CN103050667A - Composite anode of multi-layer structure for lithium-sulfur rechargeable battery and preparation method - Google Patents
Composite anode of multi-layer structure for lithium-sulfur rechargeable battery and preparation method Download PDFInfo
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Abstract
The invention provides a composite anode of a multi-layer structure for a lithium-sulfur rechargeable battery and a preparation method, which is characterized in that: an anode active substance, a conductive agent, and a binder are uniformly mixed, and then are coated on a current collector, and after coat is dried, a layer of conductive film is sprayed on the surface. The anode surface film is used for conducting and cutting off the sulfur in a cyclic process, thereby effectively raising a first capacity conservation rate of the battery and the cyclic stability.
Description
Technical field
The invention belongs to sulfur rechargeable battery anode preparation field, it is related to a kind of preparation method of multilayered structure composite sulfur positive pole.
Background technology
With gradually exhausting for the natural resources such as coal, oil, energy crisis has become one of key subjects that human future must be solved.And safety, cheap, high-energy-density and long-life rechargeable battery are increasingly attracted much attention.
Lithium-sulphur rechargeable battery has very wide application prospect, is most to promise to be one of candidate of following lithium battery.The theoretical specific capacity of elemental sulfur is 1675mAh/g, is assembled into battery with lithium, its theoretical specific energy reaches 2600Wh/kg, meets requirement of the electric automobile to battery, also complies with requirement of the portable type electronic product to battery " light, thin, small ".Further, since sulphur also has wide material sources, low cost, advantages of environment protection will be used widely in the lithium secondary battery.
Although lithium-sulfur cell has these advantages, also many challenge needs are faced.On the one hand, the poorly conductive (~5 × 10 of sulphur-30S/cm, 25 DEG C), cause electrochemical reaction to be difficult realization, it is difficult to be used directly to as cathode material.In order to have high conductive characteristic and reversible electrochemical reaction under high current, sulphur could must be used with additional electric conductor holding close contact as cathode material.On the other hand, the dissolving in the anion organic solvent of the polysulfide intermediate formed during the discharge and recharge, and penetrate through barrier film and reach anode, produce the sediment of electric insulation in anode（Li2S2And Li2S）, the electric conductivity of cathode of lithium is reduced, causes the poorly reversible of discharge and recharge, capacitance declines.During electric discharge, solid sediment, which expands, to be stacked into cathode surface and can result in that electrochemical reaction is irreversible, and then causes the mass loss of active matter, further results in capacity attenuation.
Challenge in terms of being dissolved for sulphur positive conductive difference and sulfide, recently carry out researcher has some to be in progress in terms of electrode material, optimization operating process and selection suitable electrolyte is improved, such as develops new electrolyte system to reduce the dissolving of sulfide in the electrolytic solution；The multiple material of carbon-sulphur is compounded to form using the carbon and sulphur of highly conductive high-specific surface area；It is carrier using conducting polymer, sulphur is penetrated into or is linked into substituted mode in polymer, conducting polymer-sulphur composite is formed；Polymer overmold is modified sulfur-bearing positive electrode etc..
The content of the invention
The technical problems to be solved by the invention are to provide a kind of many of stability for improving capability retention first and circulation for lithium-sulfur rechargeable battery（For single anode structure, one layer of plating is added on its surface）Hierarchical structure composite sulfur positive pole and preparation method.
To achieve these goals, the present inventor is attempted by the improvement to anode pole piece.Inventor attempts to pass through chemical deposition on anode pole piece surface first, electrochemical deposition, this several means is sputtered directly to spray conductive film on positive electrode to improve positive electrode, control the electric conductivity of positive electrode, and the dissolving and shuttle of sulfide in the electrolytic solution are suppressed by this fine and close conductive film sprayed on anode pole piece simultaneously, but inventor is fathomless to be whether above-mentioned trial can effectively improve the stability of capability retention first and circulation, in addition, inventor does not know what condition should be controlled yet, it can be made to be remained in the anode pole piece for coating conductive film with relatively low impedance and good electric conductivity.When inventor has found the thickness of the conductive film in the present invention for 10~1000nm by further researching and developing, it can make it that lithium-sulfur rechargeable battery has the stability of higher capability retention first and circulation.If higher than 1000nm, contact of the material with electrolyte, which can be received, to be significantly affected, and interracial contact impedance is significantly increased, substantially, chemical property is deteriorated battery polarization, weak to be less than 10nm, then plated barrier film can not effectively obstruct the dissolving of sulfide in the electrolytic solution, and efficiency and cycle performance are poor first.
Therefore, inventor proposes that technical scheme of the invention below, including step are by above-mentioned research and development：
Positive active material, conductive agent, binding agent are well mixed, on a current collector, then on its surface, the mode through magnetron sputtering, chemical deposition or electrochemical deposition sprays layer of conductive film for coating；The thickness of the conductive film is 10~1000nm.
The active material is the one or more in sulphur powder, sulphur carbon complex, inorganic sulphide, organic sulfur compound；The conductive agent is the one or more in conductive carbon black, acetylene black, graphite powder；The binding agent is the one or more in polyvinyl alcohol, ptfe emulsion, sodium carboxymethylcellulose, TPO, SBR rubber, Viton, PVDF/NMP, Polyurethane；The active material, conductive agent, the mass ratio of binding agent are 50~98：1~20：1~30.
The sulphur carbon complex is the one or more in porous carbon-sulfur compound, CNT-sulfur compound, carbon fiber-sulfur compound, graphene-sulfur compound, hollow carbon balls-sulfur compound.The weight/mass percentage composition of sulphur is 10%~90% in the sulphur carbon complex.
The collector is one kind in aluminium foil, aluminium net, carbon net, carbon film.
The composition of the conductive film is the one or more in carbon, paper tinsel, gold, silver, copper, indium, indium oxide, indium tin oxide, ruthenic oxide, polyaniline, polypyrrole.
The surface film in anode structure designed by the present invention serves conductive during circulating battery and cut of both sulphur, so as to improve the capability retention first and cyclical stability of battery.
The invention has the advantages that：
The multilayered structure composite sulfur positive pole prepared by the method for the present invention, with advantages below：On anode pole piece surface by chemical deposition, electrochemical deposition, sputtering means direct spraying conductive film, the film of spraying can have surfacing, and thickness is controllable, the characteristics of required raw material are few.The conductive film and positive electrode for being sprayed on material surface are in close contact, and technical scheme is controlled while fully suppression sulfide dissolves shuttle in the electrolytic solution well, the generation of the excessive situation of interracial contact impedance, it can make it that one aspect of the present invention adds the electric conductivity of electrode, on the other hand the exposed sulphur on surface is wrapped up, so as to which the lithium sulfide generated can be retained in cyclic process, suppress the dissolving and shuttle of sulfide in the electrolytic solution.The capability retention first and cycle performance of sulphur positive electrode with this structure of the invention are improved significantly.
In summary, the present invention is a kind of efficient method prepared with high conductivity and the multilayered structure composite sulfur positive pole that can suppress sulfide dissolving shuttle.This method can significantly improve the capability retention first and cyclical stability of lithium-sulfur cell.
Brief description of the drawings
Accompanying drawing is the structural representation of positive plate of the present invention.
Embodiment
With reference to embodiment, the invention will be further described.Following examples are intended to illustrate invention rather than limitation of the invention further.
Embodiment 1：
Using polyvinyl alcohol as binding agent, using conductive black as conductive agent, using sulfur content be respectively 10%, 25%, 50%, 75% CNT-sulphur composite as active material, according to active material：Conductive agent：Binding agent is 8:1:1 mass ratio mixing, grinding is uniform, scratches in aluminum foil current collector, 24h is dried in 60 DEG C of vacuum drying chambers, is then placed in magnetron sputter, one layer of conductive carbon is sputtered on its surface（Sputtering time is 10min, and target used is conductive carbon target）, you can multilayered structure composite sulfur positive pole is obtained, carbon film thickness is 10nm, it is assembled into button cell and its electrochemistry cycle performance is tested in 3.0~1.5V voltage ranges.1 is shown in Table under 160mA/g (S) current density.
The experiment condition and result of the example 1 of table 1
Embodiment 2：
Using PVDF as binding agent（NMP is solvent）, using acetylene black as conductive agent, using the sulphur powder that distils as active material, according to active material：Conductive agent：Binding agent is 6:3:1 mass ratio mixing, grinding is uniform, blade coating is on carbon net collector, 24h is dried in 60 DEG C of vacuum drying chambers, using it as negative electrode, using silver plate as anode, electroplate is carried out in silver nitrate solution, can obtain multilayered structure composite sulfur positive pole, thickness of coating is respectively 2,100,750,2000nm, its be assembled into button cell in 3.0~1.5V voltage ranges, its electrochemistry cycle performance is tested under 160mA/g (S) current density.It 1st、2ndWith 50thSpecific discharge capacity such as table 2.
The experiment condition and result of the example 2 of table 2
Embodiment 3：
Using sodium carboxymethylcellulose as binding agent, using conductive black as conductive agent, using molybdenum disulfide as active material, according to active material：Conductive agent：Binding agent is 5:3:2 mass ratio mixing, grinding is uniform, blade coating is on aluminium net collector, 24h is dried in 60 DEG C of vacuum drying chambers, it is inserted into after being processed in the solution containing aniline monomer, potassium persulfate solution is added dropwise dropwise, the polyaniline of generation is set to stick to pole piece, drying can obtain multilayered structure composite sulfur positive pole, thickness of coating is 1000nm, and it, which is assembled into button cell, tests its electrochemistry cycle performance in 3.0~0.3V voltage ranges, under 160mA/g (S) current density and test its electrochemistry cycle performance.It 1st、2ndWith 50thSpecific discharge capacity is respectively 1051,903,843mAh/g.
Claims (6)
1. the preparation method of a kind of multilayered structure anode composite for lithium-sulfur rechargeable battery, it is characterised in that including following preparation process：Positive active material, conductive agent, binding agent are well mixed, on a current collector, then on its surface, the mode through magnetron sputtering, chemical deposition or electrochemical deposition sprays layer of conductive film for coating；The thickness of the conductive film is 10~1000nm.
2. it is according to claim 1 a kind of for multilayered structure anode composite of lithium-sulfur rechargeable battery and preparation method thereof, it is characterised in that：The active material is the one or more in sulphur powder, sulphur carbon complex, inorganic sulphide, organic sulfur compound；The conductive agent is the one or more in conductive carbon black, acetylene black, graphite powder；The binding agent is the one or more in polyvinyl alcohol, ptfe emulsion, sodium carboxymethylcellulose, TPO, SBR rubber, Viton, PVDF/NMP, Polyurethane；The active material, conductive agent, the mass ratio of binding agent are 50~98：1~20：1~30.
3. it is piece according to claim 2 a kind of for multilayered structure anode composite of lithium-sulfur rechargeable battery and preparation method thereof, it is characterised in that：The sulphur carbon complex is the one or more in porous carbon-sulfur compound, CNT-sulfur compound, carbon fiber-sulfur compound, graphene-sulfur compound, hollow carbon balls-sulfur compound；The weight/mass percentage composition of sulphur is 10%~90% in the sulphur carbon complex.
4. it is according to claim 1 a kind of for multilayered structure anode composite of lithium-sulfur rechargeable battery and preparation method thereof, it is characterised in that：The collector is one kind in aluminium foil, aluminium net, carbon net, carbon film.
5. it is according to claim 1 a kind of for multilayered structure anode composite of lithium-sulfur rechargeable battery and preparation method thereof, it is characterised in that：The composition of the conductive film is the one or more in carbon, platinum, gold, silver, copper, indium, indium oxide, indium tin oxide, ruthenic oxide, polyaniline, polypyrrole.
6. a kind of multilayered structure anode composite for lithium-sulfur rechargeable battery obtained by the method described in claim any one of 1-5.
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| CN103515646A (en) * | 2013-09-09 | 2014-01-15 | 中南大学 | Lithium-sulfur battery with conductive adsorption layer, and application of conductive polymer film |
| CN103647104A (en) * | 2013-12-18 | 2014-03-19 | 中国科学院上海硅酸盐研究所 | Lithium-sulfur battery |
| CN104183820A (en) * | 2014-03-03 | 2014-12-03 | 河南师范大学 | Membrane material for lithium sulfur battery positive electrode |
| CN104282885A (en) * | 2013-07-10 | 2015-01-14 | 通用汽车环球科技运作有限责任公司 | Surface coating method, and method for improving the electrochemical performance of an electrode for a lithium-based battery |
| CN104300128A (en) * | 2013-07-18 | 2015-01-21 | 中国科学院大连化学物理研究所 | Integrated membrane electrode structure for lithium sulfur battery and preparation method thereof |
| CN104577051A (en) * | 2013-10-14 | 2015-04-29 | 中国电子科技集团公司第十八研究所 | Preparation method of positive electrode for lithium-sulfur secondary battery |
| CN104577060A (en) * | 2013-10-11 | 2015-04-29 | 通用汽车环球科技运作有限责任公司 | Porous interlayer for a lithium-sulfur battery |
| CN104600251A (en) * | 2014-12-26 | 2015-05-06 | 中南大学 | Lithium-sulfur battery positive electrode and preparation method thereof |
| CN104716324A (en) * | 2013-12-15 | 2015-06-17 | 中国科学院大连化学物理研究所 | Lithium-sulfur battery positive electrode making method |
| TWI504048B (en) * | 2013-10-08 | 2015-10-11 | Christine Jill Lee | Method for manufacturing lithium battery electrode |
| CN105322136A (en) * | 2014-06-24 | 2016-02-10 | 现代自动车株式会社 | Cathode for lithium-sulfur battery |
| CN105374982A (en) * | 2015-12-11 | 2016-03-02 | 中国电子科技集团公司第十八研究所 | Electrode structure of lithium sulfur battery and processing technology therefor |
| CN105514378A (en) * | 2015-12-22 | 2016-04-20 | 湘潭大学 | Lithium-sulfur battery positive-pole composite material with imitated cellular structure and preparation method thereof |
| CN105720231A (en) * | 2014-12-05 | 2016-06-29 | 中国科学院大连化学物理研究所 | Sulfonated graphene-modified sulfur-carbon electrode and preparation and application thereof |
| CN106207088A (en) * | 2016-09-30 | 2016-12-07 | 上海空间电源研究所 | A kind of lithium-sulphur cell positive electrode and preparation method thereof |
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| CN110649222A (en) * | 2019-09-29 | 2020-01-03 | 江西省科学院应用物理研究所 | Preparation method of lithium-sulfur battery positive electrode |
| CN110649222B (en) * | 2019-09-29 | 2023-02-03 | 江西省科学院应用物理研究所 | Preparation method of lithium-sulfur battery positive electrode |
| CN110911682A (en) * | 2019-11-06 | 2020-03-24 | 华南理工大学 | Electrode of lithium-sulfur battery and preparation method and application thereof |
| CN114530577A (en) * | 2020-11-23 | 2022-05-24 | 西安石油大学 | Preparation method of cobalt molybdate/1T-phase molybdenum disulfide composite lithium ion battery cathode, composite electrode material and lithium ion battery |
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