CN102368561B - Chargeable and dischargeable lithium sulfur cell - Google Patents
Chargeable and dischargeable lithium sulfur cell Download PDFInfo
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- CN102368561B CN102368561B CN2011103217990A CN201110321799A CN102368561B CN 102368561 B CN102368561 B CN 102368561B CN 2011103217990 A CN2011103217990 A CN 2011103217990A CN 201110321799 A CN201110321799 A CN 201110321799A CN 102368561 B CN102368561 B CN 102368561B
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Abstract
The invention discloses a chargeable and dischargeable lithium sulfur cell system. The system which treats a prelithiated carbon family compound as an active substance of a cathode of a lithium sulfur cell and a sulfur carbon compound as an active substance of an anode of the lithium sulfur cell allows a dendrite problem brought by a case that metallic lithium is used as the cathode to be avoidedand the safety performance of the system to be improved; and an electrolyte solution containing an ionic liquid is simultaneously used as an ionic conductor of the lithium sulfur cell, so a potentialsafety hazard brought by the use of traditional inflammable and volatile organic electrolytes is solved. The finally prepared full lithium sulfur cell has the advantages of high safety and high energy density. In addition, the system which is a full cell system which can be directly used without charge is different from traditional full cells, and the system can be directly used because the open-circuit voltage of the system is zero.
Description
Technical field
The present invention relates to a kind of lithium-sulfur cell that discharges and recharges.
Background technology
Along with the continuous progress of science and technology, the fast development of various electronic products requires used power supply to have the characteristics such as quality is light, volume is little, capacity is large, and present commercial secondary cell is subjected to the restriction of positive electrode capacity, its specific energy to be difficult to continue to improve.Because the theoretical specific capacity of lithium-sulfur cell is 1672mAhg
-1, specific energy can reach 2600Wh kg
-1, and the raw material elemental sulfur has advantages such as the source is abundant, low price, be considered to the secondary cell system that has research and application potential most of future generation, caused numerous research workers' concern.But elemental sulfur at room temperature is typical electronics and ion insulator (5 * 10
-3025 ℃ of S/cm), the sulphur reduction generates Li and in charging process
2The process of S is a multistep reaction, and many lithium sulfides of product are soluble in organic liquid electrolyte in the middle of it, and these problems all cause the electrode active material utilance low poor with cycle performance of battery.Therefore, at present most of research all concentrate on the conductivity of improving positive electrode and with the aspects such as compatibility of electrolyte.Yet, in use there is serious potential safety hazard in traditional lithium-sulfur cell: (1) is owing to use lithium metal to be negative pole, the a large amount of Li dendrites that in the process of repeated charge, easily produce on lithium sheet surface, can penetrate porous barrier film and the short circuit of inside battery occurs, have serious safety issue; (2) at present the electrolyte that uses of lithium-sulfur cell for traditional organic bath (for example: LiPF
6-EC-DMC, the liquid electrolytes such as LiTFSI-DOL-DME), there is inflammable, volatile problem in these electrolyte, so that adopt the lithium-sulfur cell of traditional organic bath to have obvious potential safety hazard.Therefore, be very significant work by the lithium-sulfur cell system that designs novel battery structure, selects the good electrolyte of fail safe to construct high security.
Summary of the invention
The purpose of this invention is to provide a kind of high security and can discharge and recharge lithium-sulfur cell.
A kind of lithium-sulfur cell that discharges and recharges provided by the invention comprises sulphur positive electrode, cathode of lithium material and electrolyte; Described electrolyte is by ionic liquid and contain lithium electrolyte salt and form.
In the above-mentioned lithium-sulfur cell, described ionic liquid can be N-ethyl-N-propyl pyrrole alkane bis trifluoromethyl sulfimide salt (P24TFSI), N-ethyl-N-butyl piperidine bis trifluoromethyl sulfimide salt (PP24TFSI), N-methyl-N-pi-allyl pyrrolidines bis trifluoromethyl sulfimide salt (P1A3TFSI), N-methyl-N-propyl pyrrole alkane bis trifluoromethyl sulfimide salt (P13TFSI), N-methyl-N-butyl pyrrolidine bis trifluoromethyl sulfimide salt (P14TFSI), N-methyl-N-pi-allyl piperidines bis trifluoromethyl sulfimide salt (PP1A3TFSI), N-methyl-N-propyl group piperidines bis trifluoromethyl sulfimide salt (PP13TFSI), N, N-dimethyl-N-ethyl-N propyl group bis trifluoromethyl sulfimide salt (N1123TFSI), trimethyl butylamine bis trifluoromethyl sulfimide salt (N1114TFSI), N, N-dimethyl-N-ethyl-N butylamine bis trifluoromethyl sulfimide salt (N1124TFSI), N, N-dimethyl-N-propyl group-N butylamine bis trifluoromethyl sulfimide salt (N1134TFSI), trimethyl hexyl amine bis trifluoromethyl sulfimide salt (N1116TFSI), the two fluorine sulfimide salt (P24FSI) of N-ethyl-N-propyl pyrrole alkane, the two fluorine sulfimide salt (PP24FSI) of N-ethyl-N-butyl piperidine, the two fluorine sulfimide salt (P1A3FSI) of N-methyl-N-pi-allyl pyrrolidines, the two fluorine sulfimide salt (P13FSI) of N-methyl-N-propyl pyrrole alkane, the two fluorine sulfimide salt (P14FSI) of N-methyl-N-butyl pyrrolidine, the two fluorine sulfimide salt (PP1A3FSI) of N-methyl-N-pi-allyl piperidines, the two fluorine sulfimide salt (PP13FSI) of N-methyl-N-propyl group piperidines, trimethyl nitrile methyl amine bis trifluoromethyl sulfimide salt (CTMATFSI), 4-butyl amine bis trifluoromethyl sulfimide salt (N2222TFSI), N, N, N-trimethyl-N-methoxy ethyl amine bis trifluoromethyl sulfimide salt (N1111O2TFSI), N, N-diethyl-N-methyl-N-methoxy ethyl amine bis trifluoromethyl sulfimide salt (N2211O2TFSI), N, N-dimethyl-N, N-diethoxy ethylamine bis trifluoromethyl sulfimide salt (N11 (2O2)
2TFSI) and N, N, one or more in N-tributyl-N-ethoxyethyl group amine bis trifluoromethyl sulfimide salt (N4442O2TFSI); The described lithium electrolyte salt that contains can be LiBF
4, LiPF
6, LiN (CF
3SO
2)
2And LiN (FSO
2)
2In one or more.
In the above-mentioned lithium-sulfur cell, in the described electrolyte, the described molar concentration that contains lithium electrolyte salt can be 0.2mol/L～1.2mol/L, specifically can be 0.5mol/L～1mol/L, 0.5mol/L or 1mol/L.
In the above-mentioned lithium-sulfur cell, described sulphur positive electrode can be one or more in sulphur-carbon mano-tube composite, sulphur-carbon hollow microsphere compound and the sulphur-mesoporous nano carbon complex; In the described positive electrode, the ratio of quality and the number of copies of two kinds of components can be (1～10): (1～10) specifically can be (1～5): (1～5), 1: 1,2: 3,3: 4,5: 4 or 3: 2.
In the above-mentioned lithium-sulfur cell, described cathode of lithium material can be the carbon group compound of pre-lithiumation, and described carbon group compound can be one or more in graphite negative electrodes material, silicon and silicon based composite material, germanium and germanium based composites and tin and the Tin Composite Material.
In the above-mentioned lithium-sulfur cell, described graphite negative electrodes material can be one or more in Delanium, native graphite and the carbonaceous mesophase spherules (MCMB); Described silicon based composite material can be one or more in silicon nanowires, silicon nanosphere, silicon-carbon micro-nano compound and the silicon nanowires carbon complex; Described germanium based composites is one or more in germanium nanosphere, Ge nanoline, germanium carbon micro-nano compound and the germanium-graphene complex; Described Tin Composite Material is one or more in tin carbon complex, stannous oxide and the tin oxide.
In the above-mentioned lithium-sulfur cell, the carbon group compound of described pre-lithiumation can prepare according to the method that comprises the steps: electrode slice and lithium metal that described carbon group compound is coated are assembled into half-cell, carry out the carbon group compound that discharge process namely gets described pre-lithiumation.
In the above-mentioned lithium-sulfur cell, the carbon group compound of described pre-lithiumation also can prepare according to the method that comprises the steps: described carbon group compound and n-BuLi are reacted the carbon group compound that namely gets described pre-lithiumation.
The present invention also provides a kind of energy storage elements, and this energy storage element comprises above-mentioned lithium-sulfur cell.
The present invention also provides a kind of portable electric appts, and this electronic equipment comprises above-mentioned can measure memory element.
Compared with prior art, the full battery of lithium sulphur that discharges and recharges provided by the invention has the characteristics of high security, high-energy-density: on the one hand, the carbon group compound of pre-lithiumation provides enough lithium sources for the full battery of this lithium sulphur, and has solved the safety problems such as short circuit that the Li dendrite generation brings; On the other hand, ionic liquid can effectively be avoided the potential safety hazard brought because of inflammable, the volatile organic electrolyte that uses at present as electrolyte; Simultaneously, lithium-sulfur cell provided by the present invention is when the carbon group compound of the pre-lithiumation of selecting high power capacity during as negative material, because negative material has higher specific capacity equally, so that the novel lithium-sulfur cell of preparation has higher energy density; In addition, the directly full battery system of use that need not to charge provided by the invention is different from the full battery of traditional secondary (must charge first and could use) fully; In sum, battery system provided by the invention has high security, high-energy-density, characteristics easy to use, has very important significance for the development of lithium ion battery industry.
Description of drawings
Fig. 1 is the constant-current discharge curve that the pre-lithiumation process of silicon-carbon micro-nano compound obtains among the embodiment 1.
Fig. 2 is the constant current charge-discharge curve of the full battery of lithium sulphur of preparation among the embodiment 1.
Fig. 3 is the cycle performance curve of the full battery of lithium sulphur of preparation among the embodiment 1.
Embodiment
Employed experimental technique is conventional method if no special instructions among the following embodiment.Used material, reagent etc. if no special instructions, all can obtain from commercial channels.
Pre-lithiumation process and battery performance test system among the following embodiment of the present invention all adopt the Swagelok battery system to test: with the active material in following examples (being the full battery of each embodiment preparation), binding agent Kynoar (PVDF) and conductive additive carbon black or acetylene black are made into slurry with mass ratio mixing in 80: 10: 10, be coated to equably on Copper Foil or the aluminum foil current collector and obtain work electrode, glass fibre membrane (Britain Whatman company) is as barrier film, electrolyte is by ionic liquid and contain lithium electrolyte salt and form, and assembling obtains Swagelok type battery in glove box.
The battery of above-mentioned assembling is carried out charge-discharge test at Arbin BT2000 charge-discharge test instrument, and the interval that discharges and recharges of test is 0.6-2.4V.
The preparation of embodiment 1, the full battery of lithium sulphur
(1) silicon-carbon micro-nano compound is coated with on Copper Foil, obtains electrode, with 1MLiPF
6-DOL/DME is electrolyte, and lithium metal by discharge process, prepares the silicon-carbon micro-nano cathode composite materials of pre-lithiumation for electrode is prepared half-cell;
(2) with the silicon-carbon micro-nano compound of the above-mentioned pre-lithiumation that makes as negative pole, (wherein, the ratio of quality and the number of copies of sulphur and carbon nano-tube is 2: 3 to sulphur-carbon mano-tube composite; This composite material prepares by the following method: take aluminium oxide as template, polyacrylonitrile is carbon source, the preparation carbon nano-tube, under 155 ℃ condition, be filled to sulphur in the above-mentioned carbon nano-tube and get final product), with N-methyl-N-pi-allyl pyrrolidines bis trifluoromethyl sulfimide salt (P1A3TFSI) as solvent and LiN (CF
3SO
2)
2Consist of electrolyte for containing lithium electrolyte salt, and LiN (CF
3SO
2)
2Molar concentration be 0.5mol/L; Consist of the full battery of lithium sulphur by above-mentioned electrode material and electrolyte.
Fig. 1 is the discharge curve that the pre-lithiumation process of silicon-carbon micro-nano compound obtains, and as can be seen from the figure discharge capacity reaches 3365mAhg
-1, illustrate that this alloy material can provide sufficient lithium source for full battery.
Fig. 2 is the charging and discharging curve of the full battery of lithium sulphur of present embodiment preparation, and the first circle discharge capacity is up to 1457mAhg
-1, and open circuit voltage 2.5V, need not charge and can directly use.
Fig. 3 is the cycle performance of the full battery of lithium sulphur of present embodiment preparation, and capacity still can keep 670mAhg behind circulation 50 circles
-1, this full battery has good cycle performance.
The preparation of embodiment 2, the full battery of lithium sulphur
(1) germanium carbon micro-nano compound is coated with on Copper Foil, obtains electrode, with 1MLiPF
6-DOL/DME is electrolyte, and lithium metal by discharge process, prepares the germanium carbon micro-nano cathode composite materials of pre-lithiumation for electrode is prepared half-cell;
(2) with the germanium carbon micro-nano compound of the above-mentioned pre-lithiumation that makes as negative pole, (wherein, the ratio of quality and the number of copies of sulphur and carbon hollow microsphere is 3: 4 to sulphur-carbon hollow microsphere compound; This composite material prepares by the following method: prepare the carbon hollow microsphere take glucose as carbon source, after 800 ℃ of processing, under 155 ℃ condition, be filled to sulphur in the above-mentioned carbon hollow microsphere and get final product), with N-methyl-N-propyl pyrrole alkane bis trifluoromethyl sulfimide salt (P13TFSI) as solvent and LiN (CF
3SO
2)
2Consist of electrolyte for containing lithium electrolyte salt, and LiN (CF
3SO
2)
2Molar concentration be 0.5mol/L; Consist of the full battery of lithium sulphur by above-mentioned electrode material and electrolyte.
The test result of the full battery of present embodiment preparation is listed in the table 1.
The preparation of embodiment 3, the full battery of lithium sulphur
(1) the silicon nanowires carbon complex is coated with on Copper Foil, obtains electrode, with 1MLiPF
6-DOL/DME is electrolyte, and lithium metal by discharge process, prepares the silicon nanowires carbon complex negative material of pre-lithiumation for electrode is prepared half-cell;
(2) with the silicon nanowires carbon complex of the above-mentioned pre-lithiumation that makes as negative pole, (wherein, the ratio of quality and the number of copies of sulphur and carbon nano-tube is 1: 1 to sulphur-carbon mano-tube composite; This composite material prepares by the following method: take aluminium oxide as template, polyacrylonitrile is carbon source, the preparation carbon nano-tube, under 155 ℃ condition, be filled to sulphur in the above-mentioned carbon nano-tube and get final product), with N-methyl-N-butyl pyrrolidine bis trifluoromethyl sulfimide salt (P14TFSI) as solvent and LiN (CF
3SO
2)
2Consist of electrolyte for containing lithium electrolyte salt, and LiN (CF
3SO
2)
2Molar concentration be 1mol/L; Consist of the full battery of lithium sulphur by above-mentioned electrode material and electrolyte.
The test result of the full battery of present embodiment preparation is listed in the table 1.
The preparation of embodiment 4, the full battery of lithium sulphur
(1) carbonaceous mesophase spherules (MCMB) is coated with on Copper Foil, obtains electrode, with 1MLiPF
6-DOL/DME is electrolyte, and lithium metal by discharge process, prepares the intermediate phase carbon microsphere negative materials of pre-lithiumation for electrode is prepared half-cell;
(2) with the carbonaceous mesophase spherules of the above-mentioned pre-lithiumation that makes as negative pole, (wherein, the ratio of quality and the number of copies of sulphur and carbon hollow microsphere is 5: 4 to sulphur-carbon hollow microsphere compound; This composite material prepares by the following method: prepare the carbon hollow microsphere take glucose as carbon source, after 800 ℃ of processing, with sulphur under 155 ℃ condition, be filled to above-mentioned carbon hollow little in and get final product), with N-methyl-N-propyl group piperidines bis trifluoromethyl sulfimide salt (PP13TFSI) as solvent and LiN (CF
3SO
2)
2Consist of electrolyte for containing lithium electrolyte salt, and LiN (CF
3SO
2)
2Molar concentration be 1mol/L; Consist of the full battery of lithium sulphur by above-mentioned electrode material and electrolyte.
The test result of the full battery of present embodiment preparation is listed in the table 1.
The preparation of embodiment 5, the full battery of lithium sulphur
(1) the tin carbon complex is coated with on Copper Foil, obtains electrode, with 1MLiPF
6-DOL/DME is electrolyte, and lithium metal by discharge process, prepares the tin carbon complex negative material of pre-lithiumation for electrode is prepared half-cell;
(2) with the tin carbon complex of the above-mentioned pre-lithiumation that makes as negative pole, (wherein, the ratio of quality and the number of copies of sulphur and mesoporous nano carbon is 6: 4 to sulphur-mesoporous nano carbon complex; This composite material prepares by the following method: take SBA-15 as template, P123 is the mesoporous nano material with carbon element that carbon source prepares ordered arrangement, under 155 ℃ condition, be filled to sulphur in the above-mentioned mesoporous nano carbon and get final product), with N-methyl-N-butyl piperidine bis trifluoromethyl sulfimide salt (PP14TFSI) as solvent and LiN (CF
3SO
2)
2Consist of electrolyte for containing lithium electrolyte salt, and LiN (CF
3SO
2)
2Molar concentration be 1mol/L; Consist of the full battery of lithium sulphur by above-mentioned electrode material and electrolyte.
The test result of the full battery of present embodiment preparation is listed in the table 1.
The test result of the lithium-sulfur cell of table 1, embodiment 1-5 preparation
From the results shown in Table 1, the safe lithium-sulfur cell system of height provided by the invention, when using the high power capacity negative material of silicon, germanium, tin class, the capacity of whole battery all can reach more than the 500mAh/g, the lithium-sulfur cell system of high security not only is provided, and the battery system of high-energy-density is provided.
Claims (1)
1. one kind can discharge and recharge lithium-sulfur cell, is prepared as follows:
(1) silicon-carbon micro-nano compound is coated with on Copper Foil, obtains electrode, with 1MLiPF
6-DOL/DME is electrolyte, and lithium metal by discharge process, prepares the silicon-carbon micro-nano cathode composite materials of pre-lithiumation for electrode is prepared half-cell;
(2) with the silicon-carbon micro-nano compound of the above-mentioned pre-lithiumation that makes as negative pole; Sulphur-carbon mano-tube composite is as positive pole; The ratio of quality and the number of copies of sulphur and carbon nano-tube is 2:3 in sulphur-carbon mano-tube composite; This composite material prepares by the following method: take aluminium oxide as template, polyacrylonitrile is carbon source, and the preparation carbon nano-tube is filled to sulphur in the above-mentioned carbon nano-tube under 155 ℃ condition and get final product; With N-methyl-N-pi-allyl pyrrolidines bis trifluoromethyl sulfimide salt as solvent and LiN (CF
3SO
2)
2Consist of electrolyte for containing lithium electrolyte salt, and LiN (CF
3SO
2)
2Molar concentration be 0.5mol/L; Consist of the full battery of lithium sulphur by above-mentioned electrode material and electrolyte.
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| CN102683747A (en) * | 2012-05-07 | 2012-09-19 | 上海交通大学 | Flame-retardant electrolyte for secondary lithium-sulfur battery and preparation method thereof |
| CN102694158A (en) * | 2012-06-13 | 2012-09-26 | 上海空间电源研究所 | Silicon-containing lithium cathode, preparation method thereof and lithium sulfur battery with silicon-containing lithium cathode |
| CN103833675B (en) * | 2012-11-26 | 2016-04-27 | 海洋王照明科技股份有限公司 | Piperidines ionic liquid and its preparation method and application |
| CN105322230A (en) * | 2014-05-29 | 2016-02-10 | 福建省辉锐材料科技有限公司 | Graphene-combining rechargeable lithium-ion battery and manufacturing method thereof |
| CN104201000B (en) * | 2014-08-21 | 2017-05-17 | 清华大学 | High-power lithium ion capacitor and manufacturing method thereof |
| CN104409770B (en) * | 2014-12-05 | 2017-01-25 | 哈尔滨工业大学 | Preparation method of polymer electrolyte containing allyl functionalized ionic liquid |
| CN105470465B (en) * | 2015-01-21 | 2018-02-13 | 万向一二三股份公司 | The prelithiation handling process and device of a kind of silicon-based anode |
| US10658701B2 (en) * | 2016-01-29 | 2020-05-19 | Semiconductor Energy Laboratory Co., Ltd. | Storage battery, battery control unit, and electronic device |
| DE102016216267A1 (en) * | 2016-08-30 | 2018-03-01 | Robert Bosch Gmbh | Chemical lithiation of electrode active material |
| US12087933B2 (en) | 2016-08-31 | 2024-09-10 | William Marsh Rice University | Anodes, cathodes, and separators for batteries and methods to make and use same |
| CN107464919A (en) * | 2017-09-12 | 2017-12-12 | 合肥国轩高科动力能源有限公司 | Method for pre-lithiating negative pole piece of lithium ion battery |
| US11984576B1 (en) | 2019-10-01 | 2024-05-14 | William Marsh Rice University | Alkali-metal anode with alloy coating applied by friction |
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