CN104091966A - Aluminum-containing electrolyte and secondary aluminium battery using same - Google Patents
Aluminum-containing electrolyte and secondary aluminium battery using same Download PDFInfo
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- CN104091966A CN104091966A CN201410320601.0A CN201410320601A CN104091966A CN 104091966 A CN104091966 A CN 104091966A CN 201410320601 A CN201410320601 A CN 201410320601A CN 104091966 A CN104091966 A CN 104091966A
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
- C07D233/56—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms
- C07D233/58—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring nitrogen atoms
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01M10/0566—Liquid materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/46—Alloys based on magnesium or aluminium
- H01M4/463—Aluminium based
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a novel secondary aluminium battery which comprises a positive electrode, a negative electrode and electrolyte, wherein an active material of the negative electrode is metallic aluminium or aluminium alloy; an active material of the positive electrode is elemental sulfur or organic sulfide; the electrolyte is halogenated aluminate ionic liquid which is formed by halogenated aluminate and N-alkyl imidazole hydrochloride.
Description
Technical field
The invention belongs to electrochemistry and new energy field, relate to a kind of secondary aluminium cell, especially relate to a kind of secondary aluminium-sulfur battery that uses halogen aluminic acid ionic liquid electrolyte.
Background technology
Aluminum secondary battery is the chemical power source of new generation after lead-acid battery, nickel-cadmium cell, Ni-MH battery and lithium secondary battery.Aluminum secondary battery system, compared with other secondary cells, has that energy is larger, cost is lower, weight is lighter, volume is less, a more environmental protection, safer stable, more high of cost performance, is the renewable new forms of energy that can recycle sustainable development.Metallic aluminium cheapness, be easy to get, easily reclaim, and aluminium is the richest metallic element of content on the earth, exploits, develops, processes, utilizes cost very low; The specific energy of aluminium is very high, and theoretical electrochemistry specific capacity reaches 2980mAh/g, is only second to lithium in metallic element; The volume and capacity ratio of aluminium is 8050 mAh/cm
3, higher than present all cell negative electrode materials, be desirable negative material.Elementary sulfur also has larger theoretical energy density (1670mAh/g), is the positive electrode of known energy density maximum.Therefore, aluminium-sulfur battery be all from every side a kind of cheap, energy density is high, use safe ideal battery.
Although the theoretical energy density of aluminium-air cell can reach 8100Wh/Kg, actual energy density only has 350Wh/kg.This is because a lot of problems that aluminium electrode can produce in aqueous electrolyte: between (1) aluminium alloy and oxygen, have very strong affinity, in air and the aqueous solution, the passive oxidation film of Surface Creation one deck densification, make the electrode potential of aluminium in neutral solution not reach due theoretical electrode potential, the real work current potential of aluminium is more much lower than theoretical value, the voltage delay phenomenon while simultaneously also causing electric discharge.(2) aluminium is typical amphoteric metal, and activity is higher, easily with acid, alkali effect, oxide-film is destroyed, once and oxide-film is destroyed will be corroded rapidly, make the utilance of electrode low, and wet poor storage performance.(3) aluminium is larger from corrosion in alkaline solution, and serious evolving hydrogen reaction occurs easy and medium, has reduced the utilance of electrode, affects the normal work of battery.(4), in alkaline medium, aluminium anodes becomes stream reaction and corrosion reaction product to be gluey Al (OH)
3, not only reduce electrolytic conductivity but also increase aluminium anodes polarization, aluminum cell performance is worsened.(5) need heat-exchange system to get rid of the dissolving of aluminium in alkaline solution and a large amount of heat of corrosion generation.Therefore, want to realize the chargeable of aluminium-sulfur battery, what first need solution is exactly electro-deposition-stripping problem of the aluminium in electrolyte.Electrolytical selection is determining the working mechanism of secondary aluminium cell to a great extent, affects specific energy, cycle performance, rate charge-discharge performance, fail safe, storge quality and the cost etc. of battery.Selecting suitable electrolyte is the important prerequisite that realizes secondary cell high-performance, long-life, fail safe and low cost.。
Summary of the invention
(1) goal of the invention
The object of the present invention is to provide a kind of halogen aluminic acid ionic liquid electrolyte, to realize the electrochemical deposition-stripping of aluminium.
The present invention also aims to provide a kind of secondary aluminium cell that uses this electrolyte.
Term " two aluminium primary cells " in the present invention for example comprises " aluminum secondary battery ", " rechargeable aluminium battery ", " aluminium storage battery ", " aluminium energy-storage battery " and similar concept.
(2) technical scheme
To achieve these goals, the invention provides a kind of secondary aluminium cell scheme, comprising:
(a) electrolyte, wherein said electrolyte is N-alkyl imidazole hydrochloride-aluminum halide ionic liquid;
(b) positive pole that comprises electro-chemical activity sulphur-containing substance;
(c) negative pole containing aluminium active material;
The preferred negative pole of electrochemical cell of the present invention, positive pole, electrolytical description below.
Anodal
The positive pole of battery of the present invention comprises the positive active material, conductive agent, binding agent and the collector that contain electro-chemical activity sulphur-containing substance.Wherein, term " electro-chemical activity sulphur-containing substance " refers to the positive active material that comprises element sulphur here, and wherein, electro-chemical activity relates to fracture or the formation of sulphur-sulphur covalent bond.
Electro-chemical activity sulphur-containing substance described in scheme, includes but not limited to elementary sulfur and the organosulfur compound that comprises sulphur atom and carbon atom, and they can be polymerizations or non-polymeric.Organosulfur compound comprises Polyacetylene sulfide, carbyne polysulfide, many sulfo-s polystyrene, vulcanized polyvinyl chloride, Phenyl polysulfide, sulfurized polyacrylonitrile, many sulfo-s naphthalene, Phenyl polysulfide amine, many sulfo-s pyridine, many sulfo-s thiophene, many sulfo-s pyrroles, many thio-furans etc.
Conductive agent described in scheme includes but not limited to graphite-based material, carbon-based material and conducting polymer.Graphite-based material comprises electrically conductive graphite KS6, and carbon-based material comprises that Super P, Ketjen are black, acetylene black or carbon black.Conducting polymer comprises polyaniline, polypyrrole, polythiophene, polyacetylene, or their mixture.
Adhesive described in scheme is polyvinyl alcohol (PVA), polytetrafluoroethylene (PTFE), sodium carboxymethylcellulose (CMC), Kynoar (PVDF), polystyrene butadiene copolymer (SBR), Viton and polyurethane, PVP, polyethyl acrylate, polyvinyl chloride, polyacrylonitrile, polycaprolactam, polybutadiene, polyisoprene, polyacrylic acid, and derivative, mixture or copolymer.
Collector includes but not limited to stainless steel, copper, nickel, titanium, aluminium.The more preferably aluminium collector of carbon coating, more easily covers the coating that comprises positive active material, has lower contact resistance, and can suppress the corrosion of sulfide.
Negative pole
Described in scheme containing aluminium negative active core-shell material, include but not limited to: aluminum metal, for example aluminium foil and be deposited on the aluminium on base material; Aluminium alloy, comprises and contains at least one element of being selected from Li, Na, K, Ca, Fe, Co, Ni, Cu, Zn, Mn, Sn, Pb, Ma, Ga, In, Cr, Ge and the alloy of Al.
Electrolyte
Ionic liquid described in scheme is halogen aluminic acid type ionic liquid.
Halogen aluminic acid type ionic liquid described in scheme is N-alkyl imidazole hydrochloride-aluminum halide system.
N-alkyl imidazole hydrochloride-aluminum halide system described in scheme, is characterized in that, N-alkyl imidazole hydrochloride is N-methylimidazole hydrochloride, N-ethyl imidazol(e) hydrochloride, N-isopropylimdazole hydrochloride, the one in N-normal-butyl imidazole hydrochloride.
Described in scheme, the concrete preparation method of imidazole hydrochloride is as follows:
Under the condition of ice-water bath, be that 1:1.0～1.2 slowly splash in hydrochloric acid solution by N-alkyl imidazole salt according to mol ratio, continue to stir 30min, product vacuum is revolved and steamed after a few hours, product is placed in to 80 DEG C of vacuum drying chamber inner drying 12h, gained solid is imidazole hydrochloride again.
N-alkyl imidazole hydrochloride-aluminum halide system described in scheme, is characterized in that, described aluminum halide is the one in aluminium chloride, aluminium bromide or silver iodide.
N-alkyl imidazole hydrochloride-aluminum halide system described in scheme, is characterized in that, the mol ratio of N-alkyl imidazole hydrochloride and aluminum halide is 1:1.1～3.0.
The preparation method of the secondary aluminium-sulfur battery described in scheme is as follows:
By positive electrode active materials, conductive agent, binding agent (ratio is 7:2:1), making active material slurry is applied on the nickel foam substrate that 0.6mm is thick, oven dry roll to 0.33 millimeter be cut into 40mm wide × the long pole piece of 15mm, be wound into battery core with the thick barrier film of 0.16mm and the negative pole made as negative active core-shell material with aluminium flake and pack nickel plating box hat into, the non-water that reinjects is containing aluminium electrolyte, and secondary aluminium cell is made in sealing.
(3) beneficial effect
(1) the halogen aluminic acid ionic liquid being formed with N-alkyl imidazole hydrochloride by aluminum halide provided by the invention, has high conductivity, low viscosity and wider electrochemical window.Taking this ionic liquid as electrolyte, the aluminum cell that metal aluminum or aluminum alloy is negative pole, has realized electrochemical reversible deposition and the stripping of element aluminum on negative pole, makes it to become the secondary aluminium cell that can discharge and recharge.
(2) preparation of the halogen aluminic acid ionic liquid being formed with N-alkyl imidazole hydrochloride by aluminum halide provided by the invention, method is simple, raw material wide material sources, be easy to make, green non-poisonous, with the secondary aluminium-sulfur battery that negative pole aluminium and anodal sulphur form, be a kind of environmental friendliness, cheap, use safe secondary cell.
Brief description of the drawings
Fig. 1 is " aluminium chloride/N-ethyl imidazol(e) hydrochloride ionic liquid " cyclic voltammetry curve.
Embodiment
Below with reference to embodiment, the technique effect of design of the present invention, concrete structure and generation is described further, to understand fully object of the present invention, feature and effect.The following examples have been described several execution mode of the present invention, and they are only illustrative, and nonrestrictive.
Embodiment mono-
Taking " aluminium chloride/N-methylimidazole hydrochloride ionic liquid ", electrolyte is as example, and preparation process is as follows:
1. the concentration of utilizing NaOH titer to calibrate hydrochloric acid used is 9.776mol/kg, then takes 10.611g(0.104mol) hydrochloric acid solution, be transferred in constant pressure funnel;
2. in 500mL round-bottomed flask, take 8.21g(0.1 mol) N-methylimidazole, add stirrer, after connecting with constant pressure funnel, flask is placed in to ice-water bath;
3. open magnetic stirring apparatus, regulate after rotating speed, regulate constant pressure funnel, hydrochloric acid solution is slowly splashed in flask, after hydrochloric acid is added dropwise to complete, continue to stir 30min, until hydrochloric acid and 1-methylimidazole fully react, obtain the thick product of [mim] Cl;
4. the flask containing thick product is connected on Rotary Evaporators, steams 2h at negative pressure 0.1MPa and 80 DEG C of backspins, except the volatile impurity such as moisture and unreacted hydrogen chloride in thick product, obtain lurid liquid;
5. [mim] Cl liquid obtaining is placed in to 80 DEG C of vacuum drying chamber inner drying 24h, cooling rear formation solid.
6. under stirring condition, by 26.668g AlCl
3slowly join in N-methylimidazole hydrochloride, after formation liquid, continue to stir 24h.
Embodiment bis-
Taking " aluminium chloride/N-ethyl imidazol(e) hydrochloride ionic liquid ", electrolyte is as example, and preparation process is as follows:
1. the concentration of utilizing NaOH titer to calibrate hydrochloric acid used is 9.776mol/kg, then takes 11.252g(0.110 mol) hydrochloric acid solution, be transferred in constant pressure funnel;
2. in 500 mL round-bottomed flasks, take 9.613g(0.100 mol) N-ethyl imidazol(e), add stirrer, after connecting with constant pressure funnel, flask is placed in to ice-water bath;
3. open magnetic stirring apparatus, regulate after rotating speed, regulate constant pressure funnel, hydrochloric acid solution is slowly splashed in flask, after hydrochloric acid is added dropwise to complete, continue to stir 30min, until hydrochloric acid and 1-methylimidazole fully react, obtain the thick product of [eim] Cl;
4. the flask containing thick product is connected on Rotary Evaporators, steams 2h at negative pressure 0.09 MPa and 100 DEG C of backspins, except the volatile impurity such as moisture and unreacted hydrogen chloride in thick product, obtain yellow liquid;
5. [eim] Cl liquid obtaining is placed in to 80 DEG C of vacuum drying chamber inner drying 24h, cooling rear formation solid.
6. under stirring condition, by 26.668g AlCl
3slowly join in N-ethyl imidazol(e) hydrochloride, after formation liquid, continue to stir 24h.
Adopt the tungsten electrode of working, aluminium wire is as reference electrode, and platinum, as to electrode, adds this electrolyte of 3ml, is assembled into three-electrode system, carries out cyclic voltammetry in nitrogen glove box, and sweep speed is 100mV/s, and cyclic voltammetric result as shown in Figure 1.
Taking mesoporous carbon-sulphur composite material (sulphur mass fraction 60%) as positive electrode, adding conductive agent acetylene black, binding agent PVDF(ratio is 7:2:1), making active material slurry is applied on the nickel foam substrate that 0.6mm is thick, oven dry roll to 0.33 millimeter be cut into 40mm wide × the long pole piece of 15mm, be wound into electric stamen with the thick non-negative pole of knitting barrier film and make as negative active core-shell material with aluminium flake of glass fibre of 0.16mm and pack nickel plating box hat into, the reinject electrolyte of preparation in embodiment mono-, two, AA type secondary aluminium cell is made in sealing.
Battery is discharged and recharged to experiment, charge to 2.4V with 1C, 0.5C electric discharge, electric discharge is by voltage 0.8V.
The made battery of embodiment mono-, open circuit voltage 1.83V, discharge capacity 655mAh first, circulates after 50 times, discharge capacity 441mAh.
The made battery of embodiment bis-, open circuit voltage 1.85V, discharge capacity 671mAh first, circulates after 50 times, discharge capacity 453mAh.
Although the present invention is described in detail with reference to embodiment, but those skilled in the art is to be understood that, in the case of the spirit and scope of the present invention described in not departing from appended claims and equivalent thereof, can make various amendments and replacement to it.
Claims (7)
1. a secondary aluminium cell, comprising:
(a) electrolyte, wherein said electrolyte is N-alkyl imidazole hydrochloride-aluminum halide ionic liquid;
(b) positive pole that comprises electro-chemical activity sulphur-containing substance;
(c) negative pole containing aluminium active material.
2. secondary aluminium cell as claimed in claim 1, is characterized in that, described electro-chemical activity sulphur-containing substance includes but not limited to: elementary sulfur and the organosulfur compound that comprises sulphur atom and carbon atom, they can be polymerizations or non-polymeric.
3. secondary aluminium cell as claimed in claim 1, is characterized in that, the described negative pole containing aluminium active material comprises: metal aluminum or aluminum alloy.
4. secondary aluminium cell as claimed in claim 1, is characterized in that: in described N-alkyl imidazole hydrochloride-aluminum halide ionic liquid, the mol ratio of N-alkyl imidazole hydrochloride and aluminum halide is 1:1.1～3.0.
5. secondary aluminium cell as claimed in claim 1, is characterized in that: described N-alkyl imidazole hydrochloride is N-methylimidazole hydrochloride, N-ethyl imidazol(e) hydrochloride, N-isopropylimdazole hydrochloride, the one in N-normal-butyl imidazole hydrochloride.
6. secondary aluminium cell as claimed in claim 1, is characterized in that: described aluminum halide is the one in aluminium chloride, aluminium bromide and silver iodide.
7. a preparation method for the alkyl imidazole of N-described in claim 5 hydrochloride, comprises the following steps:
Under the condition of ice-water bath, be that 1:1.0～1.2 slowly splash in hydrochloric acid solution by N-alkyl imidazole salt according to mol ratio, continue to stir 30min, product vacuum is revolved and steamed after a few hours, vacuumize 24h under 80 DEG C of conditions again, gained solid is N-alkyl imidazole hydrochloride.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104393264A (en) * | 2014-12-01 | 2015-03-04 | 杨成 | High-capacity battery and preparation method thereof |
| CN105406074A (en) * | 2015-12-09 | 2016-03-16 | 江苏科技大学 | Secondary ion battery with graphene composite electrode as positive electrode and preparation method |
| CN107665987A (en) * | 2016-07-29 | 2018-02-06 | 横店集团东磁股份有限公司 | A kind of battery and its assemble method using brominated ionic liquid as positive active material |
| CN108365257A (en) * | 2018-02-23 | 2018-08-03 | 山东科技大学 | A kind of aluminium ion battery and preparation method thereof based on carbon nanotube anode |
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| CN103181016A (en) * | 2010-09-13 | 2013-06-26 | 加利福尼亚大学董事会 | Ionic gel electrolyte, energy storage devices, and methods of manufacture thereof |
| WO2014030500A1 (en) * | 2012-08-21 | 2014-02-27 | トヨタ自動車株式会社 | Electrode body and cell provided with same |
| CN103825045A (en) * | 2014-03-26 | 2014-05-28 | 北京科技大学 | Aluminium ion battery and preparation method thereof |
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| CN101764254A (en) * | 2009-11-20 | 2010-06-30 | 无锡欧力达新能源电力科技有限公司 | Secondary aluminum battery and preparation method of anode thereof |
| CN103181016A (en) * | 2010-09-13 | 2013-06-26 | 加利福尼亚大学董事会 | Ionic gel electrolyte, energy storage devices, and methods of manufacture thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104393264A (en) * | 2014-12-01 | 2015-03-04 | 杨成 | High-capacity battery and preparation method thereof |
| CN105406074A (en) * | 2015-12-09 | 2016-03-16 | 江苏科技大学 | Secondary ion battery with graphene composite electrode as positive electrode and preparation method |
| CN107665987A (en) * | 2016-07-29 | 2018-02-06 | 横店集团东磁股份有限公司 | A kind of battery and its assemble method using brominated ionic liquid as positive active material |
| CN107665987B (en) * | 2016-07-29 | 2020-03-27 | 横店集团东磁股份有限公司 | Battery using bromine-containing ionic liquid as positive electrode active material and assembling method thereof |
| CN108365257A (en) * | 2018-02-23 | 2018-08-03 | 山东科技大学 | A kind of aluminium ion battery and preparation method thereof based on carbon nanotube anode |
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