CN101267057A - High ratio energy chargeable full-solid lithium air battery - Google Patents
High ratio energy chargeable full-solid lithium air battery Download PDFInfo
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Abstract
The present invention belongs to electrochemical technical field, specifically a high specific energy charging full-solid lithium air battery. The battery structure is: firstly an air diffusion layer, then an air electrode, composed of a meso-porous carbon/manganese oxide composite material, an oxygen-reduction catalyst and a macromolecule lithium electrolyte, next a multilayer aqueous vapour cover, not only serving as a electrolyte layer of the battery, but also blocking water an oxidation entering of the air, finally a metal lithium. The whole battery is sealed in the multiplayer metal/plastic, a portable sealing is on the top of the air diffusion layer which is opened when the battery is used, closed when the battery is not used. The invention adopts lithium air battery made by the meso-porous carbon / manganese oxide composite material and the room temperature ionic liquid electrolyte, the capacity achieves 800mAh/g, cycling more than 50 times. In the lithium air battery, the metal lithium has effective protection, making the Li/O<SUB>2</SUB> reaction only in the electrochemical reaction, the lithium air battery not only has battery electrochemical capability, but also has excellent safety ability.
Description
Technical field
The invention belongs to technical field of electrochemistry, be specifically related to a kind of lithium-air battery, more particularly, relate to a kind of high ratio energy chargeable formula lithium-air battery.
Background technology
Along with constant development of economy, must cause the aggravation of the exhaustion of petroleum resources and environmental pollution, greenhouse effects of the earth.Human necessary economic growth (Economic Growth), the equilibrium relation between " three E " of environmental protection (Environmental Protection) and energy resource supply (Energy Security) held.New forms of energy are economized energy technology, and the development and utilization that reaches the comprehensive high-efficiency rate of Environmental Technology has become very necessary problem, and the power supply system and the material of research and development high-energy-density are imperative.
In recent ten years, dominated the development of heavy-duty battery based on the battery of lithium metal, this is that lithium metal has minimum density because in all cell negative electrode materials, the highest voltage, best electronic conductance and the highest electrochemical equivalent.Actively developed in the global range and improved the energy density of lithium battery and the Study on Stability of electrode material.LiCoO
2With material with carbon element as the successful commercialization of the positive and negative pole material of lithium ion, LiFePO
4Be the up-and-coming youngster of positive electrode.Because the influencing factor of aspects such as price, fail safe, specific energy is sought the direction that higher, the more cheap positive electrode of specific energy is the lithium battery development always.But positive electrode has limited to the energy storage performance of lithium battery in the lithium battery.Such as, the electrochemistry capacitance of lithium metal is 3860mAh/g, but the electrochemistry capacitance of most of positive electrode has only 200mAh/g, and in addition, lithium ion is lower at the diffusion coefficient of metal positive-pole material, has also limited the energy output of lithium battery.
On the other hand, metal/oxygen (air) battery provides high electrochemical performance.Because in these batteries, be not stored in the battery as the oxygen (air) of positive pole.Aerial oxygen can become negative oxygen ion or crosses negative oxygen ion and then generate metal oxide or peroxide by electrochemical reaction by catalyst.Be different from conventional aluminum-air cell, the aqueous electrolyte cell system of zinc-air cell, lithium-air battery is a kind of brand-new metal-air cell, uses organic series electrolyte or all solid state electrolyte.The operation principle of lithium-air battery is based on following two reaction: 4Li+O
2→ 2Li
2O; Li+O
2→ Li
2O
2Calculate by first reaction, battery open circuit voltage is 2.91V, and theoretical energy density is 5200Wh/kg.In actual applications, oxygen is provided by external environment, and the energy density of therefore getting rid of behind the oxygen reaches surprising 11140Wh/kg, and height has a battery system 1-2 order of magnitude.
But, if with air as positive pole, lithium metal can react rapidly with the moisture that exists in the air, causes lithium metal to be corroded.Like this, in the use, battery safety is a big hidden danger.Yet huge energy density has determined lithium-air battery to be widely used in aviation and mobile energy field.If can successfully solve design of safety and etching problem and associated materials thereof and preparation problem, lithium-air battery will be the once great revolution on the energy history.
The research of metal/oxygen (air) battery is at the early-stage, and relevant report seldom.The science group of whole world research lithium-air battery mainly contains three, is respectively the founder K.M.Abraham of lithium-air battery, the P.G.Bruce of breadboard J.Read of u.s.a. military affairs and Britain.Their research mainly concentrates on the working mechanism of battery, and electrolyte is to the influence of battery performance.
It is electrolytical lithium-air battery that the article that K.M.Abraham reports lithium-air battery has first been introduced with gelatin polymer (PAN-PVDF), this battery open circuit voltage is near 3V, operating voltage is between 2.0-2.8V, with the catalyst of phthalocyanine cobalt, has good coulombic efficiency and three circles that can circulate as air electrode.The author thinks that discharge mechanism is that lithium ion and oxygen generate lithium peroxide on the carbon back air electrode.
J.Read is at the lithium-air battery discharge mechanism, and electrode material and electrolyte composition are done a lot of work.The maximum difference of lithium-air battery and water system metal-air cell is that its discharging product is to be deposited on negative electrode rather than anode.Because lithium peroxide and lithia all are not dissolved in the organic electrolyte, so discharging product can only have O2
2-And O
2-Air electrode on deposit.Under the excessive situation of anode, the termination of discharge is because discharging product is stopped up due to the air electrode duct.J.Read has studied air electrode material in great detail, electrolyte is formed, partial pressure of oxygen, the oxygen solvability is to discharge capacity, high rate performance and circulative influence, think that the electrolyte composition has very big influence to battery performance and the behavior of discharging product deposition, and propose with the electrolyte of ether solvent as lithium-air battery.
People such as the Kuboki of Toshiba report hydrolysis when the lithium ion liquid with waterproof can prevent that lithium metal from contacting with steam in nearest report, can prolong the life-span of lithium-air battery like this.Different with common liquid lithium electrolyte, the vapour pressure of ionic liquid electrolyte can be ignored, so can use in the open environment of gentleness.
P.G.Bruce makes major contribution in the research of lithium-air battery charging mechanism, result of study is thought and reacted 2Li
++ 2e
-+ O
2→ Li
2O
2Be reversible reaction, show that battery has the property of charging and discharging when discharging product is lithium peroxide, realized 50 circulations, capacity is 600mAh/g.P.G.Bruce makes major contribution in the research of lithium-air battery charging mechanism, result of study is thought and reacted 2Li
++ 2e
-+ O
2→ Li
2O
2Be reversible reaction, show that battery has the property of charging and discharging when discharging product is lithium peroxide, realized 50 circulations, capacity is 600mAh/g.
The patent application of lithium-air battery also seldom, K.M.Abraham had once reported the lithium-oxygen battery system (patent No.: US 5561004) based on the PAN-PVDF system, and other patent then includes only a few things aspect ionic liquid (US4804448) and positive electrode (US 71477967) such as Eltron company.
Summary of the invention
The objective of the invention is to propose that a kind of chemical property is good, the full-solid lithium air battery of security performance advantage.
The present invention proposes the full-solid lithium air battery notion first, and has proved its feasibility.By this notion, adopt mesoporous carbon/manganese oxide composite material and normal temperature ionic liquid electrolyte etc., prepared small-sized lithium-air battery, and driven electronic clock with it.Here, design studies gets mesoporous carbon/manganese oxide composite material voluntarily, provides good gas-liquid-solid three-phase structure to the electro-catalysis of oxygen, and its catalysis characteristics is higher than carbon nano tube compound material far away.
Adopt the lithium-air battery of preparations such as mesoporous carbon/manganese oxide composite material and normal temperature ionic liquid electrolyte, its capacity reaches 800mAh/g, and is capable of circulation more than 50 times.
In this lithium-air battery, lithium metal is effectively protected, and makes Li/O
2Reaction is only carried out in electrochemical reaction, thereby makes lithium-air battery except having extraordinary chemical property, also has the excellent safety energy.
The high ratio energy chargeable formula lithium-air battery that the present invention proposes, constitute by packaging material film phonograph seal packing by air electrode, lithium anode, the multilayer flashing solid-state electrolyte layer between air electrode and cathode of lithium film, the air diffusion layer that links with air electrode, the multiple layer metal/polymer film of sealing metal cathode of lithium, wherein:
Air diffusion layer is made up of how empty metal aluminum foil, simultaneously also as the positive electrode collector conjuncted part of positive outside wire of holding concurrently;
Air electrode is made up of carbon black, oxygen catalyst and macromolecule lithium electrolyte;
The waterproof solid electrolyte adopts the high molecular hybrid films of the ultra-thin LIPON/ of multilayer, guarantees that electrolyte layer has certain toughness and can protect lithium metal effectively;
Lithium anode is made on electrolyte layer by the lithium metal evaporation; Evaporation has Parylene PARYLENE on the lithium anode, as protective layer;
What be used for the entire cell encapsulation is macromolecule and metallic multilayer packaging material.
Cell making process of the present invention is as follows:
(1) cleaning of porous aluminum foil substrate
Substrate is cleaned with acetone, clean 3-5 time with distilled water then, oven dry;
(2) making of positive outside wire
Welding one nickel sheet is made positive outside wire in substrate;
(3) making of air positive pole
Cobalt-containing catalyst becomes O as oxicracking
2-Or O
2 2-Catalyst, mesoporous carbon/manganese oxide composite material and catalyst mix is even, and roasting at high temperature mixes with PEO type macromolecule lithium electrolyte then,, smears (Spin Coating) back in substrate with rotation then and dries as TDS with ethene cyanogen;
(4) making of solid electrolyte
In blanket of nitrogen, LiPON inorganic electrolyte liquid is by radio frequency sputtering Li
3PO
4Target is deposited on the air anode thin film, thickness 0.1-0.2 micron, and the similar thickness Parylene of evaporation macromolecule paryline material repeats to deposit operation 3-4 time of Lipon inorganic electrolyte liquid and evaporation Parylene, and gross thickness is the 1-2 micron;
(5) making of negative pole
10
-3-10
-5Under the vacuum degree of Pa, in argon gas atmosphere, vacuum vapour deposition heating lithium source, on the LiPON dielectric substrate plated metal lithium thin layer as negative pole,
(6) interpolation of negative electrode collector
By welding or metal-sol metal levels such as metallic nickel are connected with negative pole,
(7) composite multilayer membrane of package metals/macromolecular material is aluminium/polyethylene multilayer compound or aluminium/polypropylene multi-layer compound.
The present invention proposes the full-solid lithium air battery notion,, adopt mesoporous carbon/manganese oxide composite material and normal temperature ionic liquid electrolyte etc. by this notion, prepared small-sized lithium-air battery, and driving electronic clock with it, its capacity reaches 800mAh/g, and is capable of circulation more than 50 times.In this lithium-air battery, lithium metal is effectively protected, Li/O
2Reaction is only carried out in electrochemical reaction, thereby makes this lithium-air battery except having extraordinary chemical property, also has the excellent safety energy.
Description of drawings
Fig. 1 is a lithium-air battery structural diagrams of the present invention.
Fig. 2 is lithium-air battery cycle performance figure of the present invention.
Fig. 3 charges and discharge performance map for lithium-air battery of the present invention.
Number in the figure: 1, just formula air duct seal cover, 2, multiple layer metal/plastic casing, 3, cathode current aluminium foil collector electrode, 4, the cathode terminal end, 5, carbon/polyelectrolyte air electrode, 6, polymer dielectric transition zone, 7, LiPON electrolyte aqueous vapor barrier layer, 8, lithium metal anode, 9, anode lead wire end, 10, lithium organic passivation layer, 11, the polymer encapsulated layer, 12, multiple layer metal/composite membrane of polymer.
Embodiment
Below, with reference to accompanying drawing, specify the present invention for embodiment.
Fig. 1 is the structural diagrams of lithium-air battery, and battery is by air electrode, multilayer flashing solid-state electrolytic solution, the composition of lithium anode.It at first is air diffusion layer; be air electrode then; next be multilayer aqueous vapor protective layer; it promptly serves as the dielectric substrate of battery, and moisture in the blocks air and oxygen enter and chemical reaction takes place again, and the lithium metal layer is made negative pole then; the entire cell sealing encapsulates with multiple layer metal/composite plastic film; have once formula in the air diffusion layer front on encapsulating film and seal, open when battery uses, the time spent does not close.In air electrode, soak into hydrophobic type lithium ion liquid.
Specific implementation method: the lithium electrode protection of multilayer electrolyte: fine and close LIPON layer is proved to be able to stop effectively the infiltration of water and air, and still, as surpassing certain thickness, film will produce slight crack.Here, we adopt vacuum sputtering and the high molecular hybrid multilayer film of the ultra-thin LIPON/ of vacuum evaporation, guarantee that electrolyte layer has certain toughness and can protect lithium metal effectively; Adopt a series of electrode materials that possess special shape (tubulose, sheet and flakes etc.) and structure (mesoporous with micropore etc.) such as the synthetic metal oxide with high electrocatalytic active of water under high pressure thermal synthesis method, electrochemical deposition, template and methods such as in-situ chemical or electrochemical polymerization, nanocarbon/metal oxide; By the auxiliary method such as synthetic of microwave, ultrasonic and electrochemistry, synthetic prepared have macroion conductivity and thermal stability, the novel ion liquid electrolyte of wide electrochemical window; With the even dispersion technology of nano material in conductive auxiliary agent, good electrode coating process, high hydrophobic, high gaseous diffusion, low-resistance electrode have been prepared; Optimize hydrophobic layer, diffusion layer in the air electrode material and urge the The Nomenclature Composition and Structure of Complexes of layer, improve specific energy, power density and the cycle life of battery greatly.
Described kind of high ratio energy chargeable formula lithium-air battery entity by the multiple layer metal/polymer film of air electrode, lithium anode, the multilayer flashing solid state electrolysis liquid layer between air electrode, negative film, the air diffuser tunic that links with air electrode, sealing metal lithium with and the packaging material film pack and constitute, wherein:
Air diffusion layer is made up of the porous aluminium foil, simultaneously also is the positive electrode collector conjuncted part of positive outside wire of holding concurrently;
Air electrode is by carbon black, and oxygen catalyst and macromolecule lithium electrolyte are formed;
The waterproof solid-state electrolytic solution adopts the high molecular hybrid films of the ultra-thin LIPON/ of multilayer, guarantees that electrolyte layer has certain toughness and can protect lithium metal effectively;
Negative pole is made in the lithium metal evaporation on electrolyte layer; Again Parylene PARYLENE evaporation is protected on lithium metal;
What be used for the entire cell encapsulation is macromolecule and metallic multilayer packaging material.
Specifically cell making process is,
(1) cleaning of porous aluminum foil substrate
Substrate is cleaned with acetone, clean 3-5 time with distilled water then, oven dry;
(2) making of positive outside wire
Welding one nickel sheet is made positive outside wire in substrate;
(3) making of air positive pole
Cobalt-containing catalyst becomes O as oxicracking
2-Or O
2 2-Catalyst, mesoporous carbon/manganese oxide composite material and catalyst mix is even, and roasting at high temperature mixes with PEO type macromolecule lithium electrolyte then,, smears (Spin Coating) back in substrate with rotation then and dries as TDS with ethene cyanogen;
(4) making of solid electrolyte
In blanket of nitrogen, LiPON inorganic electrolyte liquid is by radio frequency sputtering Li
3PO
4Target is deposited on the air anode thin film, thickness 0.1-0.2 micron, and the similar thickness Parylene of evaporation macromolecule paryline material repeats to deposit operation 3-4 time of Lipon inorganic electrolyte liquid and evaporation Parylene, and gross thickness is the 1-2 micron;
(5) making of negative pole
10
-310
-5Under the vacuum degree of Pa, in argon gas atmosphere, vacuum vapour deposition heating lithium source, on the LiPON dielectric substrate plated metal lithium thin layer as negative pole,
(6) interpolation of negative electrode collector
By welding or metal-sol metal levels such as metallic nickel are connected with negative pole,
(7) composite multilayer membrane of package metals/macromolecular material is aluminium/polyethylene multilayer compound or aluminium/polypropylene multi-layer compound.
Claims (2)
1, a kind of high ratio energy chargeable formula lithium-air battery, it is characterized in that multiple layer metal/polymer film by air electrode, lithium anode, the multilayer flashing solid-state electrolyte layer between air electrode and lithium anode film, the air diffuser tunic that links with air electrode, sealing metal lithium is packed by the packaging material film constitutes, wherein:
Described air diffusion layer is made up of the porous aluminium foil, simultaneously also as the positive electrode collector conjuncted part of positive outside wire of holding concurrently;
Air electrode is by mesoporous carbon/manganese oxide composite material, and oxygen catalyst and macromolecule lithium electrolyte are formed;
The waterproof solid electrolyte adopts the high molecular hybrid films of the ultra-thin LIPON/ of multilayer;
Lithium anode is made on electrolyte layer by the lithium metal evaporation; Evaporation has Parylene PARYLENE as protective layer on the lithium anode.
2. the preparation method of battery as claimed in claim 1 is characterized in that concrete steps are as follows:
(1) cleaning of porous aluminum foil substrate
Substrate is cleaned with acetone, clean 3-5 time with distilled water then, oven dry;
(2) making of positive outside wire
Welding one nickel sheet is made positive outside wire in substrate;
(3) making of air electrode
Cobalt-containing catalyst becomes O as oxicracking
2-Or O
2 2-Catalyst, mesoporous carbon/manganese oxide composite material and catalyst mix is even, and roasting at high temperature mixes with PEO type macromolecule lithium electrolyte then,, spreads upon in the substrate back with rotation then and dries as TDS with ethene cyanogen;
(4) making of solid electrolyte
In blanket of nitrogen, LiPON inorganic electrolyte liquid is by radio frequency sputtering Li
3PO
4Target is deposited on the air anode thin film, thickness 0.1-0.2 micron, and the similar thickness Parylene of evaporation macromolecule paryline material repeats to deposit operation 3-4 time of Lipon inorganic electrolyte liquid and evaporation Parylene, and gross thickness is the 1-2 micron;
(5) making of negative pole
10
-3-10
-5Under the vacuum degree of Pa, in argon gas atmosphere, vacuum vapour deposition heating lithium source, plated metal lithium thin layer is as negative pole on the LiPON dielectric substrate;
(6) interpolation of negative electrode collector
By welding or metal-sol metal levels such as metallic nickel are connected with negative pole;
(7) composite multilayer membrane of package metals/macromolecular material is aluminium/polyethylene multilayer compound or aluminium/polypropylene multi-layer compound.
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| CN101533935A (en) * | 2009-04-14 | 2009-09-16 | 黄穗阳 | A high-energy safe rechargeable lithium-oxygen battery |
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