigh elemental sulfur respectively（S）And fluorographite（CFx）, it is uniform to be placed in ball milling mixing in ball mill, mistake Sieve, is placed in hermetically sealed can by mixing material and seal and vacuumizing, be passed through into hermetically sealed can nitrogen as inert gas 15 ~ 20min.Hermetically sealed can is placed in Muffle furnace be heated at 155 DEG C keep 5h ~ 6h, continue to be heated to afterwards at 325 DEG C keep 2h ~ 3h, then closes Muffle furnace heater switch, and natural cooling, is ground up, sieved, that is, the fluorination that sulfur content is 60 wt.% is prepared Graphite-sulphur（CFx/S）Composite material.
In pure water and dispersant sodium carboxymethylcellulose（CMC）Mixed solution in add fluorographite-sulphur（CFx/S）It is multiple Condensation material, stirs 1h；Add conductive agent carbon nanotubes（CNTs）, stir 1h；Add conductive agent superconduction carbon black（SuperP Li）, Stir 1h；Add binding agent butadiene-styrene latex（SBR）, stir 2h；Slurry is made and is coated in aluminum foil current collector, obtains fluorination stone Ink-sulphur cathode.Then using lithium band as anode, Celgard2325 films are membrane, are encapsulated with plastic-aluminum packaging film, inject 1.0M LiTFSI+0.2M LiNO3/DOL+ DME（V/v, 1：1）Organic electrolyte, battery is formed after sealing.
Embodiment 3：
In mass ratio 80：20 weigh elemental sulfur respectively（S）And fluorographite（CFx）, it is uniform to be placed in ball milling mixing in ball mill, mistake Sieve, is placed in hermetically sealed can by mixing material and seal and vacuumizing, be passed through into hermetically sealed can nitrogen as inert gas 15 ~ 20min.Hermetically sealed can is placed in Muffle furnace be heated at 155 DEG C keep 5h ~ 6h, continue to be heated to afterwards at 325 DEG C keep 2h ~ 3h, then closes Muffle furnace heater switch, and natural cooling, is ground up, sieved, that is, the fluorination that sulfur content is 80 wt.% is prepared Graphite-sulphur（CFx/S）Composite material.
In pure water and dispersant sodium carboxymethylcellulose（CMC）Mixed solution in add fluorographite-sulphur（CFx/S）It is multiple Condensation material, stirs 1h；Add conductive agent carbon nanotubes（CNTs）, stir 1h；Add conductive agent superconduction carbon black（SuperP Li）, Stir 1h；Add binding agent butadiene-styrene latex（SBR）, stir 2h；Slurry is made and is coated in aluminum foil current collector, obtains fluorination stone Ink-sulphur cathode.Then using lithium band as anode, Celgard2325 films are membrane, are encapsulated with plastic-aluminum packaging film, inject 1.0M LiTFSI+0.2M LiNO3/DOL+ DME（V/v, 1：1）Organic electrolyte, battery is formed after sealing.

Claims (9)

1. the preparation method of fluorographite-sulfur electrode, it is characterised in that：Comprise the following steps：（1）Weigh fluorographite and simple substance Sulphur, uniform by ball milling mixing, sieving, obtains the mixed-powder material of fluorographite and elemental sulfur；（2）By step 1）Prepare Mixed-powder material loads hermetically sealed can and vacuumizing and is passed through inert gas, hermetically sealed can is placed in Muffle furnace be heated to 150 DEG C ~ 5h ~ 6h is kept at 160 DEG C, holding 2h ~ 3h at 320 DEG C ~ 330 DEG C is then heated to, is ground up, sieved, that is, prepares after natural cooling Obtain fluorographite-sulphur composite material；（3）By step 2）The composite material of preparation is added in the mixed liquor of pure water and dispersant, And stir；（4）In step 3）Conductive agent I is added in obtained slurry, and is stirred；（5）In step 4）Added in obtained slurry Conductive agent II, and stir；（6）In step 5）Binding agent is added in obtained slurry, and is stirred；（7）By step 6）Obtained slurry Material is coated uniformly in aluminum foil current collector, is placed in 60 DEG C ~ 70 DEG C of baking oven and is dried.
2. the preparation method of fluorographite-sulfur electrode according to claim 1, it is characterised in that：The composite material, Dispersant, conductive agent I, the mass ratio of conductive agent II and binding agent are 80：2.5：5.5：7：5.
3. the preparation method of fluorographite-sulfur electrode according to claim 1, it is characterised in that：The fluorographite Fluorine carbon ratio is between 0.9 ~ 1.0.
4. the preparation method of fluorographite-sulfur electrode according to claim 1, it is characterised in that：The hermetically sealed can is tool There are the ceramic pot or stainless cylinder of steel for vacuumizing function, tank body volume is between 100ml ~ 300ml.
5. the preparation method of fluorographite-sulfur electrode according to claim 1, it is characterised in that：The fluorographite- By percentage to the quality, sulfur content is between 60wt.% ~ 80wt.% for sulfur content in sulphur composite material.
6. the preparation method of fluorographite-sulfur electrode according to claim 1, it is characterised in that：The dispersant is Sodium carboxymethylcellulose.
7. the preparation method of fluorographite-sulfur electrode according to claim 1, it is characterised in that：The conductive agent I is Carbon nanotubes.
8. the preparation method of fluorographite-sulfur electrode according to claim 1, it is characterised in that：The conductive agent II For superconduction carbon black.
9. the preparation method of fluorographite-sulfur electrode according to claim 1, it is characterised in that：The binding agent is Butadiene-styrene latex.
CN201711272570.6A 2017-12-06 2017-12-06 The preparation method of fluorographite-sulfur electrode Pending CN108039469A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109742354A (en) * 2018-12-29 2019-05-10 贵州梅岭电源有限公司 A kind of fluorination carbon composite electrode and preparation method thereof
CN111362257A (en) * 2018-12-26 2020-07-03 中国科学院福建物质结构研究所 Fluorinated graphene/sulfur composite material, preparation method thereof and application of fluorinated graphene/sulfur composite material in lithium battery

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104716296A (en) * 2013-12-11 2015-06-17 上海空间电源研究所 Sulfur-containing composite anode, preparation method thereof and lithium-sulfur battery using sulfur-containing composite anode as anode
CN106159267A (en) * 2016-09-12 2016-11-23 贵州梅岭电源有限公司 A kind of preparation method of sulfur carbon composite
CN106169561A (en) * 2016-09-30 2016-11-30 上海空间电源研究所 A kind of sulfur system anode composite pole piece, the battery comprising it and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104716296A (en) * 2013-12-11 2015-06-17 上海空间电源研究所 Sulfur-containing composite anode, preparation method thereof and lithium-sulfur battery using sulfur-containing composite anode as anode
CN106159267A (en) * 2016-09-12 2016-11-23 贵州梅岭电源有限公司 A kind of preparation method of sulfur carbon composite
CN106169561A (en) * 2016-09-30 2016-11-30 上海空间电源研究所 A kind of sulfur system anode composite pole piece, the battery comprising it and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111362257A (en) * 2018-12-26 2020-07-03 中国科学院福建物质结构研究所 Fluorinated graphene/sulfur composite material, preparation method thereof and application of fluorinated graphene/sulfur composite material in lithium battery
CN111362257B (en) * 2018-12-26 2022-02-18 中国科学院福建物质结构研究所 Fluorinated graphene/sulfur composite material, preparation method thereof and application of fluorinated graphene/sulfur composite material in lithium battery
CN109742354A (en) * 2018-12-29 2019-05-10 贵州梅岭电源有限公司 A kind of fluorination carbon composite electrode and preparation method thereof

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Application publication date: 20180515