CN102163712B - Preparation method of sulfur positive material of lithium sulfur battery - Google Patents
Preparation method of sulfur positive material of lithium sulfur battery Download PDFInfo
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- CN102163712B CN102163712B CN2011100631927A CN201110063192A CN102163712B CN 102163712 B CN102163712 B CN 102163712B CN 2011100631927 A CN2011100631927 A CN 2011100631927A CN 201110063192 A CN201110063192 A CN 201110063192A CN 102163712 B CN102163712 B CN 102163712B
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- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a preparation method of a sulfur positive material of a lithium sulfur battery. The preparation method comprises the following steps: dissolving weighed acetylene black in absolute ethanol, adding a binder, carrying out ultrasonic oscillation for evenly mixing the acetylene black and the binder so as to obtain a mixed slurry, wherein the mass part ratio of the acetylene black to the binder is (2:1)-(8:1); smearing the obtained slurry on the surface of a conductive material, then placing in a drying oven, and evaporating so that the conductive material smeared with the slurry is used as a positive electrolysis sheet; cutting metal or conductive non-metal material of the same specification to be used as a negative electrolysis sheet; and preparing a 0.1-1.0moL/L Na2S solution and a corresponding NaOH solution, connecting the positive electrolysis sheet and the negative electrolysis sheet, separating a positive groove from a negative groove by using a diaphragm, and introducing 10-50mA/cm<2> of current to electrolyze for 5 hours-9 hours so as to obtain the sulfur positive material of the lithium sulfur battery. The sulfur positive compound material exhibits good electrochemistry property, the initial discharge specific capacity is up to 615.5mAh/g, the discharge specific capacity of the battery is still 276.9mAh/g after 30-time circulation at room temperature, and the capacity maintaining rate is up to 53.61%.
Description
Technical field
The present invention relates to a kind of preparation method of sulphur positive electrode of lithium-sulfur cell.
Background technology
Now, " bottleneck " of restriction lithium battery capacity is the positive electrode of lithium battery, and all the time, there is increase but no decrease in enthusiasm to this research for people.Elemental sulfur has the electrochemistry ability of polyelectron reduction reaction, and the relative atomic mass of its sulphur is less, therefore elemental sulfur has the high theoretical specific capacity up to 1675mAh/g, the theoretical energy content of battery density of lithium-sulfur cell can reach 2600W/kg especially, be far longer than existing business-like secondary cell, the lithium-sulfur cell operating voltage can be used for most of occasions about 2.1V; Secondly, sulphur aboundresources and cheap.
The advantages such as the sulfur compound positive electrode is with its high power capacity, low cost, and hypotoxicity, cycle performance are better become and have one of positive electrode of development prospect at present most.Solving electrolytical coupling, the generation of inhibition Li dendrite and improving on the basis of the problems such as cycle performance, being expected to can be the energy storage material industrialization of this type of excellent performance, thereby have very important significance for the research tool of this type of positive electrode, the researcher who hankers after lithium-sulfur cell mainly usefulness be that ball milling and distribution heating prepare the sulphur positive pole, also do not prepare the relevant report of sulphur positive electrode at present with electrolysis.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the sulphur positive electrode that discharges and recharges, overcome preparation method's complexity in the prior art, cost is high, and the poor shortcoming of the not high invertibity of electro-chemical activity.
Preparation method's technical scheme of the sulphur positive pole of lithium-sulfur cell of the present invention is as follows:
A) take by weighing acetylene black it is dispersed in the absolute ethyl alcohol, add binding agent, sonic oscillation mixes it, gets mixed slurry; The ratio of quality and the number of copies of acetylene black and binding agent is 2: 1～8: 1;
B) mixed slurry that step a) is obtained evenly is applied in the electric conducting material surface, places drying box dry, evaporates fully to ethanol, as anodal electrolytic strip;
C) cutting and step b) metal or the conductive non-metals material of same size, use absolute ethanol washing, drying is as the negative pole electrolytic strip;
D) Na of configuration 0.1-1.0moL/L
2The NaOH solution of S solution and respective concentration, sodium sulfide solution is injected the anodal groove of electrolytic cell, the NaOH solution of respective concentration is injected the negative pole groove of electrolytic cell, connect anodal electrolytic strip and negative pole electrolytic strip, separate logical 10～50mA/cm between anodal groove and the negative pole groove with barrier film
2Current electroanalysis 5h～19h;
E) with steps d) the anodal electrolytic strip of gained washs with distilled water, removes surperficial alkali lye, places drying box to be dried to distilled water and evaporates fully, obtains the sulphur positive electrode of lithium-sulfur cell.
Described binding agent is polytetrafluoroethylene, poly(ethylene oxide), polymethyl methacrylate or polyvinylidene fluoride.
The electric conducting material of described anodal electrolytic strip is wire netting, porous metal material or carbon fiber felt.
The used barrier film of electrolytic cell is perfluorinated sulfonic acid type proton exchange membrane.
The present invention is that electrolysis has successfully prepared the sulphur anode composite material that a kind of lithium-sulfur cell is used with a kind of brand-new preparation method, characterize by the performance of x-ray powder crystal diffraction (XRD) analytical test means to composite material, utilize the Land battery test system that the chemical property of material is tested.The result shows: this composite material has shown good chemical property, and its initial discharge specific capacity at room temperature still remains on 276.9mAh/g through battery discharge specific capacity after 30 circulations up to 516.5mAh/g, and capability retention is up to 53.61%.
Description of drawings
The XRD spectra of Fig. 1 embodiment 5 (nickel foam) gained positive electrode;
The charge-discharge performance figure of Fig. 2 embodiment 5 (nickel foam) resulting materials assembled battery;
The charging and discharging curve first time of Fig. 3 embodiment 5 (nickel foam) resulting materials assembled battery.
Embodiment
Embodiment 1
The sodium sulfide solution of configuration 0.1moL/L injects electrolysis tank as anode electrolyte.The sodium hydroxide solution of configuration same concentrations injects electrolysis tank as negative pole electrolyte.As positive plate, the nickel sheet leads to 10mA/cm as negative plate with nickel foam acetylene black composite material (mass ratio of acetylene black and polytetrafluoroethylene is 2: 1)
2Current electroanalysis stops energising when nickel foam begins to be dissolved in electrolyte.With the anodal electrolytic strip of distilled water washing gained, remove surperficial remaining alkali lye, place the dry circular positive plate that is washed into afterwards certain specification with punching pin of vacuum drying chamber, lithium metal is as negative plate, and PP/PE/PP is as barrier film LiPF
6-EC/DMC assembles the performance that button cell is used Land battery test system test battery as electrolyte in being full of the vacuum drying chamber of argon gas.
Embodiment 2
The sodium sulfide solution of configuration 0.2moL/L injects electrolysis tank as anode electrolyte.The sodium hydroxide solution of configuration same concentrations injects electrolysis tank as negative pole electrolyte.As positive plate, the conduction carbon paper leads to 15mA/cm as negative plate with carbon fiber felt acetylene black composite material (mass ratio of acetylene black and poly(ethylene oxide) is 5: 1)
2Current electroanalysis stops electrolysis when being covered with sulphur simple substance on the carbon fiber felt.With the anodal electrolytic strip of distilled water washing gained, remove surperficial remaining alkali lye, place the dry circular positive plate that is washed into afterwards certain specification with punching pin of vacuum drying chamber, lithium metal is as negative plate, and PP/PE/PP is as barrier film LiPF
6-EC/DMC assembles the performance that button cell is used Land battery test system test battery as electrolyte in being full of the vacuum drying chamber of argon gas.
Embodiment 3
The sodium sulfide solution of configuration 0.3moL/L injects electrolysis tank as anode electrolyte.The sodium hydroxide solution of configuration same concentrations injects electrolysis tank as negative pole electrolyte.As positive plate, the titanium net leads to 25mA/cm as negative plate with titanium net acetylene black composite material (mass ratio of acetylene black and polymethyl methacrylate is 3: 1)
2Current electroanalysis stops electrolysis when titanium is covered with sulphur simple substance on the net.With the anodal electrolytic strip of distilled water washing gained, remove surperficial remaining alkali lye, place the dry circular positive plate that is washed into afterwards certain specification with punching pin of vacuum drying chamber, lithium metal is as negative plate, and PP/PE/PP is as barrier film LiPF
6-EC/DMC assembles the performance that button cell is used Land battery test system test battery as electrolyte in being full of the vacuum drying chamber of argon gas.
Embodiment 4
The sodium sulfide solution of configuration 0.4moL/L injects electrolysis tank as anode electrolyte.The sodium hydroxide solution of configuration same concentrations injects electrolysis tank as negative pole electrolyte.As positive plate, the titanium net leads to 35mA/cm as negative plate with nickel foam acetylene black composite material (mass ratio of acetylene black and polyvinylidene fluoride is 7: 1)
2Current electroanalysis stops energising when nickel foam begins to be dissolved in electrolyte.With the anodal electrolytic strip of distilled water washing gained, remove surperficial remaining alkali lye, place the dry circular positive plate that is washed into afterwards certain specification with punching pin of vacuum drying chamber, lithium metal is as negative plate, and PP/PE/PP is as barrier film LiPF
6-EC/DMC assembles the performance that button cell is used Land battery test system test battery as electrolyte in being full of the vacuum drying chamber of argon gas.
The sodium sulfide solution of configuration 0.5moL/L injects electrolysis tank as anode electrolyte.The sodium hydroxide solution of configuration same concentrations injects electrolysis tank as negative pole electrolyte.As positive plate, copper sheet leads to 25mA/cm as negative plate with nickel foam acetylene black composite material (mass ratio of acetylene black and polytetrafluoroethylene is 2: 1)
2Current electroanalysis stops energising when nickel foam begins to be dissolved in electrolyte.With the anodal electrolytic strip of distilled water washing gained, remove surperficial remaining alkali lye, place the dry circular positive plate that is washed into afterwards certain specification with punching pin of vacuum drying chamber, lithium metal is as negative plate, and PP/PE/PP is as barrier film LiPF
6-EC/DMC assembles the performance that button cell is used Land battery test system test battery as electrolyte in being full of the vacuum drying chamber of argon gas.Such as Fig. 1, Fig. 2 and shown in Figure 3, a series of comparatively sharp-pointed diffraction maximums appear in the XRD figure of composite material, show crystalline state sulphur and the amorphous state sulphur in the material and deposit, the battery that this composite material the is assembled 516.5mAh/g that discharges for the first time, also remain 276.9mAh/g after 30 circulations, capability retention is up to 53.61%, and about charging platform 2.1V, discharge platform is greatly about 1.8V.
Embodiment 6
The sodium sulfide solution of configuration 0.6moL/L injects electrolysis tank as anode electrolyte.The sodium hydroxide solution of configuration same concentrations injects electrolysis tank as negative pole electrolyte.As positive plate, copper sheet leads to 45mA/cm as negative plate with titanium net acetylene black composite material (mass ratio of acetylene black and polymethyl methacrylate is 4: 1)
2Current electroanalysis stops energising when the titanium net surface is covered with elemental sulfur.With the anodal electrolytic strip of distilled water washing gained, remove surperficial remaining alkali lye, place the dry circular positive plate that is washed into afterwards certain specification with punching pin of vacuum drying chamber, lithium metal is as negative plate, and PP/PE/PP is as barrier film LiPF
6-EC/DMC assembles the performance that button cell is used Land battery test system test battery as electrolyte in being full of the vacuum drying chamber of argon gas.
Embodiment 7
The sodium sulfide solution of configuration 0.7moL/L injects electrolysis tank as anode electrolyte.The sodium hydroxide solution of configuration same concentrations injects electrolysis tank as negative pole electrolyte.As positive plate, the conduction carbon paper leads to 50mA/cm as negative plate with nickel foam acetylene black composite material (mass ratio of acetylene black and poly(ethylene oxide) 8: 1)
2Current electroanalysis stops energising when nickel foam begins to be dissolved in electrolyte.With the anodal electrolytic strip of distilled water washing gained, remove surperficial remaining alkali lye, place the dry circular positive plate that is washed into afterwards certain specification with punching pin of vacuum drying chamber, lithium metal is as negative plate, and PP/PE/PP is as barrier film LiPF
6-EC/DMC assembles the performance that button cell is used Land battery test system test battery as electrolyte in being full of the vacuum drying chamber of argon gas.
Embodiment 8
The sodium sulfide solution of configuration 0.8moL/L injects electrolysis tank as anode electrolyte.The sodium hydroxide solution of configuration same concentrations injects electrolysis tank as negative pole electrolyte.As positive plate, the nickel sheet leads to 25mA/cm as negative plate with titanium net acetylene black composite material (mass ratio of acetylene black and polytetrafluoroethylene is 6: 1)
2Current electroanalysis stops energising when titanium is covered with elemental sulfur on the net.With the anodal electrolytic strip of distilled water washing gained, remove surperficial remaining alkali lye, place the dry circular positive plate that is washed into afterwards certain specification with punching pin of vacuum drying chamber, lithium metal is as negative plate, and PP/PE/PP is as barrier film LiPF
6-EC/DMC assembles the performance that button cell is used Land battery test system test battery as electrolyte in being full of the vacuum drying chamber of argon gas.
Embodiment 9
The sodium sulfide solution of configuration 0.9moL/L injects electrolysis tank as anode electrolyte.The sodium hydroxide solution of configuration same concentrations injects electrolysis tank as negative pole electrolyte.Carbon fiber felt acetylene black composite material (mass ratio of acetylene black and poly(ethylene oxide) is 3: 1) is as positive plate, and copper sheet leads to 25mA/cm as negative plate
2Current electroanalysis stops electrolysis when being covered with sulphur simple substance on the carbon fiber felt.With the anodal electrolytic strip of distilled water washing gained, remove surperficial remaining alkali lye, place the dry circular positive plate that is washed into afterwards certain specification with punching pin of vacuum drying chamber, lithium metal is as negative plate, and PP/PE/PP is as barrier film LiPF
6-EC/DMC assembles the performance that button cell is used Land battery test system test battery as electrolyte in being full of the vacuum drying chamber of argon gas.
The sodium sulfide solution of configuration 1.0moL/L injects electrolysis tank as anode electrolyte.The sodium hydroxide solution of configuration same concentrations injects electrolysis tank as negative pole electrolyte.As positive plate, the titanium net leads to 25mA/cm as negative plate with carbon fiber felt acetylene black composite material (mass ratio of acetylene black and polyvinylidene fluoride is 2: 1)
2Current electroanalysis stops electrolysis when being covered with sulphur simple substance on the carbon fiber felt.With the anodal electrolytic strip of distilled water washing gained, remove surperficial remaining alkali lye, place the dry circular positive plate that is washed into afterwards certain specification with punching pin of vacuum drying chamber, lithium metal is as negative plate, and PP/PE/PP is as barrier film LiPF
6-EC/DMC assembles the performance that button cell is used Land battery test system test battery as electrolyte in being full of the vacuum drying chamber of argon gas.
Can prepare at ambient temperature lithium-sulfur cell sulfur-bearing positive electrode by this method, the carbyne polysulfide particle diameter that electrolysis makes is less, and closer to acetylene black, electrolysis is easier to implant in the nano aperture of the acetylene black with space chain structure sulphur.
Table one
The method of precise marking lithium-sulfur cell state-of-charge of the present invention, those skilled in the art can be by using for reference this paper content, and the links such as appropriate change technological parameter, structural design realize.System of the present invention is described by different examples of implementation, and person skilled obviously can be changed or suitably change and combination system as herein described within not breaking away from content of the present invention, spirit and scope, realizes the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are deemed to be included in spirit of the present invention, scope and the content.
Claims (5)
1. the preparation method of the sulphur positive pole of a lithium-sulfur cell is characterized in that step is as follows:
A) take by weighing acetylene black it is dispersed in the absolute ethyl alcohol, add binding agent, sonic oscillation mixes it, gets mixed slurry; The ratio of quality and the number of copies of acetylene black and binding agent is 2: 1～8: 1;
B) mixed slurry that step a) is obtained evenly is applied in the electric conducting material surface, places drying box dry, evaporates fully to ethanol, as anodal electrolytic strip;
C) cutting and step b) metal or the conductive non-metals material of same size, use absolute ethanol washing, drying is as the negative pole electrolytic strip;
D) Na of configuration 0.1-1.0moL/L
2The NaOH solution of S solution and respective concentration, sodium sulfide solution is injected the anodal groove of electrolytic cell, the NaOH solution of respective concentration is injected the negative pole groove of electrolytic cell, connect anodal electrolytic strip and negative pole electrolytic strip, separate logical 10～50mA/cm between anodal groove and the negative pole groove with barrier film
2Current electroanalysis 5h～19h;
E) with steps d) the anodal electrolytic strip of gained washs with distilled water, removes surperficial alkali lye, places drying box to be dried to distilled water and evaporates fully, obtains the sulphur positive electrode of lithium-sulfur cell.
2. preparation method as claimed in claim 1 is characterized in that described binding agent is polytetrafluoroethylene, poly(ethylene oxide), polymethyl methacrylate or polyvinylidene fluoride.
3. preparation method as claimed in claim 1, the electric conducting material that it is characterized in that described anodal electrolytic strip is porous metal material or carbon fiber felt.
4. preparation method as claimed in claim 3 is characterized in that described porous metal material is wire netting.
5. preparation method as claimed in claim 1 is characterized in that the used barrier film of electrolytic cell is perfluorinated sulfonic acid type proton exchange membrane.
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| CN105070893A (en) * | 2015-07-07 | 2015-11-18 | 大连理工大学 | Porous carbon/sulfur cathode material of lithium-sulfur battery and preparation method for cathode material |
| CN110010857B (en) * | 2018-01-04 | 2022-07-05 | 天津大学 | Composite material based on metal phthalocyanine compound-carbon and application thereof in lithium-sulfur battery |
| CN114284491A (en) * | 2021-12-28 | 2022-04-05 | 杭州电子科技大学 | Hard carbon electrode with high coulombic efficiency and preparation method thereof |
| CN114597411B (en) * | 2022-03-02 | 2023-03-14 | 陕西科技大学 | Acetylene black flexible sulfur fixation material, preparation method thereof, sulfur fixation method and lithium-sulfur battery positive electrode |
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| CN101958414A (en) * | 2010-10-21 | 2011-01-26 | 武汉工程大学 | Method for preparing anode of lithium sulfur battery |
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| CN101958414A (en) * | 2010-10-21 | 2011-01-26 | 武汉工程大学 | Method for preparing anode of lithium sulfur battery |
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| JP特开2010-153296A 2010.07.08 |
| 王圣平等.锂硫电池硫电极的研究现状.《电池》.2010,第40卷(第4期),232-235. |
| 锂硫电池硫电极的研究现状;王圣平等;《电池》;20100831;第40卷(第4期);232-235 * |
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Effective date of registration: 20191008 Address after: 300072 Tianjin City, Nankai District Wei Jin Road No. 92 Co-patentee after: Feng Ci Dong Patentee after: Tianjin University Address before: 300072 Tianjin City, Nankai District Wei Jin Road No. 92, Tianjin University Co-patentee before: Zhejiang Zhenlong Battery Co., Ltd. Patentee before: Tianjin University |
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