CN102487154A - Preparation method of multilayer electrolyte air cell - Google Patents
Preparation method of multilayer electrolyte air cell Download PDFInfo
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- CN102487154A CN102487154A CN2010105743750A CN201010574375A CN102487154A CN 102487154 A CN102487154 A CN 102487154A CN 2010105743750 A CN2010105743750 A CN 2010105743750A CN 201010574375 A CN201010574375 A CN 201010574375A CN 102487154 A CN102487154 A CN 102487154A
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Abstract
The invention relates to a preparation method of a multilayer electrolyte lithium air cell. The preparation method comprises the following steps: 1, preparing air electrodes; 2, cladding metallic lithium cathodes; and 3, putting the cladded metallic lithium cathodes and the air electrodes into a cell casing, adding an ionic liquid electrolyte to places to prepare the multilayer electrolyte lithium air cell, wherein each of the places is between one solid electrolyte membrane and one air electrode. The preparation method of the multilayer electrolyte lithium air cell, which adopts the transition electrolyte/solid electrolyte/ionic liquid electrolyte multilayer electrolyte to protect, allows the contact of the metallic lithium cathodes with water, carbon dioxide and oxygen to be prevented, so the metallic lithium cathodes are effectively protected; and the ionic liquid which has properties of incombustibility and non-volatility is used to replace an aqueous solution to improve the safety of the cell under destroy conditions. The cathode utilization rate and the internal resistance of the lithium air cell are not influenced under common air conditions, the long-term high efficiency working of the lithium air cell in air environment is realized, and the good safe reliability of the cell is guaranteed.
Description
Technical field
The invention belongs to the lithium-air battery technical field, particularly relate to a kind of preparation method of multilayer electrolyte lithium-air battery.
Background technology
Lithium-air battery be with lithium metal as negative pole, air electrode is anodal high-specific energy battery, it estimates that attainable specific energy is more than the 1000Wh/kg, is high-energy battery of new generation.
At present, can be divided into aqueous systems lithium-air battery and organic system (being non-aqueous system) lithium-air battery to the research of lithium-air battery according to the difference of employing electrolyte.For the organic system lithium-air battery, when battery was worked in air, airborne moisture and carbon dioxide can penetrate in the electrolyte; And then be penetrated into negative pole lithium metal surface side reaction takes place; Simultaneously, positive active material oxygen also can arrive lithium metal surface through the diffusion in electrolyte and reacts in the battery operated process, thereby has reduced the utilance of GND; Bring problems such as internal resistance increase simultaneously, can't realize the long-term efficient operation of battery; And the aqueous systems lithium-air battery is the multilayer electrolyte system that utilizes nonaqueous electrolytic solution/solid electrolyte/aqueous solution electrolysis liquid; But owing to adopted aqueous electrolyte; Brought hidden danger in air ambient, for the fail safe of battery; In case and to break appear in solid electrolyte at work, then the aqueous solution will directly contact with lithium metal, causes serious safety issue.Thereby two kinds of present system lithium-air batteries all are difficult to reach degree of being practical.
Summary of the invention
The objective of the invention is to overcome the weak point of prior art, a kind of preparation method of multilayer electrolyte lithium-air battery is provided, this battery can and have good fail safe in the medium-term and long-term efficient operation of normal air environment.
The preparation method of multilayer electrolyte lithium-air battery of the present invention adopts following technical scheme:
A kind of preparation method of multilayer electrolyte lithium-air battery comprises following preparation process:
(1) preparation air electrode: with the insulating properties porous film material as the air transfer layer; With mass percent is after ptfe emulsion, the 0%-50% manganese dioxide-catalyst of Delanium, the 5%-50% of 30%-90% mixes; Be coated in air transfer layer one side; Roll-in to thickness is the even lamella of 0.1mm-3mm being heated on 40 ℃-80 ℃ the roll squeezer repeatedly, prepares the air reaction layer; Aperture 10 orders-100 purpose aluminium net, titanium net or iron net are plus plate current-collecting body 1; Successively collector, air reaction layer and air transfer layer are put together from bottom to top; Be hot pressed into one with the hot press 10-1000Pa that exerts pressure, prepare lithium-air battery with air electrode 2;
(2) clad metal cathode of lithium: with solid film, liquid state organic electrolyte, ionic liquid; Colloidal state, all solid state organic bath are a kind of as transition electrolyte 5; Overlay on solid electrolyte 4 one sides; Form double layer electrolytic film, be wrapped in the transition electrolyte of double layer electrolytic film being pressed with lithium metal 7 negative poles of copper mesh as negative current collector 6;
(3) assembling of multilayer electrolyte lithium-air battery: the lithium metal that has double layer electrolytic film in (2) and (1) air electrode are put into battery container 8; Between solid electrolyte film and air electrode, add il electrolyte 3, promptly be prepared into the multilayer electrolyte lithium-air battery.
And said solid electrolyte film is between the thickness 50-5000 μ m, the NASICON glass ceramic film that ionic conductivity 10-4S/cm is above.
And said transition electrolyte is a kind of for directly being deposited in the surperficial LiPON lithium ion solid film of solid electrolyte film, liquid state organic electrolyte, ionic liquid, colloidal state, all solid state organic bath.
And, a kind of in the perchlorate that said il electrolyte electrolyte is imidazoles or piperidines, hexafluorophosphate, tetrafluoroborate, the trifluoromethyl sulfonic acid.
And, containing the organic solvent of electrolyte total content below 40% in the said il electrolyte electrolyte, said organic solvent is a kind of in monobutyl tri-methylimidazolium hexafluorophosphate, propene carbonate, ethylene carbonate and the butyrolactone.
And said air electrode is made up of plus plate current-collecting body, air reaction layer and the hot pressing of air transfer layer:
And said plus plate current-collecting body is aperture 10 orders-100 purpose aluminium net, titanium net or iron net.
And said negative current collector is a copper mesh.
Advantage that the present invention has and good effect:
The preparation method of multilayer electrolyte lithium-air battery of the present invention adopts the electrolytical multilayer electrolyte protection of transition electrolyte/solid electrolyte/il electrolyte; Prevented that moisture, carbon dioxide and oxygen from touching lithium anode; Effectively protected lithium anode; And ionic liquid has incombustibility and nonvolatile character, and its place of water solution has improved the fail safe of battery under failure condition.Guaranteed that lithium-air battery negative pole utilance and internal resistance under the normal air condition are unaffected, realized the long-term efficient operation of lithium-air battery in air ambient, guaranteed that again battery has good security reliability.
Description of drawings
Fig. 1 is preparation method's sectional structure sketch map of multilayer electrolyte lithium-air battery of the present invention;
Fig. 2 is that the present invention uses back lithium metal surface topography map for a long time;
Fig. 3 is that common lithium-air battery uses back lithium metal surface topography map for a long time.
Wherein, 1-plus plate current-collecting body, 2-air electrode, 3-il electrolyte electrolyte, 4-solid electrolyte, 5-transition electrolyte, 6-negative current collector, 7-lithium metal, 8-battery container.
Embodiment
Below in conjunction with accompanying drawing and through specific embodiment the present invention is made further detailed description, following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
A kind of preparation method of multilayer electrolyte lithium-air battery comprises battery container 8, is positioned at the anodal of battery container inwall and is positioned at the negative pole at housing center; The said air electrode 2 that just very is welded with plus plate current-collecting body 1; Said negative pole is the lithium metal 7 that has negative current collector 6, and solid electrolyte 4 is arranged between air electrode and the lithium metal.
Innovative point of the present invention is:
Lithium metal and solid electrolyte film have transition electrolyte 5, and il electrolyte electrolyte 3 is arranged between air electrode and the solid electrolyte film.
Embodiment 1: with reference to accompanying drawing 1.
According to document (Solid State Ionics; 171 (2004): the method that 207-213.) adopts prepares the NASICON solid electrolyte film, this material is carried out high-temperature fusion, quenching moulding, controlled micro crystallization, machine finishing make the glass ceramics dielectric film that the about 130 μ m of thickness, ionic conductivity reach the densification more than the 10-4S/cm.
Air electrode of the present invention is the air electrode that one constitutes by collector, air reaction layer and the hot pressing of air transfer layer, and collector is aperture 20 purpose titanium nets; The air reaction layer is that hot-rolling was pressed into the even lamella of 50 μ m after 40% Delanium, 20% ptfe emulsion and 40% manganese dioxide-catalyst mixed; The air transfer layer is the glass fibre membrane of 20 μ m.
Consider that redox reaction slowly can take place for lithium metal and NASICON solid electrolyte material; Therefore need between to add to the stable transition electrolyte of lithium metal; Preventing that lithium metal from directly contacting with solid electrolyte film, and can realize the transmission of lithium ion.This layer transition electrolyte can be the LiPON lithium ion thin film electrolyte of solid film, also can be liquid state organic electrolyte, ionic liquid, or colloidal state, all solid state organic bath.If adopt LiPON film electrolyte can directly deposit the double layer electrolytic film that the surface that is prepared in the glass ceramics dielectric film is integrally formed as the transition electrolyte; Lithium anode is pressed on the copper mesh, with the lithium metal adhering and sealing in the LiPON of above-mentioned double layer electrolytic film film.
Above-mentioned lithium metal and the air electrode that has double layer electrolytic film put into battery case; Between solid electrolyte film and air electrode, add electrolytic salt 0.5mol/L LiClO4; Solvent be monobutyl tri-methylimidazolium hexafluorophosphate as il electrolyte, formed the preparation method of the multilayer electrolyte lithium-air battery of transition electrolyte/solid electrolyte/compound formation of il electrolyte electrolyte.
The il electrolyte used among the present invention requires that the air electrode of lithium-air battery is had electrochemical stability, and these ionic liquids are stable in the air simultaneously, can not decompose, reaction such as oxidation.The ionic liquid kind that satisfies this condition is more, and like the perchlorate of imidazoles or piperidines, hexafluorophosphate, tetrafluoroborate, trifluoromethyl sulfonic acid etc., common having among BMImClO4, BMImPF6, BMImBF4, EMImPF6, the EMImBF4 is a kind of.
The present invention can also add the ionic liquid total amount below 40% in the il electrolyte of using; Boiling point more than 100 ℃, not volatile; The organic electrolyte of the propene carbonate that can use for a long time, ethylene carbonate and butyrolactone; This can reduce ion electrolysis fluid viscosity, improves the wettability between il electrolyte and the air electrode, improves the air electrode discharge performance.The ratio of organic solvent that control simultaneously adds still can keep the incombustibility of electrolyte.
With the preparation method of multilayer electrolyte lithium-air battery of the present invention and common employing il electrolyte and there is not the lithium-air battery of solid electrolyte to be positioned in the air simultaneously; And with the current discharge of 0.1mA/cm2 after 24 hours separately lithium electrode take out; And with the residual transition electrolyte of DMC clean surface; Compare the lithium metal surface appearance; Result the present invention as shown in Figure 2 uses back lithium metal surface topography map for a long time and shown in Figure 3 (common lithium-air battery uses back lithium metal surface topography map for a long time; Obviously the preparation method's of the multilayer electrolyte lithium-air battery of employing transition electrolyte/solid electrolyte of the present invention/compound formation of il electrolyte electrolyte lithium electrode has the surface of good situation; And the lithium electrode in the lithium-air battery of employing conventional ion liquid electrolyte has partly turned black, and this will influence the serviceability of lithium electrode.
The preparation method of above-mentioned multilayer electrolyte lithium-air battery and the lithium-air battery of conventional aqueous systems electrolyte are punctured from the front with iron nail respectively, observe the phenomenon when destroying.The result is as shown in table 1.
Security test result when table 1 different lithium air cell punctures
Obviously; Adopt the preparation method of invention multilayer electrolyte lithium-air battery to compare with the lithium-air battery of solid electrolyte/aqueous electrolyte structure; Demonstrated good battery security, violent side reaction did not take place in lithium metal and ionic liquid joint yet when solid electrolyte film was damaged even this is.This brings great improvement to battery security.
Operation principle: because the existence of the solid electrolyte in the multilayer electrolyte structure; Can prevent moisture, carbon dioxide; And oxygen reaches the metal lithium electrode surface through the diffusion in liquid electrolyte and reacts, thereby realizes the effectively purpose of protection metal lithium electrode.And the ionic liquid electrolyte in the multilayer electrolyte structure can guarantee the fail safe of battery.Il electrolyte has incombustibility and nonvolatile character, simultaneously between it and the lithium metal violent, uncontrollable reaction can not take place yet, thereby guarantee the fail safe of battery.By contrast; Common organic electrolyte (like electrolyte of lipid or ethers etc.) has tangible combustibility and effumability; And vigorous reaction can take place in aqueous systems electrolyte when contacting with lithium metal; So adopt common organic electrolyte or aqueous systems electrolyte under special circumstances, meet high temperature or structural deterioration when causing lithium metal to contact like battery with electrolyte, all can cause the dangerous of battery.
Claims (8)
1. the preparation method of a multilayer electrolyte lithium-air battery is characterized in that: comprise following preparation process:
(1) preparation air electrode: with the insulating properties porous film material as the air transfer layer; With mass percent is after ptfe emulsion, the 0%-50% manganese dioxide-catalyst of Delanium, the 5%-50% of 30%-90% mixes; Be coated in air transfer layer one side; Roll-in to thickness is the even lamella of 0.1mm-3mm being heated on 40 ℃-80 ℃ the roll squeezer repeatedly, prepares the air reaction layer; Aperture 10 orders-100 purpose aluminium net, titanium net or iron net are collector, successively collector, air reaction layer and air transfer layer are put together from bottom to top, are hot pressed into one with the hot press 10-1000Pa that exerts pressure, and prepare lithium-air battery and use air electrode;
(2) clad metal cathode of lithium: with solid film, liquid state organic electrolyte, ionic liquid; Colloidal state, all solid state organic bath are a kind of as the transition electrolyte; Overlay on the solid electrolyte film one side; Form double layer electrolytic film, the lithium anode that is pressed with copper mesh is wrapped in the transition electrolyte of double layer electrolytic film;
(3) assembling of multilayer electrolyte lithium-air battery: the lithium metal that has double layer electrolytic film in (2) and (1) air electrode are put into battery container; Between solid electrolyte film and air electrode, add il electrolyte, promptly be prepared into the multilayer electrolyte lithium-air battery.
2. the preparation method of multilayer electrolyte lithium-air battery according to claim 1; It is characterized in that: the preparation method of multilayer electrolyte lithium-air battery according to claim 1; It is characterized in that: said solid electrolyte film is between the thickness 50-5000 μ m, the NASICON glass ceramic film that ionic conductivity 10-4S/cm is above.
3. the preparation method of multilayer electrolyte lithium-air battery according to claim 1 is characterized in that: said transition electrolyte is a kind of for directly being deposited in the surperficial LiPON lithium ion solid film of solid electrolyte film, liquid state organic electrolyte, ionic liquid, colloidal state, all solid state organic bath.
4. the preparation method of multilayer electrolyte lithium-air battery according to claim 1 is characterized in that: a kind of in the perchlorate that said il electrolyte electrolyte is imidazoles or piperidines, hexafluorophosphate, tetrafluoroborate, the trifluoromethyl sulfonic acid.
5. according to the preparation method of claim 1 or 4 described multilayer electrolyte lithium-air batteries; It is characterized in that: contain the organic solvent of electrolyte total content below 40% in the said il electrolyte electrolyte, said organic solvent is a kind of in monobutyl tri-methylimidazolium hexafluorophosphate, propene carbonate, ethylene carbonate and the butyrolactone.
6. the preparation method of multilayer electrolyte lithium-air battery according to claim 1 is characterized in that: said air electrode is made up of plus plate current-collecting body, air reaction layer and the hot pressing of air transfer layer:
7. according to the preparation method of claim 1 or 6 described multilayer electrolyte lithium-air batteries, it is characterized in that: said plus plate current-collecting body is aperture 10 orders-100 purpose aluminium net, titanium net or iron net.
8. the preparation method of multilayer electrolyte lithium-air battery according to claim 1 is characterized in that: said negative current collector is a copper mesh.
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| CN2010105743750A CN102487154A (en) | 2010-12-06 | 2010-12-06 | Preparation method of multilayer electrolyte air cell |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103326034A (en) * | 2013-06-14 | 2013-09-25 | 武汉理工大学 | Air electrode of lithium air battery and preparation method thereof |
| CN105514491A (en) * | 2015-12-29 | 2016-04-20 | 湖州创亚动力电池材料有限公司 | Preparation of all-solid-state inorganic solid lithium ion electrolyte |
| CN105655632A (en) * | 2016-03-17 | 2016-06-08 | 湖北知本信息科技有限公司 | Method for preparing lithium-air battery and prepared lithium-air battery |
| CN105789682A (en) * | 2014-12-17 | 2016-07-20 | 中国电子科技集团公司第十八研究所 | Preparation method of safe high-rate and all-solid-state battery |
| CN106328955A (en) * | 2015-06-25 | 2017-01-11 | 清华大学 | Lithium air battery positive electrode and lithium air battery |
| CN106463803A (en) * | 2014-05-15 | 2017-02-22 | 宝马股份公司 | Lithium-air battery |
| CN111602217A (en) * | 2017-11-22 | 2020-08-28 | 罗伯特·博世有限公司 | Capacitor with a capacitor element |
| CN114975889A (en) * | 2021-02-19 | 2022-08-30 | 通用汽车环球科技运作有限责任公司 | Method for manufacturing anode of lithium battery cell |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103326034A (en) * | 2013-06-14 | 2013-09-25 | 武汉理工大学 | Air electrode of lithium air battery and preparation method thereof |
| CN103326034B (en) * | 2013-06-14 | 2016-01-06 | 武汉理工大学 | A kind of air electrode of lithium air battery and preparation method thereof |
| CN106463803A (en) * | 2014-05-15 | 2017-02-22 | 宝马股份公司 | Lithium-air battery |
| US10693204B2 (en) | 2014-05-15 | 2020-06-23 | Bayerische Motoren Werke Aktiengesellschaft | Lithium-air battery |
| CN105789682A (en) * | 2014-12-17 | 2016-07-20 | 中国电子科技集团公司第十八研究所 | Preparation method of safe high-rate and all-solid-state battery |
| CN106328955A (en) * | 2015-06-25 | 2017-01-11 | 清华大学 | Lithium air battery positive electrode and lithium air battery |
| CN106328955B (en) * | 2015-06-25 | 2019-02-12 | 清华大学 | Lithium air battery positive electrode and lithium-air battery |
| CN105514491A (en) * | 2015-12-29 | 2016-04-20 | 湖州创亚动力电池材料有限公司 | Preparation of all-solid-state inorganic solid lithium ion electrolyte |
| CN105514491B (en) * | 2015-12-29 | 2018-06-26 | 湖州创亚动力电池材料有限公司 | A kind of preparation of all solid state inoganic solids lithium-ion electrolyte |
| CN105655632A (en) * | 2016-03-17 | 2016-06-08 | 湖北知本信息科技有限公司 | Method for preparing lithium-air battery and prepared lithium-air battery |
| CN111602217A (en) * | 2017-11-22 | 2020-08-28 | 罗伯特·博世有限公司 | Capacitor with a capacitor element |
| CN114975889A (en) * | 2021-02-19 | 2022-08-30 | 通用汽车环球科技运作有限责任公司 | Method for manufacturing anode of lithium battery cell |
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Application publication date: 20120606 |