CN106935905A - A kind of fibrous lithium-air battery of high-temperature stable and preparation method thereof - Google Patents
A kind of fibrous lithium-air battery of high-temperature stable and preparation method thereof Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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Abstract
The invention belongs to technical field of new energies, the fibrous lithium-air battery of specially a kind of high-temperature stable and preparation method thereof.Traditional lithium-air battery is because organic electrolyte is inflammable, explosive, volatile property limitation, often it is difficult to bear temperature higher in actual use, and the liquid condition of electrolyte often there is also the risk of leakage pollution, so as to limit its application as the wearable energy device of flexible fiber shape.And ionic liquid has relatively low vapour pressure, electrochemical window wider and superior stability, so that with splendid application prospect.The present invention is prepared for the resistant to elevated temperatures solid polymer electrolyte of energy, and the fibrous lithium-air battery for constructing high-temperature stable is combined with orientation carbon nanotube film and lithium metal based on ionic liquid and high-molecular bone frame material.The battery can at a temperature of up to 140 DEG C steady operation, and in 10 A g‑1High current under cycle charge discharge up to 380 circle more than, there is larger application prospect in high-temperature resistant fabric field.
Description
Technical field
The invention belongs to technical field of new energies, and in particular to a kind of fibrous lithium-air battery of high-temperature stable and preparation
Method.
Background technology
In recent years, new wearable energy device is emerged in multitude, wherein lithium-air battery due to its huge energy it is close
Degree has obtained extensive concern [1,2], so that the research of correlation has been promoted, further to improve their chemical property.And
In addition, an important problem is lithium-air battery performance in extreme circumstances.Under such as hot environment, generally
The organic electrolyte for using potential security risk due to its inflammable, explosive, volatile feature, and electrochemical window is inadequate
Width, and liquid electrolyte there is also the risk of leakage in use, these all limit lithium-air battery development [3,
4], so a kind of lithium-air battery for being capable of steady operation in high temperature environments has significant importance.
At present it has been reported that the lithium-air battery of high-temperature stable have been realized in battery tolerable temperature relative to room temperature
Preliminary lifting, and with preferable stability [5,6].But the strategy of majority is using the electrolyte of inoganic solids, this kind
Electrolyte prepares complicated, condition harshness, and the most fragility of electrolyte, pliability deficiency [5]；Another strategy is to employ
Used as electrolyte, this kind of shortcoming of electrolyte is then embodied in that temperature must be up to more than fuse salt fusing point could just for mixed melting salt
Often work so that cannot under common room temperature environment normal work [6].And ionic liquid is used as a kind of new green solvent,
With relatively low vapour pressure, electrochemical window wider and superior stability, so that with splendid application prospect.For upper
State situation, we employ ionic liquid composite high-molecular material, devise it is a kind of can steady operation in high temperature environments
Fibrous lithium-air battery.This kind of lithium-air battery can at a temperature of up to 140 DEG C steady operation, and in 10 A g-1
High current under cycle charge discharge 380 circle more than.
The content of the invention
It is an object of the invention to provide it is a kind of can steady operation at high temperature fibrous lithium-air battery and its system
Preparation Method.
The fibrous lithium-air battery of the high-temperature stable that the present invention is provided, concrete composition is as follows：
（1）To be placed in the long and thin metal lithium silk of battery internal layer as negative pole；
（2）With the ionic liquid composite high-molecular material being placed in the middle part of fibrous lithium-air battery coaxial configuration, as high temperature resistant
Solid polymer electrolyte；
（3）To be placed in the porous carbon nanomaterial of battery outer layer as positive pole.
In the present invention, described long and thin metal lithium silk any surface finish, not oxidized, diameter is in 0.1-3 mm.
In the present invention, described lithium metal silk is inserted into conducting metal collector（Material can be copper, nickel, aluminium, stainless steel
Deng）Extraction electrode.
In the present invention, described high temperature resistant solid polymer electrolyte is by (Kynoar-hexafluoropropene) copolymer
The acetonitrile solution of 1-METHYLPYRROLIDONE solution and lithium salts and ionic liquid is mixing cured to be obtained.I.e. described high temperature resistant solid-state
In polymer dielectric, it is embedded in as framework material, lithium salts and ionic liquid using (Kynoar-hexafluoropropene) copolymer
Wherein.
In the present invention, the quality in the 1-METHYLPYRROLIDONE solution of (Kynoar-hexafluoropropene) copolymer
Than for：(Kynoar-hexafluoropropene) copolymer：1-METHYLPYRROLIDONE solution=(3 ~ 6):(7~4)；And lithium salts：Ionic liquid
Body：Acetonitrile=(2 ~ 3):(3~5):(3~4)（Mass ratio）.
In the present invention, the lithium salts is bis-trifluoromethylsulfoandimide lithium, lithium hexafluoro phosphate, double（Trifluoromethane sulfonyl group）Miaow
One kind in azoles lithium, TFMS lithium, hexafluoroarsenate lithium, di-oxalate lithium borate, LiBF4, lithium perchlorate etc., or its
In several mixing；Ionic liquid is (trimethyl fluoride sulfonyl) acid imide of 1- normal-butyl -1- crassitudes two, 1- butyl -3- first
Base imidazoles tetrafluoro boric acid, trimethyl n-hexyl ammonium two (trimethyl fluoride sulfonyl) imines, (fluoroform of N- Methyl-N-propyls pyrroles two
Base sulphonyl) one kind in imines, (trimethyl fluoride sulfonyl) imines of 1- butyl -4- picolines two etc., or wherein several mixing.
In the present invention, described porous carbon nanomaterial is to be orientated or random carbon nano-tube material, grapheme material etc..
The preparation method of the fibrous lithium-air battery of the above-mentioned high-temperature stable that the present invention is provided, comprises the following steps that：
（1）By extraction electrode in the not oxidized long and thin metal lithium silk of conducting metal collector insertion light；
（2）The particle and 1-METHYLPYRROLIDONE of (Kynoar-hexafluoropropene) copolymer are mixed by a certain percentage
Uniformly, Polymer Solution is obtained；
（3）By lithium salts, ionic liquid and acetonitrile mixing and stirring by a certain percentage, mixing salt solution is obtained；
（4）By step（2）And step（3）Resulting Polymer Solution is mixed by a certain percentage with mixing salt solution
It is even, obtain Electrolyte Gel；
（5）By step（4）Resulting Electrolyte Gel dipping is in step（1）On resulting lithium metal silk negative pole and solidify；
（6）In step（5）Porous carbon nanomaterial is swathed on the resulting lithium for having wrapped up solid electrolyte silk negative pole to be used in combination
Conductive wire or carbon nano-fiber extraction electrode, that is, obtain the fibrous lithium-air battery of described high-temperature stable.
Traditional lithium-air battery because organic electrolyte is inflammable, explosive, the limitation of volatile property, in actually used mistake
Often it is difficult to bear temperature higher in journey, and the liquid condition of electrolyte often there is also the risk of leakage pollution, from
And limit its application as the wearable energy device of flexible fiber shape.It is wider and ionic liquid has relatively low vapour pressure
Electrochemical window and superior stability so that with splendid application prospect.The present invention is based on ionic liquid and macromolecule
Framework material, be prepared for can resistant to elevated temperatures solid polymer electrolyte, and with orientation carbon nanotube film and lithium metal combination structure
The fibrous lithium-air battery of high-temperature stable is built.The battery can at a temperature of up to 140 DEG C steady operation, and
10 A g-1High current under cycle charge discharge up to 380 circle more than.In wearable field, especially high temperature wearable electronic device neck
Domain has larger application prospect.
Brief description of the drawings
Fig. 1 is the structural plan schematic diagram of the fibrous lithium-air battery of high-temperature stable.
Fig. 2 is charge and discharge platform voltage change of the fibrous lithium-air battery of high-temperature stable in the case where high/low temperature condition is changed
Figure.
Fig. 3 is temperature and 10 A gs of the fibrous lithium-air battery of high-temperature stable at 140 DEG C-1Current density under
Cycle performance.
Specific embodiment
Below in conjunction with specific implementation case, exemplary explanation and help further understands the present invention, but case study on implementation has
Body details does not represent whole technical schemes under present inventive concept merely to the explanation present invention, thus should not be construed as it is right
The restriction of the total technical scheme of the present invention, some in technical staff, increase without departing from the unsubstantiality of present inventive concept and
Change, for example, simply changed with the technical characteristic with same or similar technique effect or replaced, belong to present invention protection model
Enclose.
Embodiment 1
（1）It is prepared by lithium metal silk negative pole：Take any surface finish, not oxidized diameter then takes one in one section of the lithium metal silk of 1 mm
Copper wire is cut, in partial insertion lithium metal silk, extraction electrode；
（2）It is prepared by Polymer Solution：By the particle of (Kynoar-hexafluoropropene) copolymer and 1-METHYLPYRROLIDONE according to
Mass ratio 3:After 7 mixing, achromaticity and clarification clear viscous liquids are obtained after 10 h being stirred at 60 DEG C, is completely dissolved, it is as (poly- inclined
PVF-hexafluoropropene) copolymer 1-METHYLPYRROLIDONE solution；
（3）It is prepared by the solution of lithium salts and ionic liquid：By lithium salts bis-trifluoromethylsulfoandimide lithium and ionic liquid 1- normal-butyls -1-
(trimethyl fluoride sulfonyl) acid imide of crassitude two and acetonitrile solution in mass ratio 2:3:3 mixing, after ultrasonic dissolution is uniform
To achromaticity and clarification transparency liquid, as bis-trifluoromethylsulfoandimide lithium and (the trifluoromethyl sulphur of 1- normal-butyl -1- crassitudes two
Acyl) imido acetonitrile solution；
（4）It is prepared by high temperature resistant ionic liquid polymer composite electrolyte：By step（2）In prepared (Kynoar-hexafluoro
Propylene) copolymer 1-METHYLPYRROLIDONE solution and step（3）In prepared bis-trifluoromethylsulfoandimide lithium and the positive fourths of 1-
Base -1- crassitudes two (trimethyl fluoride sulfonyl) imido acetonitrile solution in mass ratio 3:After 7 mixing, stirring ultrasound is
Even, the min of vacuum removal bubble 3 obtains ionic liquid polymer composite electrolyte；
（5）It is prepared by porous carbon nanomaterial：First on a silicon substrate by electron beam evaporation process deposit catalyst layers, structure is
Al2O3/Fe.Wherein, Al2O3Thickness is 3 nm, and Fe thickness is 0.5 nm, Al2O3Positioned at silicon chip and the centre of Fe, as buffering
Layer, Fe is used as catalyst.Chemical vapour deposition technique is used afterwards, carbon source is done with ethene, be to go back Primordial Qi with hydrogen, be to carry with argon gas
Gas, synthesizes aligned carbon nanotube array on the silicon substrate for have catalyst.Wherein ethene flow is 80sccm, and argon flow amount is
300sccm, hydrogen flowing quantity is 20 sccm, and growth temperature is 720 DEG C, and growth time is 10 min.From aligned carbon nanotube array
Directly single-orientated CNT monofilm can be obtained by membrane, by controlling angle between layers and number of plies acquisition
Certain thickness and the aligned carbon nanotube film of arrangement, carbon nano-tube film are twisted and can obtain aligned carbon nanotube fibre
Dimension；
（6）It is prepared by the fibrous lithium-air battery of high-temperature stable：By step（1）In prepared lithium metal silk electrode dipping step
（4）In preparation-obtained ionic liquid polymer composite electrolyte, solidify at room temperature 3 h obtain ionic liquid polymer answer
Electrolyte is closed, afterwards again by step（5）In prepared carbon nano-tube film be wrapped in bath surface, the number of plies is 10 layers, is twined
It it is 30 degree around angle.The fibrous lithium of high-temperature stable is obtained with an aligned carbon nanotube fiber extraction electrode again afterwards
Air cell.
Embodiment 2
（1）It is prepared by lithium metal silk negative pole：Take any surface finish, not oxidized diameter then takes one in one section of the lithium metal silk of 2 mm
Aluminium wire is cut, in partial insertion lithium metal silk, extraction electrode；
（2）It is prepared by Polymer Solution：By the particle of (Kynoar-hexafluoropropene) copolymer and 1-METHYLPYRROLIDONE according to
Mass ratio 4:After 6 mixing, achromaticity and clarification clear viscous liquids are obtained after 10 h being stirred at 70 DEG C, is completely dissolved, it is as (poly-
Biasfluoroethylene-hexafluoropropylene) copolymer 1-METHYLPYRROLIDONE solution；
（3）It is prepared by the solution of lithium salts and ionic liquid：By lithium salts bis-trifluoromethylsulfoandimide lithium and ionic liquid 1- normal-butyls -1-
(trimethyl fluoride sulfonyl) acid imide of crassitude two and acetonitrile solution in mass ratio 2.5:4:3.5 mixing, ultrasonic dissolution is uniform
After obtain achromaticity and clarification transparency liquid, as bis-trifluoromethylsulfoandimide lithium and the (fluoroform of 1- normal-butyl -1- crassitudes two
Base sulphonyl) imido acetonitrile solution；
（4）It is prepared by high temperature resistant ionic liquid polymer composite electrolyte：By step（2）In prepared (Kynoar-hexafluoro
Propylene) copolymer 1-METHYLPYRROLIDONE solution and step（3）In prepared bis-trifluoromethylsulfoandimide lithium and the positive fourths of 1-
Base -1- crassitudes two (trimethyl fluoride sulfonyl) imido acetonitrile solution in mass ratio 4:After 6 mixing, stirring ultrasound is
Even, the min of vacuum removal bubble 3 obtains ionic liquid polymer composite electrolyte；
（5）It is prepared by porous carbon nanomaterial：First on a silicon substrate by electron beam evaporation process deposit catalyst layers, structure is
Al2O3/Fe.Wherein, Al2O3Thickness is 10 nm, and Fe thickness is 1 nm, Al2O3Positioned at silicon chip and the centre of Fe, as cushion,
Fe is used as catalyst.Chemical vapour deposition technique is used afterwards, carbon source is done with ethene, be also Primordial Qi with hydrogen, with argon gas as carrier gas,
Synthesize aligned carbon nanotube array on the silicon substrate for have catalyst.Wherein ethene flow is 100 sccm, and argon flow amount is 500
Sccm, hydrogen flowing quantity is 40sccm, and growth temperature is 760 DEG C, and growth time is 10 min.Can from aligned carbon nanotube array
Single-orientated CNT monofilm is obtained with direct membrane, by controlling angle between layers and number of plies acquisition one
Determine the aligned carbon nanotube film of thickness and arrangement, carbon nano-tube film is twisted and can obtain aligned carbon nanotube fiber；
（6）It is prepared by the fibrous lithium-air battery of high-temperature stable：By step（1）In prepared lithium metal silk electrode dipping step
（4）In preparation-obtained ionic liquid polymer composite electrolyte, solidify at room temperature 3 h obtain ionic liquid polymer answer
Electrolyte is closed, afterwards again by step（5）In prepared carbon nano-tube film be wrapped in bath surface, the number of plies is 20 layers, is twined
It it is 45 degree around angle.The fibrous lithium-air battery of high-temperature stable is obtained with a copper wire extraction electrode again afterwards.
Bibliography
[1] Z. Peng, S. A. Freunberger, Y. Chen, P. G. Bruce, Science2012, 337,
563.
[2] P. G. Bruce, S. A. Freunberger, L. J. Hardwick, J. M. Tarascon, Nat. Mater.2012, 11, 19.
[3] B. D. Adams, R. Black, Z. Williams, R. Fernandes, M. Cuisinier, E. J.
Berg, P. Novak, G. K. Murphy, L. F. Nazar, Adv. Energy Mater.2015, 5,
1400867.
[4] J. O. Besenhard, M. Winter, J. Yang, W. Biberacher, J. Power Sources1995, 54, 228.
[5] H. Kitaura, H. Zhou, Sci. Rep.2015, 5, 13271.
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Claims (7)
1. the fibrous lithium-air battery of a kind of high-temperature stable, it is characterised in that concrete composition is as follows：
（1）To be placed in the long and thin metal lithium silk of battery internal layer as negative pole；
（2）With the ionic liquid composite high-molecular material being placed in the middle part of fibrous lithium-air battery coaxial configuration, as high temperature resistant
Solid polymer electrolyte；
（3）To be placed in the porous carbon nanomaterial of battery outer layer as positive pole；
Wherein, described high temperature resistant solid polymer electrolyte by (Kynoar-hexafluoropropene) copolymer N- methyl pyrroles
The acetonitrile solution of pyrrolidone solution and lithium salts and ionic liquid is mixing cured to be obtained, described high temperature resistant solid polymer electrolyte
In matter, it is embedded as framework material, lithium salts and ionic liquid using (Kynoar-hexafluoropropene) copolymer.
2. the fibrous lithium-air battery of high-temperature stable according to claim 1, it is characterised in that described elongated gold
Category lithium silk any surface finish, not oxidized, diameter is in 0.1-3 mm.
3. the fibrous lithium-air battery of high-temperature stable according to claim 1, it is characterised in that described long and thin metal
Lithium silk is inserted into conducting metal collector extraction electrode.
4. the fibrous lithium-air battery of the high-temperature stable according to claim 1, it is characterised in that (polyvinylidene fluoride
Alkene-hexafluoropropene) copolymer 1-METHYLPYRROLIDONE solution in, (Kynoar-hexafluoropropene) copolymer and N- methyl
The mass ratio of pyrrolidone solution is (3 ~ 6):(7~4)；Lithium salts, ionic liquid, the mass ratio of acetonitrile are：=(2~3):(3~
5):(3~4)。
5. the fibrous lithium-air battery of the high-temperature stable according to claim 1,2,3 or 4, it is characterised in that the lithium
Salt is bis-trifluoromethylsulfoandimide lithium, lithium hexafluoro phosphate, double（Trifluoromethane sulfonyl group）Imidazoles lithium, TFMS lithium, hexafluoro
One kind in arsenic acid lithium, di-oxalate lithium borate, LiBF4, lithium perchlorate etc., or wherein several mixing；The ionic liquid
It is (trimethyl fluoride sulfonyl) acid imide of 1- normal-butyl -1- crassitudes two, 1- butyl -3- methylimidazoles tetrafluoro boric acid, front three
Base n-hexyl ammonium two (trimethyl fluoride sulfonyl) imines, N- Methyl-N-propyls pyrroles two (trimethyl fluoride sulfonyl) imines, 1- butyl-
One kind in 4- picolines two (trimethyl fluoride sulfonyl) imines etc., or wherein several mixing.
6. the fibrous lithium-air battery of the high-temperature stable according to claim 1,2,3 or 4, it is characterised in that described
Porous carbon nanomaterial is to be orientated or random carbon nano-tube material, or grapheme material.
7. a kind of preparation method of the fibrous lithium-air battery of high-temperature stable as described in one of claim 1-6, its feature
It is to concretely comprise the following steps：
（1）By extraction electrode in the not oxidized long and thin metal lithium silk of conducting metal collector insertion light；
（2）By the particle of (Kynoar-hexafluoropropene) copolymer and 1-METHYLPYRROLIDONE mixing and stirring in proportion,
Obtain Polymer Solution；
（3）By lithium salts, ionic liquid and acetonitrile mixing and stirring in proportion, mixing salt solution is obtained；
（4）By step（2）And step（3）Resulting Polymer Solution and mixing salt solution mixing and stirring in proportion, obtain
To Electrolyte Gel；
（5）By step（4）Resulting Electrolyte Gel dipping is in step（1）On resulting lithium metal silk negative pole and solidify；
（6）In step（5）Porous carbon nanomaterial is swathed on the resulting lithium for having wrapped up solid electrolyte silk negative pole to be used in combination
Conductive wire or carbon nano-fiber extraction electrode, that is, obtain the fibrous lithium-air battery of described high-temperature stable.
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| CN107579229A (en) * | 2017-09-05 | 2018-01-12 | 复旦大学 | A kind of super flexible silicon aeration cell fiber and preparation method thereof |
| CN108493459A (en) * | 2018-04-04 | 2018-09-04 | 江南大学 | A kind of threadiness air cell |
| CN108550808A (en) * | 2018-04-09 | 2018-09-18 | 中航锂电技术研究院有限公司 | A kind of composition metal cathode of lithium and preparation method thereof |
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| CN109273721A (en) * | 2017-07-18 | 2019-01-25 | 丰田自动车株式会社 | Negative electrode collector, cathode and aquo-lithium ion secondary cell |
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| CN112467258A (en) * | 2020-11-25 | 2021-03-09 | 北京航空航天大学 | Preparation method of lithium-air battery based on gel electrolyte-lithium cathode integrated structure |
| CN113178646A (en) * | 2021-04-29 | 2021-07-27 | 南京大学 | Magnesium air fiber battery and preparation method thereof |
| CN113178646B (en) * | 2021-04-29 | 2022-07-22 | 南京大学 | Magnesium air fiber battery and preparation method thereof |
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