CN109360953A - A kind of method synthesizing vulcanization lithium/carbon composite material and the lithium-sulfur cell using the material - Google Patents

A kind of method synthesizing vulcanization lithium/carbon composite material and the lithium-sulfur cell using the material Download PDF

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Publication number
CN109360953A
CN109360953A CN201811138305.3A CN201811138305A CN109360953A CN 109360953 A CN109360953 A CN 109360953A CN 201811138305 A CN201811138305 A CN 201811138305A CN 109360953 A CN109360953 A CN 109360953A
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lithium
temperature
carbon source
carbon
warming
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师春生
王宁
赵乃勤
何春年
刘恩佐
何芳
马丽颖
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Tianjin University
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Tianjin University
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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
    • 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
    • H01M4/58—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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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 present invention relates to a kind of methods of heat treatment lithium sulfate and carbon source synthesis vulcanization lithium/carbon composite material, including following procedure: pressing carbon source: sulfuric acid monohydrate lithium molar ratio (0.5-2): 1 obtained aqueous solution, 60-100 DEG C of heating stirring, it is subsequently placed in 60-100 DEG C of heat drying of baking oven, grind into powder.Powder made from step (1) is placed on to the flat-temperature zone of tube furnace; 500-700 DEG C is warming up under argon atmosphere; keep the temperature 0.5-4h; then 700-1000 DEG C is warming up to 2-10 DEG C/min; keep the temperature 0.5-4h; it is cooled to 300-350 DEG C with the rate of 5-10 DEG C/min under the atmosphere of argon gas protection, room temperature is cooled to the furnace then to get to lithium sulfate and carbon source and synthesizes lithium sulfide/carbon complex.And it is related to using prepared vulcanization lithium/carbon composite material as positive electrode, lithium-sulfur cell of the graphite as negative electrode material.

Description

A kind of method synthesizing vulcanization lithium/carbon composite material and the lithium sulphur using the material Battery
Technical field
The present invention relates to it is a kind of by heat treatment lithium sulfate and carbon source synthesis vulcanization lithium/carbon composite material preparation method and Use the material as the graphite of positive electrode-lithium sulfide full battery, belongs to the technical field of lithium-sulfur cell.
Background technique
Solve the problems, such as fossil fuel consumption and therewith bring environmental pollution have become a globalization, therefore adjust Whole energy resource structure is extremely urgent using clean energy resourcies such as solar energy, wind energies.Matched energy storage technology is the one of key Ring, wherein electrochemical energy storage great potential.
Conventional lithium ion battery positive electrode theoretical specific capacity is both less than 300mAhg-1, actual energy density is less than 200 Wh·kg-1, cruising ability is not able to satisfy the needs in market.And elemental sulfur can match with lithium metal, theoretical specific capacity is up to 1675mAh·g-1, theoretical energy density is also up to 2600Whkg-1, and resourceful, environmental-friendly, cheap, tool There is very big prospect.Therefore, elemental sulfur is a kind of positive active material of serondary lithium battery to have a great attraction.
Existing research show sulphur positive electrode there is also storage the volume expansion of lithium process it is larger, cannot be free of lithium cathode (such as: Si, Sn) it matches, be not easy to carry out the unfavorable factors such as high-temperature process (fusing point is low).Using the lithiumation state material Li of sulphur2S is just Pole can preferably avoid the above-mentioned unfavorable factor of sulphur anode.In recent years, Li2The research of S positive electrode is increasingly closed Note and attention.Other than there are problems that storing up the dissolution of the more lithium sulfides of lithium intermediate state and poorly conductive as sulphur positive electrode, Li2Main problem existing for S positive electrode is to the moisture-sensitive in air and to be synthetically prepared route difficulty.Current is big Partially synthetic route can be divided into the direct application of commercialization lithium sulfide and chemical method synthesizes lithium sulfide, but there are at high cost, preparations Li in process complexity, compound2The disadvantages of S content is not high limits its practical application on lithium-sulfur cell.
It is current to be concentrated mainly on the high material of Si, Sn these specific capacities without lithium safe negative pole, but it is in charge and discharge The big problem of huge volume change does not solve at all in electric process, can't directly be commercialized.
Summary of the invention
It is an object of that present invention to provide one kind to synthesize lithium sulfide/porous carbon composite by heat treatment lithium sulfate and carbon source Method, this method process is simple, raw material is cheap, it is environmental-friendly, be suitble to large-scale production.The market share is accounted for using existing 90% or more graphite can reduce cost as cathode.Existing lithium-ion electric can also be continued to use on cell manufacturing techniques The production line in pond, it is only necessary to which lithium ion battery can be substituted by changing positive electrode and electrolyte and cell activation technique, real The rapid business of existing a new generation's lithium sulfide-graphite cell.The present invention is achieved by the following technical solutions,
A method of heat treatment lithium sulfate and carbon source synthesis vulcanization lithium/carbon composite material, including following procedure:
(1) press carbon source: sulfuric acid monohydrate lithium molar ratio (0.5-2): then 1 obtained aqueous solution, 60-100 DEG C of heating stirring are set In 60-100 DEG C of heat drying of baking oven, grind into powder.
(2) powder made from step (1) is placed on to the flat-temperature zone of tube furnace, under 10-300mL/min argon atmosphere with 2-10 DEG C/min is warming up to 500-700 DEG C, keeps the temperature 0.5-4h, is then warming up to 700-1000 DEG C with 2-10 DEG C/min, heat preservation 0.5-4h is cooled to 300-350 DEG C under the atmosphere of argon gas protection with the rate of 5-10 DEG C/min, then cools to room with the furnace Temperature synthesizes lithium sulfide/carbon complex to get to lithium sulfate and carbon source.
The carbon source is sucrose, glucose, citric acid or polyvinylpyrrolidone.
Prepared vulcanization lithium/carbon composite material is as positive electrode, lithium-sulfur cell of the graphite as negative electrode material.
Present invention has an advantage that dissolving be precipitated again in aqueous solution using lithium sulfate and carbon source as raw material, obtain organic The lithium sulfate particle of carbon source package, then the method heated by two steps, the first step is heat-treated so that organic carbon source is carbonized, so that water Vapour is sufficiently discharged, and second step is heat-treated so that lithium sulfate is reduced to lithium sulfide by carbon, and porous carbon coating nano-sulfur is formed in situ The structure of lithium particle.Its raw material is cheap, and preparation process and equipment are simple, it is easy to accomplish and promote.With commercialized lithium cell negative pole Material graphite can play the DOL/DME of lithium sulfide capacity as electrolyte (including LiNO as cathode, to maximize3Addition Agent).New the one of this substitution lithium ion battery may be implemented in the production equipment and technology for making full use of existing lithium ion battery For graphite-lithium sulphide battery rapid business.
Detailed description of the invention
Fig. 1 is the TEM figure of the porous carbon complex of lithium sulfide obtained by embodiment one.
Fig. 2 is the high power transmission electron microscope picture of the porous carbon complex of lithium sulfide obtained by embodiment one
Fig. 3 is the structure composition schematic diagram of lithium-sulfur cell of the present invention.
Fig. 4 is the cyclic voltammetry curve figure of lithium-sulfur cell of the present invention.
Fig. 5 is the charging and discharging curve figure of lithium-sulfur cell of the present invention.
Fig. 6 is the cycle performance figure of lithium-sulfur cell of the present invention.
Specific embodiment
Below with reference to example, the present invention will be further described, these examples are only intended to illustrate the present invention, and unlimited The system present invention.
Embodiment one
By sulfuric acid monohydrate lithium and glucose with molar ratio 2:1 obtained aqueous solution, 80 DEG C of heating water bath stirrings are subsequently placed in baking 80 DEG C of heat dryings of case, grind into powder.Obtained powder is placed on to the flat-temperature zone of tube furnace, in 200ml/min argon atmospher 600 DEG C are warming up to 10 DEG C/min under enclosing, keeps the temperature 2h, is then warming up to 800 DEG C with 10 DEG C/min, keeps the temperature 2h, is protected in argon gas Atmosphere under with the rate of 10 DEG C/min be cooled to 350 DEG C, cool to room temperature with the furnace then to get multiple to lithium sulfide@porous carbon Close object.Attached drawing 1 is the X-ray diffraction analysis of the porous carbon complex of lithium sulfide, and determination has obtained the lithium sulfide of pure phase.Attached drawing 2 is Its high power transmission electron microscope picture, display nanoscale lithium sulfide particle be evenly distributed in carbon skeleton, by choose electronic diffraction and Interplanar distance analysis can also determine lithium sulfide phase.
Attached drawing 3 is the structure composition schematic diagram of lithium-sulfur cell of the present invention.1.3:1 matches positive and negative anodes capacity and goes to assemble in proportion Battery.The battery installed is shelved and carries out electrochemical property test afterwards for 24 hours.Attached drawing 4 is that battery carries out cyclic voltammetry.First make Current value is charged to constant pressure (2V) to stop less than 0.02C, then carries out constant-current charge to 3.5-4 V using the electric current of 0.05C Battery is activated, then battery carries out charge-discharge test with the size of current of 0.01C in the section of 1.3V-2.8V, fills Discharge curve is as shown in Fig. 5.The cycle performance of battery is as shown in Fig. 6, the cycle performance figure under 0.1C multiplying power.
Embodiment two
By sulfuric acid monohydrate lithium and glucose with molar ratio 1:1 obtained aqueous solution, 80 DEG C of heating water bath stirrings are subsequently placed in baking 80 DEG C of heat dryings of case, grind into powder.Obtained powder is placed on to the flat-temperature zone of tube furnace, in 200ml/min argon atmospher 600 DEG C are warming up to 10 DEG C/min under enclosing, keeps the temperature 2h, is then warming up to 800 DEG C with 10 DEG C/min, keeps the temperature 2h, is protected in argon gas Atmosphere under with the rate of 10 DEG C/min be cooled to 350 DEG C, cool to room temperature with the furnace then to get multiple to lithium sulfide@porous carbon Close object.
1.3:1 matches positive and negative anodes capacity and goes assembled battery in proportion.The battery installed is shelved and carries out charge and discharge survey afterwards for 24 hours Examination: current value first is charged to using constant pressure (1.5V) and is stopped less than 0.02C, then carries out constant-current charge using the electric current of 0.05C Battery is activated to 3.8V, then battery carries out charge and discharge electrical measurement with the size of current of 0.01C in the section of 1.3V-2.8V Examination.
Embodiment three
By sulfuric acid monohydrate lithium and citric acid with molar ratio 2:1 obtained aqueous solution, 80 DEG C of heating water bath stirrings are subsequently placed in baking 80 DEG C of heat dryings of case, grind into powder.Obtained powder is placed on to the flat-temperature zone of tube furnace, in 200ml/min argon atmospher 600 DEG C are warming up to 10 DEG C/min under enclosing, keeps the temperature 2h, is then warming up to 800 DEG C with 10 DEG C/min, keeps the temperature 2h, is protected in argon gas Atmosphere under with the rate of 10 DEG C/min be cooled to 350 DEG C, cool to room temperature with the furnace then to get multiple to lithium sulfide@porous carbon Close object.
1.3:1 matches positive and negative anodes capacity and goes assembled battery in proportion.The battery installed is shelved and carries out charge and discharge survey afterwards for 24 hours Examination: current value first is charged to using constant pressure (2V) and is stopped less than 0.02C, then carries out constant-current charge extremely using the electric current of 0.05C 3V activates battery, and then battery carries out charge-discharge test with the size of current of 0.01C in the section of 1.3V-2.8V.
Example IV
By sulfuric acid monohydrate lithium and glucose with molar ratio 2:1 obtained aqueous solution, 60 DEG C of heating water bath stirrings are subsequently placed in baking 60 DEG C of heat dryings of case, grind into powder.Obtained powder is placed on to the flat-temperature zone of tube furnace, in 200ml/min argon atmospher 600 DEG C are warming up to 10 DEG C/min under enclosing, keeps the temperature 2h, is then warming up to 800 DEG C with 10 DEG C/min, keeps the temperature 2h, is protected in argon gas Atmosphere under with the rate of 10 DEG C/min be cooled to 350 DEG C, cool to room temperature with the furnace then to get multiple to lithium sulfide@porous carbon Close object.
1.1:1 matches positive and negative anodes capacity and goes assembled battery in proportion.The battery installed is shelved and carries out charge and discharge survey afterwards for 24 hours Examination: current value first is charged to using constant pressure (2V) and is stopped less than 0.02C, then carries out constant-current charge extremely using the electric current of 0.05C 3.8V activates battery, and then battery carries out charge and discharge electrical measurement with the size of current of 0.01C in the section of 1.3V-2.8V Examination.
Embodiment five
By sulfuric acid monohydrate lithium and glucose with molar ratio 2:1 obtained aqueous solution, 80 DEG C of heating water bath stirrings are subsequently placed in baking 80 DEG C of heat dryings of case, grind into powder.Obtained powder is placed on to the flat-temperature zone of tube furnace, in 40ml/min argon atmospher 600 DEG C are warming up to 10 DEG C/min under enclosing, keeps the temperature 2h, is then warming up to 800 DEG C with 10 DEG C/min, keeps the temperature 2h, is protected in argon gas Atmosphere under with the rate of 10 DEG C/min be cooled to 350 DEG C, cool to room temperature with the furnace then to get multiple to lithium sulfide@porous carbon Close object.
1.3:1 matches positive and negative anodes capacity and goes assembled battery in proportion.The battery installed is shelved and carries out charge and discharge survey afterwards for 24 hours Examination: current value first is charged to using constant pressure (1.5V) and is stopped less than 0.02C, then carries out constant-current charge using the electric current of 0.05C Battery is activated to 3.8V, then battery carries out charge and discharge electrical measurement with the size of current of 0.01C in the section of 1.3V-2.8V Examination.

Claims (3)

1. a kind of method of heat treatment lithium sulfate and carbon source synthesis vulcanization lithium/carbon composite material, including following procedure:
(1) press carbon source: sulfuric acid monohydrate lithium molar ratio (0.5-2): 1 obtained aqueous solution, 60-100 DEG C of heating stirring are subsequently placed in baking 60-100 DEG C of heat drying of case, grind into powder.
(2) powder made from step (1) is placed on to the flat-temperature zone of tube furnace, with 2-10 under 10-300mL/min argon atmosphere DEG C/min is warming up to 500-700 DEG C, 0.5-4h is kept the temperature, is then warming up to 700-1000 DEG C with 2-10 DEG C/min, keeps the temperature 0.5-4h, It is cooled to 300-350 DEG C with the rate of 5-10 DEG C/min under the atmosphere of argon gas protection, cools to room temperature with the furnace then to get arriving Lithium sulfate and carbon source synthesize lithium sulfide/carbon complex.
2. the method belonging to according to claim 1, which is characterized in that the carbon source is sucrose, glucose, citric acid or poly- second Alkene pyrrolidone.
3. vulcanization lithium/carbon composite material prepared by claim 1 is as positive electrode, lithium sulphur electricity of the graphite as negative electrode material Pond.
CN201811138305.3A 2018-09-28 2018-09-28 A kind of method synthesizing vulcanization lithium/carbon composite material and the lithium-sulfur cell using the material Pending CN109360953A (en)

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CN109962222A (en) * 2019-03-04 2019-07-02 杭州电子科技大学 A method of lithium sulfur battery anode material is prepared using bacteria cellulose aquagel
CN110137462A (en) * 2019-05-10 2019-08-16 浙江大学 Preparation method for aluminium/lithium sulphide battery vulcanization lithium/carbon composite material
CN110212180A (en) * 2019-05-22 2019-09-06 杭州电子科技大学 A kind of preparation method and lithium-sulfur cell of lithium sulfide self-supporting carbon ball/carbon nano-fiber composite material
CN112133919A (en) * 2020-09-23 2020-12-25 杭州怡莱珂科技有限公司 Sulfide-carbon in-situ composite material, electrode, preparation method of electrode and battery
CN112490420A (en) * 2020-11-05 2021-03-12 浙江大学 Maltose-derived carbon/lithium sulfide composite electrode material and preparation method and application thereof
CN112520763A (en) * 2020-08-03 2021-03-19 浙江工业大学 Method for preparing lithium sulfide by using lithium sulfate
CN113078304A (en) * 2021-03-24 2021-07-06 吉林师范大学 Lithium-sulfur battery mixed positive electrode and preparation method thereof

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CN107275571A (en) * 2017-08-18 2017-10-20 华南师范大学 A kind of full battery of lithium sulfide/nano-silicone wire/carbon and preparation method and application

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109962222A (en) * 2019-03-04 2019-07-02 杭州电子科技大学 A method of lithium sulfur battery anode material is prepared using bacteria cellulose aquagel
CN110137462A (en) * 2019-05-10 2019-08-16 浙江大学 Preparation method for aluminium/lithium sulphide battery vulcanization lithium/carbon composite material
CN110212180A (en) * 2019-05-22 2019-09-06 杭州电子科技大学 A kind of preparation method and lithium-sulfur cell of lithium sulfide self-supporting carbon ball/carbon nano-fiber composite material
CN112520763A (en) * 2020-08-03 2021-03-19 浙江工业大学 Method for preparing lithium sulfide by using lithium sulfate
CN112520763B (en) * 2020-08-03 2022-04-15 浙江工业大学 Method for preparing lithium sulfide by using lithium sulfate
CN112133919A (en) * 2020-09-23 2020-12-25 杭州怡莱珂科技有限公司 Sulfide-carbon in-situ composite material, electrode, preparation method of electrode and battery
CN112490420A (en) * 2020-11-05 2021-03-12 浙江大学 Maltose-derived carbon/lithium sulfide composite electrode material and preparation method and application thereof
CN112490420B (en) * 2020-11-05 2022-04-12 浙江大学 Maltose-derived carbon/lithium sulfide composite electrode material and preparation method and application thereof
CN113078304A (en) * 2021-03-24 2021-07-06 吉林师范大学 Lithium-sulfur battery mixed positive electrode and preparation method thereof

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